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    • 专利摘要:
    The present invention relates to a composition comprising a crushed plant containing proteins, maltodextrin, and silicone. It also relates to an adhesive composition and articles comprising it, their methods of preparation and their uses.
    公开号:FR3041966A1
    申请号:FR1559347
    申请日:2015-10-01
    公开日:2017-04-07
    发明作者:Aurelie Morel；Fabrice Garrigue
    申请人:Ass F I D O P；
    IPC主号:
    专利说明:

    Tableau 1 : Récapitulatif des compositions 4b à 4e exprimées en pourcentage en poids sec de chaque ingrédient sur le poids sec total de composition. 2.3. Caractérisation des compositions obtenues Les compositions 4b à 4e peuvent être utilisées comme compositions adhésives et ont été caractérisées par :
    La mesure de l’extrait sec à l’aide d’une balance halogénée (105°C, temps de stabilisation de 20 secondes),
    La mesure d’un temps d’écoulement à l’aide de la coupe de viscosité Lory Elcometer 2215 (essai non normalisé),
    La mesure du temps de gel par suivi de l’évolution de la viscosité au Trombomat (température d’essai 180 à 200°C, cette gamme de températures correspondant à celles mises en œuvre lors du passage à chaud d’un panneau de bois composite). 3. Résultats
    Les résultats des mesures de viscosité et du temps de gel des compositions sont présentés dans le tableau 2 ci-dessous et en Figure 2.
    * Vcu : Viscous Coupling Unit
    Tableau 2 : Viscosité et temps de gel des compositions (sans la cire pour l’essai 4b).
    Comme cela peut être constaté sur la Figure 2, le temps de gel de la composition adhésive est significativement réduit avec l’introduction de maltodextrine et peu affecté avec l’introduction du silicone. Toutefois, un effet synergique de réduction du temps de gel de la composition est observé avec l’introduction de la maltodextrine et du silicone.
    La réduction du temps de gel peut se traduire par un pré-durcissement prématuré de la résine. Un bénéfice attendu de ce durcissement accéléré de la résine est une limitation de la chute de température rencontrée au cours du séchage en température. Cet effet permet en particulier de réduire la filtration de la composition adhésive au travers du matériau enduit par cette composition, par exemple au travers des pores des particules de bois. La composition adhésive reste ainsi plus en surface, par exemple des particules de bois et peut mieux assurer son rôle de liant.
    Exemple 3 : Préparation de panneaux de bois aggloméré
    Des panneaux de bois aggloméré ont été préparés à l’échelle laboratoire, à partir de compositions adhésives préparées de manières similaires à celles de l’Exemple 2. Pour des raisons de dimensionnement, les panneaux ont été préparés en une couche, à base de copeaux fins (correspondant à la couche intérieure d’un panneau classique). 1. Matériel 1.1. Compositions adhésives
    Les compositions adhésives 1c à 1f mises en oeuvre dans cet Exemple sont préparées de manières identiques aux compositions 4b à 4e respectivement, préparées à l’Exemple 2.
    Les compositions 1a et 1b sont préparées à partir de résine UF et éventuellement d’eau et de tourteau de colza broyé tels que décrits dans le matériel de l’Exemple 2. La préparation de ces compositions est plus amplement détaillée ci-après. 1.2. Particules de bois
    Les particules (dans le cas présent, des copeaux) de bois fins proviennent de Kronofrance. 2. Méthode 2.1. Préparation de la composition 1 a
    La résine UF est mélangée aux copeaux de bois. Pour ce faire, celle-ci est généralement pulvérisée sur les copeaux de bois dans un mélangeur. Toutefois, lors de ces essais, la résine a été mélangée manuellement avec les copeaux de bois.
    Lors de l’utilisation de cette composition comme composition adhésive, de la cire est ajoutée à cette composition. Cet ajout est effectué manuellement après mélange de la résine et des copeaux de bois. 2.2. Préparation de la composition 1 b
    Du tourteau de colza broyé est ajouté à de l’eau en 3 minutes environ par addition successive de petites quantités, à une vitesse d’agitation allant de 400 à 500 tours/minute en fonction de l’augmentation de la viscosité (c’est-à-dire qu’au moment de l’ajout d’une nouvelle quantité de tourteau broyé, la vitesse d’agitation est augmentée à 500 tours/min), jusqu’à l’obtention d’une suspension homogène. La quantité de tourteau ajouté en poids par rapport au poids total d’eau et de tourteau est de 25% p/p.
    Cette suspension de tourteau broyé en milieu aqueux est ensuite mélangée à une résine urée-formaldéhyde, ajoutée progressivement sous très vive agitation (environ 1200 tours/minute). L’agitation est maintenue pendant 2 à 3 minutes afin de bien homogénéiser le mélange.
    La teneur en extrait sec de la composition adhésive est enfin ajustée de tel sorte que la viscosité de la formulation adhésive reste constante par rapport à celle mesurée sur une formulation adhésive sans tourteau.
    Lors de l’utilisation de cette composition comme composition adhésive, de la cire est ajoutée à cette composition. Cet ajout est effectué manuellement après mélange de la résine et des copeaux de bois. 2.3. Tableau récapitulatif des compositions adhésives 1 a à 1 f
    Tableau 3 : Récapitulatif des compositions adhésives 1 a à 1 f exprimées en pourcentage en poids sec de chaque ingrédient sur le poids sec total de composition.
    2.4. Caractérisation des compositions obtenues Les compositions adhésives 1a à 1f ont été caractérisées par :
    La mesure de l’extrait sec,
    La mesure d’un temps d’écoulement,
    La mesure du temps de gel, comme cela est décrit à l’Exemple 2. 2.5. Etuvage de copeaux de bois L’étuve utilisée est une étuve classique avec ventilation.
    Les copeaux sont placés en étuve à 60¾ dans des barquettes en aluminium d’une contenance de 100 g environ (ce qui facilite le placement des copeaux dans l’étuve). Ils sont laissés au minimum 6h à cette température. L’extrait sec des copeaux utilisés pour les panneaux de bois composition est de 97% (mesuré sur une balance à extrait sec).
    Les copeaux sont laissés dans l’étuve jusqu’à utilisation. Ils sont sortis de l’étuve peu de temps avant la réalisation du panneau de bois (environ 10 à 15 minutes, maximum afin d’éviter une reprise en humidité des particules, et qui correspondent au temps de refroidissement). 2.6. Préparation des panneaux de bois aggloméré Les panneaux ont été préparés de la façon suivante : (i) Mélange manuel des copeaux de bois (après refroidissement suite à la sortie de l’étuve) avec l’une des compositions adhésives 1a à 1f à une température de 30 à 35°C et pendant 2 min ; (ii) Pour les compositions adhésives 1a à 1c, ajout de la cire au mélange obtenu à l’étape (i) et mélange manuel pendant 1 min ; (iii) Incorporation des mélanges obtenus aux étapes (i) (mélange à partir des compositions adhésives 1 d à 1 f) et (ii) (mélange à partir des compositions adhésives 1a à 1c) dans un moule dont les dimensions ont été calculées afin de pouvoir fixer la densité du panneau à 650kg/m3 (les panneaux obtenus mesurent environ 250 x 350 mm2 pour une épaisseur finale de 7-8 mm) ; (iv) Incorporation des moules contenant les mélanges dans une presse MI41 de chez TechniHispania à 200°C pendant 4 minutes. 2.7. Tableau récapitulatif des panneaux de bois obtenus à partir des compositions adhésives 1 a à 1 f
    * % en poids sec par rapport au poids sec total du panneau de bois aggloméré
    Tableau 4 : Récapitulatif des compositions des panneaux de bois obtenus à partir des compositions adhésives 1 a à 1 f 2.8. Caractérisation des panneaux de bois aggloméré Les panneaux de bois aggloméré sont caractérisés par deux paramètres :
    Le gonflement à l’eau : la mesure de gonflement en épaisseur du panneau de bois après immersion totale dans l’eau (selon la norme NF EN 317) est effectuée à température ambiante, les mesures de l’épaisseur étant réalisées à tO, t+2h, t+24h, en moyenne sur 3 éprouvettes,
    La résistance mécanique : la mesure est effectuée par un essai de flexion 3 points visant à évaluer la contrainte maximale, et le module de flexion (MPa) Cette mesure est inspirée de la norme NF EN 310 et est effectuée sur machine de traction type MTS Criterion (model43), avec un capteur à 2 kN, une vitesse d’essai à 2 mm/min, en moyenne sur 5 éprouvettes.
    Les normes telles qu’indiquées dans la présente demande sont celles en vigueur à la date de dépôt. 3. Résultats 3.1. Résultats sur les compositions adhésives Les résultats des mesures de viscosité et du temps de gel des compositions sont présentés dans le Tableau 5 ci-dessous.
    * Vcu : Viscous Coupling Unit
    Tableau 5 : Viscosité et temps de gel des compositions adhésives 1 a à 1 f (sans la cire pour les essais a, b et c).
    Le temps de gel de la composition adhésive est : significativement réduit avec l’introduction de tourteau et de maltodextrine, et peu affecté avec l’introduction d’urée.
    Un effet synergique de réduction du temps de gel de la composition est observé là aussi avec l’introduction de la maltodextrine et du silicone. 3.2. Résultats sur les panneaux de bois aggloméré Les résultats en termes de gonflement à l’eau et résistance mécanique sont indiqués dans le Tableau 6 ci-dessous et en Figure 3.
    Tableau 6 : Propriétés mécaniques et résistance à l’eau des panneaux de bois aggloméré préparés à l’aide des compositions adhésives 1a à 1f
    Les propriétés mécaniques du panneau de bois aggloméré sont nettement améliorées lorsque celui-ci est préparé avec la composition adhésive 1d, c’est-à-dire avec la composition adhésive comportant en combinaison une maltodextrine et un silicone, à savoir de la maltodextrine et un siloxane, respectivement.
    En effet, comme cela peut être constaté sur la Figure 3A, la résistance à la contrainte est la meilleure pour le panneau de bois préparé avec une composition comportant à la fois du tourteau de colza broyé, de l’urée, de la maltodextrine et un siloxane.
    On note plus particulièrement que : l’ajout de tourteau et, dans une moindre mesure, l’ajout d’urée augmentent sensiblement la résistance à la contrainte, tandis que l’ajout de maltodextrine ou bien de siloxane seul diminue légèrement cette résistance.
    Or, de manière inattendue, l’ajout combiné de maltodextrine et de siloxane augmente notablement la résistance à la contrainte.
    Concernant le gonflement à l’eau, comme cela peut être constaté sur la Figure 3B, l’ajout de tourteau dégrade notablement la résistance du panneau de bois au gonflement lors de son immersion dans l’eau. Cette dégradation est totalement compensée par l’ajout d’urée. Toutefois, l’ajout de maltodextrine ou de siloxane
    provoque chacun une très légère augmentation du taux de gonflement à l’eau tandis que, de manière inattendue, l’ajout combiné de maltodextrine et de siloxane permet de diminuer ce taux de gonflement. Le meilleur résultat en termes de résistance au gonflement à l’eau est ainsi obtenu avec un panneau de bois aggloméré préparé avec une composition comportant à la fois du tourteau de colza broyé, de l’urée, de la maltodextrine et un siloxane.
    Exemple 4 : Effet de la nature chimique du silicone sur les propriétés du panneau de bois aggloméré 1. Matériel 1.1. Silicone
    Deux polymères à base de polydimétyl siloxane ont été testés, tous deux fournis par Evonik (Allemagne) :
    Tegostab B8460 : copolymère polyéther - polydimétyl siloxane, et
    Tegoprotect 5000 : polydimétyl siloxane fonctionnalisé hydroxy. 1.2. Compositions adhésives
    Les compositions adhésives 3a et 3b mises en oeuvre dans cet Exemple sont préparées de manière identique à la composition 4c de l’Exemple 2, la seule différence entre les compositions 3a et 3b étant la nature du silicone introduit dans la composition. 1.3. Panneaux de bois
    Les panneaux de bois aggloméré sont préparés comme indiqué à l’Exemple 3. 1.4. Tableau récapitulatif des panneaux de bois obtenus à partir des compositions adhésives 3a et 3b
    * % en poids sec par rapport au poids sec total du panneau de bois aggloméré
    Tableau 7 : Récapitulatif des compositions des panneaux de bois obtenus à partir des compositions adhésives 3a et 3b 2. Méthode 2.1. Caractérisation des compositions obtenues
    Les compositions adhésives 3a et 3b ont été caractérisées par :
    La mesure de l’extrait sec,
    La mesure d’un temps d’écoulement,
    La mesure du temps de gel, comme cela est décrit à l’Exemple 2. 2.2. Caractérisation des panneaux de bois aggloméré
    Les panneaux de bois aggloméré sont caractérisés par deux paramètres :
    Le gonflement à l’eau,
    La résistance mécanique, comme cela est décrit à l’Exemple 3. 3. Résultats 3.1. Résultats sur les compositions adhésives Les résultats des mesures de viscosité et du temps de gel des compositions sont présentés dans le Tableau 8 ci-dessous.
    * Vcu : Viscous Coupling Unit
    Tableau 8 : Viscosité et temps de gel des compositions adhésives 3a et 3b 3.3. Résultats sur les panneaux de bois aggloméré
    Les résultats en termes de gonflement à l’eau et résistance mécanique sont indiqués dans le Tableau 9 ci-dessous et en Figure 4.
    Tableau 9 : Propriétés mécaniques et résistance à l’eau des panneaux de bois aggloméré préparés à l’aide des compositions adhésives 3a et 3b
    Comme cela peut être constaté sur la Figure 4A, les propriétés mécaniques des panneaux de bois aggloméré obtenus avec les deux tensioactifs sont similaires. En revanche, la résistance à l’eau du panneau de bois aggloméré est améliorée lorsque le panneau de bois est préparé avec une composition adhésive comportant du Tegostab B8460 par rapport à un panneau de bois est préparé avec une composition adhésive comportant du Tegoprotect 5000. Toutefois, la résistance à l’eau de ce dernier reste dans la limite haute acceptable.
    The present invention relates to a composition based on ground meal, and more particularly milled oleaginous and / or proteinaceous plants, its method of production and its uses.
    In recent years, the exploitation of oleaginous and protein crops has greatly increased, to meet the needs of society.
    Oleaginous and protein crops are generally grown and grown for their seeds or fruits, which are particularly rich in fat and protein, respectively.
    The oleaginous plants include sunflower, rapeseed, peanut, sesame, cotton, flax, castor oil, olive oil, oil palm, hazelnut, walnut, almond or the coconut tree. However, although classified as "oleaginous", these plants also have a significant content of proteins.
    Soybean, which is a protein crop, is sometimes referred to as oilseed crop because it also produces oil. As a result, it is often classified separately among oilseed crops because it is rich in both fat and protein.
    Protein crops include peas (chickpeas, split peas), faba beans and lupins, but also lentils, fenugreek and beans.
    The oilseeds are mainly grown for their oil, used in various sectors, such as food and feed, lubricants, cosmetics, agronomy, especially in the phytosanitary field, oil exploitation, materials and the environment. energy industry, for the production of biofuels such as biodiesel.
    The transformation of the seeds or fruits of oleaginous plants into oil is generally done according to three main operations, that are: - the preparation of the raw material to be extracted (seeds or fruits of an oleaginous plant): during its preparation, the raw material may undergo one or more of the following steps: cleaning or dusting, sieving, dehulling or lamination. - Trituration: this operation may include several steps depending on the raw material to grind. This operation includes in all cases a step of grinding and extraction of the oil contained in the raw material. the refining of the oil, which consists in eliminating all or part of the compounds contained in an oil rendering it unfit for its use or its subsequent transformation. For example, the refining of an oil for human consumption will generally include steps of taste neutralization, discoloration, deodorization, etc. The crushing operation is a crucial transformation operation because it aims at extracting the oil contained in the seeds or the fruits of the oleaginous plants.
    This trituration operation therefore depends on the raw material from which the oil is to be extracted. By way of example, in the case of oilseed seeds, the extraction carried out during the crushing is mainly based on two traditional techniques: the so-called "rich" seeds in oil (> 35%, for example sunflower or rapeseed) are crushed by pressure and then by chemical extraction while seeds considered as "poor" in oil ( <35%, soybean for example) usually undergo chemical extraction.
    By chemical extraction, it is more particularly a solvent extraction, such as extraction with water or with an organic solvent. When the extraction is carried out with an organic solvent, this step may be followed by a desolventization step (step for removing solvents from a substrate, such as a plant cake).
    For example, in the case of rapeseed or sunflower, the trituration operation comprises the following steps: flattening: it is a step of grinding the seeds. In general, these pass between two smooth cylinders and come out crushed, in the form of "flakes". - Cooking: this step aims to facilitate the extraction of the oil contained in the seeds. In general, the flakes from flattening are heated to about 80 ° C. the extraction of the oil contained in the seeds: this step is generally carried out by pressing (or pressing) in presses.
    All these steps can be carried out with the aid of a single machine performing a continuous hot pressure, that is to say that the seeds are preheated to about 90%, crushed / flattened and then pressed into a worm where the temperature will reach up to about 120 ° C.
    Two products are recovered at the end of this pressing step: on the one hand oil, generally referred to as "crude" or "pressure", and - on the other hand, a first solid residue, namely press scales or a fat cake.
    The fat cake usually comprises between 10 and 20% of residual oil.
    In order to extract this residual oil present in the fatty cake, the trituration may comprise at the end of the pressing, a chemical extraction step by solvent. The solvent usually used for this extraction is hexane. The solvent extraction step thus gives on the one hand the "residual" oil coming from the oily meal, and on the other hand a second residue of the seeds, called deoiled cake. The deoiled cake generally comprises between 0.1 and 10%, preferably from 1 to 4% of non-extracted oil.
    In contrast, in the case of soybeans, the crushing operation essentially comprises the following steps: flattening, and the extraction of the oil contained in the seeds: this step is generally carried out by chemical extraction with solvent. At the end of the soybean crushing, two products are recovered: oil and soybean meal.
    The cake is therefore a co-product of vegetable oil production. However, the valorization of oilcakes by the oleaginous and / or oléoprotéagineuse sector has greatly increased in recent decades. Indeed, the plant meal is very rich in good quality protein, the latter was quickly used as a source of vegetable protein in animal feed, in substitution or in addition to animal protein. But the use of plant cakes has not been limited to these specific value chains and has developed more recently in other areas, particularly in the field of chemistry.
    In this field, much research has focused in recent decades on what has been called "green chemistry", the main objective of which is the use of more environmentally friendly products such as, for example, the use of of products of renewable origin and the valorization of co-products. However, plant cakes represent a bio-sourced product of the future because of their specific properties derived in particular from their remarkable levels of protein and pectin. For example, it is known to use plant cakes in the formulation of adhesive compositions for the manufacture in particular of composite wood panels. Application WO 2011/156380 discloses in particular a protein-based adhesive composition comprising a pre-polymer such as a polyisocyanate-based prepolymer, and a protein component, which may be a milled seed cake, in an amount sufficient to dispersing the prepolymer in an aqueous medium.
    There is still a need for composite wood panels based on environmentally friendly material such as crushed plant cake with improved properties.
    The work of the inventor has made it possible to demonstrate that the use of a particular plant grind composition makes it possible to improve the properties of the wood panels comprising the said composition. The invention therefore relates to a composition comprising: a crushed plant containing at least 3% of proteins, maltodextrin, and silicone.
    It will be noted that throughout the application, and unless otherwise stated, the ranges of values indicated are included limits.
    "Crushed plant material containing at least 3% protein" (hereinafter also referred to as "ground vegetable material") is intended to mean a vegetable material in the form of particles, after grinding and containing at least 3% of protein . Preferably, the crushed plant contains at least 10% of proteins, more preferably at least 20%.
    The plant meal referred to by the invention may comprise particles insoluble in water.
    Preferably, the ground meal containing at least 3% protein is: - a cake of one or more species of ground oleaginous plants (hereinafter referred to as "milled vegetable meal"), - a fruit mash and / or seeds of one or more ground proteinaceous plant species (hereinafter referred to as "crushed protein plants"), or - their mixture.
    More preferably still, the crushed plant is a crushed plant cake.
    The composition according to the invention makes it possible in particular to improve the properties of an adhesive composition and / or an article comprising it. In particular, the inventors have demonstrated that the adhesive compositions and articles based on lignocellulosic materials, comprising a composition according to the invention have improved properties such as the gel time for the adhesive composition or the mechanical strength properties and swelling with water for the items. The advantages of the composition according to the invention will be more fully presented later in the application, and in the examples.
    By "grinding" is meant any step to obtain a plant powder, and more particularly a plant meal powder. The grinding may comprise a pre-grinding and / or one or more fractionations of the grind.
    Pre-grinding is a step aimed primarily at making a first reduction in the form of coarse particles. This pre-grinding is generally followed by a fractionation step.
    The purpose of the fractionation is to select part of the particles according to their size and / or chemical composition and can be carried out by various techniques such as sieving to a particular particle diameter, or tribo separation.
    According to the invention, "plant cake" denotes a fat cake or deoiled obtained at the end of an extraction step (trituration, chemical extraction such as solvent) of the oil contained in the seeds or the fruits of oleaginous plants. Preferably, the cake is a deoiled cake derived from a trituration step followed by a solvent extraction step.
    Advantageously, the plant cake comprises a percentage of oil of 0.1 to 20%, preferably 1 to 4% by weight of the total dry weight of plant cake.
    By "maltodextrin" is meant a polysaccharide derived from the hydrolysis of starch. Derivatives of the hydrolysis of starch are generally defined by their dextrose equivalent (DE).
    DE is the amount of reducing sugars expressed as a percentage of dextrose, also called D-glucose, relative to the total dry weight of product. Generally, the DE is indicated by a number or a number without indication of the unit (%). For example, dextrose, which corresponds to the product resulting from the total hydrolysis of the starch, will be characterized by a DE equal to 100%, or 100. On the contrary, the unhydrolyzed starch will be characterized by a DE equal to 0. Maltodextrin is defined as a derivative of the hydrolysis of starch having a DE between 0 and 20. The starch derivatives having a DE in the range] 20; 100 [are, for their part, called glucose syrups.
    Advantageously, the maltodextrin will have an DE of between 0 and 13, preferably between 0.5 and 10 and more preferably between 1 and 6.
    In addition to DE, maltodextrins can also be distinguished by their sugar composition, that is the nature and the number of sugars that compose them. Indeed, depending on the source of starch used (potato, corn, wheat), the type of hydrolysis implemented (chemical or enzymatic hydrolysis) or depending on the conditions of the hydrolysis, this sugar composition may vary. .
    Advantageously, the maltodextrin used in the composition according to the invention will have good characteristics of dispersion and solubility in water. Maltodextrins that can be used in the context of the present invention are, for example, the maltodextrins marketed by ROQUETTE® under the tradename GLUCIDEX®.
    By "silicone" (also referred to as "polysiloxane" or "siloxane") is meant oligomers, polymers or co-polymers having an inorganic skeleton comprising one or more silicon-oxygen chain (s) alternately, each chain being optionally be substituted on the silicon atoms by organic groups. Reactive or non-reactive organic groups may thus be grafted at the end of the chain and / or laterally on the main backbone.
    Advantageously, the silicone is a polymer based on polydimethyl siloxane. Preferably, the silicone is a polyether-polydimethyl siloxane copolymer.
    Preferably, the amount of maltodextrin in the composition is between 0.1 and 20%, more preferably between 0.5 and 10%, more preferably between 1 and 4% by dry weight on the total dry weight of cake.
    Advantageously, the amount of silicone in the composition is between 0.5 and 30%, preferably between 5 and 20%, more preferably between 8 and 15% by dry weight on the total dry weight of cake.
    According to a first embodiment of the invention, the ground material of the composition is one or more crushed plant meal (s) chosen from the group consisting of rapeseed, canola, sunflower meal, soy, cotton, flax, walnut, olive, mustard, hemp, carnation, safflower, kapok, corn germ, rape, safflower, shea, sesame, castor , camelina, jatropha, peanut, oil palm, hazelnut, almond and copra kernels. The carnation is also known as the black poppy. Copra is the dried raw material used for the extraction of coconut oil. At the end of this extraction, a copra cake is obtained.
    Advantageously, the (s) cake (x) of crushed plants is (are) chosen (s) from the group consisting of rapeseed cake, canola, sunflower, soy and castor oil.
    Preferably, the crushed plant meal is rapeseed or canola meal.
    According to a second embodiment, the grind of plants in the composition is obtained by grinding fruit and / or seeds of proteinaceous plants selected from the group consisting of pea, faba bean, lupine, lentils, fenugreek and beans.
    Preferably, the protein crops are selected from the group consisting of pea, faba bean and lupine.
    According to the first embodiment of the invention, the crushed plant cake in the composition is in the form of a powder having a median volume diameter D50 of between 1 and 250 μm.
    The median volume diameter D50 is a characteristic known to those skilled in the art. This diameter makes it possible to characterize a size distribution of the particles of a powder and corresponds to the diameter for which 50% of the total volume of the particles has a diameter less than the D50.
    Preferably, the crushed plant meal is in the form of a powder having a median volume diameter D50 of between 5 and 100 μm, more preferably between 10 and 75 μm, more preferably between 15 and 50 μm, more preferably still between 20 and 40 μm. .
    D99 volume diameter can also be used to characterize a particle size distribution of a powder. The diameter D99 is defined similarly to the volume median diameter D50 powder and corresponds to the diameter for which 99% of the total volume of the particles to a diameter less than D99.
    Preferably, the crushed plant meal is in the form of a powder having a volume diameter D99 of between 40 and 300 μm, preferably between 70 and 180 μm, more preferably between 80 and 140 μm.
    This particle size is also the one preferred for all the other types of ground material envisaged according to the invention.
    Whatever the embodiment, the composition according to the invention is advantageously in the form of granules. When the pellet is prepared from a cake, it can also be called "coated cake". The invention also relates to a process for the preparation of a composition according to the invention comprising the following steps: (i) the grinding of the seeds and / or fruits of oleaginous and / or proteinaceous plants, (ii) the addition of maltodextrin and of silicone to the ground vegetable obtained in step (')
    By "grinding" is meant any step to obtain a plant powder, and more particularly a plant meal powder. More particularly, the powder resulting from this grinding has a median volume diameter D50 of between 1 and 250 μm.
    Preferably, the grinding is carried out so as to obtain a powder whose volume median diameter D50 is between 5 and 100 μm, preferably between 10 and 75 μm, more preferably between 15 and 50 μm, and even more preferably between 20 and 40 pm.
    Alternatively, the grinding may be performed so as to obtain a powder whose volume median D99 is between 40 and 300 μm, preferably between 70 and 180 μm, more preferably between 80 and 140 μm.
    A grinder particularly suitable for carrying out the grinding step according to the process of the invention is a chopper type chipper.
    Preferably, the grinding is performed on a cake of plants and is made so as to limit the heating of said cake. For this, the grinding is carried out at a temperature below ΙΟΟ'Ό, preferably below 80 ^ 0, more preferably below 60 ° C.
    Throughout the application, temperatures and pressures are indicated under normal temperature and pressure (CNTP) conditions.
    The grinding may, optionally, be preceded by a pre-grinding.
    Pre-grinding is a step mainly aimed at making a first reduction in the form of particles. More particularly, by pre-grinding, it is intended any step to obtain a powder, such as a plant meal powder, having a median volume diameter D50 of between 250 and 450 pm.
    This pre-grinding is preferably followed by a fractionation step. In general, this fractionation is sieving (also referred to in this particular case as "blutage"). This sieving is preferably carried out at a diameter approximately equal to the volume median diameter D50 as defined during the pre-grinding step for recovering the fines having a diameter less than the median volume diameter and the refusal having a diameter greater than the diameter. median volume.
    In the case of a plant meal, this pre-grinding followed by blutage (or sieving) makes it possible to separate a protein-rich fraction ("the fines" used for the preparation of the ground meal) of a fraction depleted in proteins ( that is to say the refusal). At the end of the pre-grinding and the possible blutage, grinding is carried out. This grinding can also be followed by a fractionation step. Such a fractionation can be achieved by a cyclone. Other dry or wet fractionation technologies may also be applied such as tribo-separation. By way of example, the application WO2015 / 097290 describes a process for tribo-separation of a plant cake.
    According to a preferred embodiment of the process according to the invention, the addition of maltodextrin and silicone carried out in step (ii) is carried out by the preparation of at least one aqueous solution comprising maltodextrin and / or silicone.
    The aqueous solution can be prepared from any type of water, such as tap water, demineralized, deionized and / or distilled water.
    Advantageously, the aqueous solution comprises maltodextrin. This solution comprises maltodextrin at a content of between 1 and 40% by dry weight of maltodextrin on the total weight of water, preferably between 10 and 30% by dry weight of maltodextrin on the total weight of water, plus preferentially still between 15 and 25% by dry weight on the total weight of water.
    The aqueous solution of maltodextrin may further comprise silicone. This solution then comprises the silicone at a content between 30 and 80% by dry weight of silicone on the total weight of water, preferably between 40 and 70% by dry weight of silicone on the total weight of water, plus preferably still between 55 and 65% by dry weight on the total weight of water.
    The total water weight of the aqueous solution is defined as the total weight of water introduced into the solution, without taking into account the water inherently included in the ground vegetable, maltodextrin or any other ingredient introduced into the solution. solution other than water.
    The aqueous solution may also include other ingredients, such as urea. For example, the urea content in the aqueous solution is between 0.01 and 40% by weight relative to the total weight of water.
    According to a first variant of the preferred embodiment, the aqueous solution is sprayed on the ground material obtained in step (i).
    Preferably, the spraying is carried out with an aqueous solution comprising both maltodextrin and silicone.
    Alternatively, two sprays can be carried out on the one hand with the aqueous solution of maltodextrin and on the other hand with the silicone. In this case, the silicone is preferably sprayed before the aqueous solution of maltodextrin.
    Advantageously, the spraying is carried out under vacuum. Preferably, the spraying system is provided with a solid cone nozzle to ensure better dispersion of the drops.
    Drying of the plant meal can then be carried out at a temperature of the order of 20 to 70 ° C, preferably of the order of 40 to 60 ° C. At the end of this drying, a granulate of ground mills (coated with maltodextrin and / or silicone) is obtained, having a moisture content of about 1 to 12% by weight, preferably of the order from 5 to 7%.
    According to a second variant of the preferred embodiment, the ground material obtained in step (i) is suspended in the aqueous solution.
    Preferably, the ground material obtained in step (i) is suspended at a content of between 30 and 80%, more preferably between 40 and 70%, even more preferably between 55 and 65% by dry weight relative to the total weight. of water and ground.
    More particularly, the ground material obtained in step (i) is suspended in an aqueous solution containing maltodextrin.
    This aqueous solution containing maltodextrin may advantageously comprise urea.
    In this case, the silicone is added to the aqueous suspension containing the ground material obtained in step (i), maltodextrin and optionally urea. The invention also relates to an adhesive composition comprising a composition according to the invention, and to one or more precursors of a resin chosen from the group consisting of polymethylene diphenyl 4,4'-diisocyanate, urea-formaldehyde, phenol- formaldehyde and / or melamine-urea-formaldehyde.
    The term "precursor of a resin" is intended to mean a component or mixture of components which, after a polymerization step, makes it possible to obtain said resin. The use of a composition according to the invention makes it possible to reduce the gel time of the adhesive composition according to the invention, as described in Examples 2 and 3 and in FIG. 2.
    Polymethylene diphenyl 4,4'-diisocyanate is also known as pMDI, urea-formaldehyde under the name UF, phenol-formaldehyde under the name PF and melamine-urea-formaldehyde under the name MUF .
    Preferred resin mixtures are pMDI and UF on the one hand and pMDI and PF on the other hand.
    The adhesive composition according to the invention may further comprise urea, a hydrophobic agent such as wax.
    By "hydrophobing agent" is meant any substance whose function is to prevent or reduce the contact or penetration of water in a material.
    More generally, the adhesive composition according to the invention may comprise one or more agents chosen from the group consisting of: formaldehyde entrapping agents or crosslinking agents such as urea, phenol, catalysts, tackifiers, fillers such as calcium carbonate, clay, thickeners or texturizing agents or gelling agents, surfactants such as siloxanes, adhesion promoters such as a polyol, for example in the case where the resin introduced in the composition is isocyanate-based, antioxidants such as polyphenols, antifoaming agents, antimicrobial agents such as oxidants, antibacterial agents such as nitrogen derivatives, fungicides such as sulfur products, preservatives such as citric acid, paraben, pigments such as titanium dioxide, moisture-enhancing agents or hydrophobing agents such as such as wax, pH modulators such as urea, and composite release or release agents, fire retardants.
    A solid binder can also be prepared from the adhesive composition according to the invention by polymerization thereof. Advantageously, the polymerization is carried out by hot curing. The curing temperature is generally between 100 and 300 ° C, more preferably between 140 and 250 ° C. The invention also relates to an article comprising an adhesive composition according to the invention and a lignocellulosic material.
    By "lignocellulosic material" is meant more particularly paper, cardboard, strips of wood, wood veneer, wood particles, wood fibers. Wood particles can be chips, sawdust or other wood waste from a sawmill. The use of a composition or an adhesive composition according to the invention makes it possible to improve the properties of articles based on lignocellulosic material (s) comprising them. In particular, these articles have an increased resistance to stress and a decreased swelling rate, as compared to articles comprising a composition or an adhesive composition based on crushed sole plants, crushed plants and maltodextrin, or ground grinds. of plants and silicone. These advantages are more fully presented in Example 3 and Figure 3.
    Advantageously, the article according to the invention is a lignocellulosic composite panel. A lignocellulosic composite panel is a combination of lignocellulosic materials and an adhesive composition called matrix, in which the lignocellulosic materials and the matrix retain their identity, do not dissolve or do not mix completely. As a result, they can be physically identifiable on a macroscopic scale.
    More particularly, the article is glue-laminated wood, plywood or a composite wood panel such as a slat or oriented particle board (OSB), particle board or chipboard, or a wood fiber board. The invention also relates to a method of manufacturing an article according to the invention. Advantageously, the method comprises the following steps: (i) contacting a lignocellulosic material with the adhesive composition according to the invention, and (ii) heating the adhesive composition so as to cure it.
    The curing temperature is generally between 100 and 300 ° C, more preferably between 140 and 250 V. The curing time is less than 10 min, preferably less than 5 min. Preferably, the heating of the adhesive composition so as to cure it is effected by thermopressing (concomitant heating and pressing step).
    Advantageously, the lignocellulosic material is wood particles. These are then brought into contact with the adhesive composition according to the invention. This contacting can be carried out by mixing the wood particles with the composition according to the invention or alternatively by spraying the composition according to the invention on the wood particles. The wood particles thus brought into contact with the adhesive composition according to the invention are then placed in a mold, pressed and heated to harden the adhesive composition.
    More particularly, a wood particle board is usually manufactured according to the following method:
    Preparation of the lignocellulosic raw material (grinding, classification, drying), mixing with the adhesive composition,
    Formation of the particle mattress,
    Thermopressing, and possibly
    Finishing panels. The invention finally relates to the use of a composition according to the invention for the preparation of an adhesive composition, a polyurethane foam, a cosmetic composition, a phytosanitary composition or a food composition.
    Preferably, the adhesive composition is an adhesive composition for lignocellulosic material, such as wood-based materials. By way of example, the characteristics of these wood-based materials, such as wood panels, and their method of manufacture are more fully described above and in Example 3.
    By "phytosanitary composition", it is more particularly a composition for the protection of crops.
    Preferably, the food composition is an animal feed composition, such as a feed composition for aquaculture. The invention will be better understood from the following examples, given by way of illustration, with reference to:
    Figure 1, which represents the typical profile of particle size distribution measured in the dry state on the powder of a milled cake of plants (for example, rapeseed, sunflower, soy ...);
    FIG. 2, which represents a diagram illustrating the effect of the introduction of maltodextrin and / or silicone on the gel time of an adhesive composition,
    FIG. 3 which represents diagrams illustrating the effect of the introduction of maltodextrin and / or silicone on the properties of an agglomerated wood panel, in particular, the mechanical strength (maximum flexural stress 3 points (MPa), Fig. 3A) and the water swelling rate of a chipboard (as a% increase in thickness) after 24h of immersion (Fig. 3B); and
    Figure 4, which presents diagrams illustrating the effect of the chemical nature of the silicone on the properties of a chipboard, in particular, the mechanical strength (maximum flexural stress 3 points (MPa), Fig. 4A) and the water swelling rate of a chipboard (in% increase in thickness) after 24 hours of immersion (Fig. 4B). Other features and advantages of the invention will become apparent in the examples which follow, given by way of illustration.
    Example 1 Composition According to the Invention in Granule Form 1. Material 1.1. oilcake
    The rapeseed cake used in this example was supplied by Saipol (Grand Couronne site, France). This cake was obtained by a hot pressing step, followed by a step of extraction by organic solvent (ie hexane) pressure flakes (which designate the product obtained at the end of the pressure step hot) to extract the vegetable oil.
    By hot pressing step is meant a step comprising a preheating of rapeseeds up to 90 ° C, then grinding said seeds and pressing in a worm where the temperature can reach up to 120 ° C. A fat meal is then obtained comprising 12% to 14% of residual oil.
    Finally, the organic solvent extraction step is followed by a desolvation step.
    The rapeseed cake thus obtained generally contains 1 to 2% residual oil for 10 to 12% moisture. 1.2. maltodextrin
    Maltodextrin is of the brand Glucidex® 1 (DE <6%) from Roquette®. This maltodextrin is in the form of a white powder with a maximum moisture content of 6% by weight. 1.3. Silicone
    Silicone is a polydimethyl siloxane-based polymer supplied by Evonik® (Germany), namely Tegostab B8460 (polyether-polydimethyl siloxane copolymer). 1.4. Water Water is demineralized water. However, tap water could be used. Indeed, a test was carried out with tap water and no effect was observed on the properties of the compositions, compared to a test using demineralised water. 2. Method 2.1. Grinding rapeseed cake
    The rapeseed cake supplied by Saipol was crushed using an 11 kW ATTRIMILL (Poittemill) mill which allowed flow rates between 10 and 300 kg / h of fine particles. The flow obtained with the mill is the result of a regulation activating the feed screw of the mill according to the intensity consumed. The screw is in operation until the power consumption of the crusher exceeds the limit of 19 Ampere (A). Once this limit is exceeded, the screw stops automatically, and restarts as soon as the amperage goes below the limit of 18 A. This system of "ping pong" lasts as long as there is product in the feed hopper of the grinder. This mill is equipped with a dynamic cyclone allowing a particle size classification and a selection of particles according to their size.
    In practice, the adjustments made are as follows: o milling speed of 4880 revolutions / minute, o dynamic cyclone at 10 Hz.
    During grinding, it was ensured that the heating of the cake was limited. For this, the outlet air temperature of the mill filter has been controlled so that it does not exceed 60 ° C. Air passing through the mill was drawn from the test hall at a temperature of 20 ° C throughout the milling period. The plant (mill and cyclone) was cleaned between each grinding.
    The yield of this operation (grinding and cyclone) is greater than 99%.
    The obtained rapeseed meal then has the following particle size distribution profile: D50 (median volume diameter) <40pm D99 <140pm.
    More particularly, the grinding and the selection of the particles by cyclone of the cake are intended to obtain a granulometric profile shown in FIG. 1. The grinding step described above may, optionally, be preceded by a step of pre-grinding the cake. at a coarse grain size having a median volume diameter D50 of about 250 to 450 μm. This pre-grinding is followed by a sieving step (or blotting) at a diameter corresponding to the D50 to separate the fines having a diameter smaller than the refusal diameter (ie particles with a diameter greater than D50). This upstream process makes it possible to separate a protein-rich fraction (ie particles with a diameter less than D50) from a protein-depleted fraction (ie particles with a diameter greater than D50). Other particle selection technologies can also be applied. For example, dry fractionation such as tribo-separation or wet such as precipitation in a solvent under given physicochemical conditions can also be carried out. 2.2. Measurement of particle size of rapeseed meal particles obtained
    The median volume diameter D50 of the rapeseed cake obtained at the end of the milling step was measured in the dry state. The particle size of the milled rapeseed meal particles was characterized using a HELOS type WINDOX 5 laser granulometer. The measurement range is 0.5 to 875pm.
    The characteristics of the grain size measurement are as follows: o Feed rate of 50%, o Measuring cycle of 100 ms, o Pressure of 1 bar. 3. Preparation of a composition according to the invention, by granulation
    The crushed cake is incorporated at room temperature in a De Dietrich blender with a jacket and spray system. This mixer is stirred at 140 rpm.
    A solution of maltodextrin in water at 10% by dry weight of maltodextrin on the total weight of water and maltodextrin (ie 11.11% of maltodextrin by dry weight on the total weight of water) is prepared with stirring. mechanically using a four-blade helix (about 400 rpm) in about 1 minute.
    The silicone is added to the aqueous solution of maltodextrin at a content of 55% by dry weight on the total weight of water and maltodextrin (ie 61.11% of silicone by dry weight on the total weight of water).
    The solution containing the maltodextrin and the silicone is then tempered preferably at a temperature between 45 and 51 ° C to ensure better solubilization, then pumped and sprayed into the stirrer at atmospheric pressure. The vacuum is then applied to the stirred mixer and reached in two to three minutes (70-100 mmHg). Then, the set temperature of the double jacket of the mixer is gradually raised to 60 ° C. The test is terminated when the moisture content of the powder is between 3 and 6% by weight (corresponding to a temperature of the powder between 52 and 57 ° C). The water content is monitored during the drying process. A maximum water content of the 6% granulated cake was chosen to maintain the specification given for that of maltodextrin alone.
    The granulate thus obtained can be easily suspended in water. To facilitate this suspension, the granulate can undergo a sieving operation, for example at 250pm, prior to its introduction into the water.
    Example 2 Preparation of a Composition According to the Invention and Comparative Compositions 1. Materials 1.1. oilcake
    The rapeseed meal used in this example is identical to that of Example 1. 1.2. maltodextrin
    Maltodextrin is that described in Example 1. 1.3. Silicone
    Silicone is the polydimethyl siloxane-based polymer described in Example 1. 1.4. Water The water is that described in Example 1. 1.5. Petrochemical resins
    The resin used for the preparation of the adhesive composition is a urea-formaldehyde resin, DYNEA®, having a solids content of 65%. Three types of resins were tested: pMDI (polymethylene diphenyl 4,4'-diisocyanate, BAYER, purity of 99%), UF (Urea-Formol, DYNEA, dry extract of 65%) and PF (Phenol-Formol, DYNEA, PF molar ratio / hardener = 1.67, 100% solids). 1.6. Urea Urea is urea U5378 from Sigma Aldrich, USA. 1.7. Wax
    The wax used is the MS27 Hydrofugant supplied by ICABOIS. Its dry extract is 58%. 2. Method 2.1. Grinding rapeseed meal and measuring the particle size of rapeseed meal particles obtained
    The grinding of the rapeseed cake and the measurement of the particle size of the obtained rapeseed cake particles are carried out as indicated in Example 1. 2.2. Preparation of compositions
    The adhesive compositions were prepared at room temperature. Their mixing was carried out mechanically using a four-blade propeller at a variable speed of 400 to 1200 revolutions / minute. a) Composition according to the invention 4c (with maltodextrin and silicone)
    Urea and maltodextrin are added to water at respective concentrations of 1 g.L'1 and 57 g.L'1 then solubilized with stirring (about 400 rpm) in about 1 minute.
    Crushed rapeseed meal is then added to the water-urea-maltodextrin mixture in about 3 minutes by successive addition of small amounts, at a stirring rate ranging from 400 to 500 rpm depending on the increase in viscosity ( that is to say that at the time of adding a new quantity of crushed cake, the stirring speed is increased to 500 revolutions / min), until a homogeneous suspension is obtained. The amount of cake added by weight relative to the total weight of water and cake is 25% w / w.
    Then, the silicone is added at 500 rpm, 11% by weight relative to the total weight of ground cake.
    This suspension of milled cake in an aqueous medium is then mixed with a urea-formaldehyde resin, added continuously under very vigorous stirring (approximately 1200 revolutions / minute), to a quantity of 93.92 g per 100 g of adhesive composition, the weights being given in dry weight. Stirring is maintained for 2 to 3 minutes to thoroughly homogenize the mixture.
    The solids content of the adhesive composition is finally adjusted so that the viscosity of the adhesive formulation remains constant with respect to that measured on an adhesive formulation without cake. b) Comparative composition 4d (with silicone only)
    Urea is added to water at a concentration of about 1 g.L'1 and solubilized with stirring (about 400 revolutions / minute) in about 1 minute
    Crushed rapeseed cake is then added to the water-urea mixture in about 3 minutes by successive addition of small amounts, at a stirring rate ranging from 400 to 500 rpm as a function of the viscosity increase. that is to say that at the time of adding a new quantity of crushed cake, the stirring speed is increased to 500 revolutions / min), until a homogeneous suspension is obtained. The amount of cake added by weight relative to the total weight of water and cake is 25% w / w.
    Then, the silicone is added at 500 rpm, at an amount of 11% by dry weight relative to the total weight of cake. This suspension of the milled cake in an aqueous medium is then mixed with a urea-formaldehyde resin, added continuously under very vigorous stirring (about 1200 rpm), to a quantity of 94.01 g per 100 g of adhesive composition, the weights being indicated in dry weight. Stirring is maintained for 2 to 3 minutes to thoroughly homogenize the mixture.
    The solids content of the adhesive composition is finally adjusted so that the viscosity of the adhesive formulation remains constant with respect to that measured on an adhesive formulation without cake. c) Comparative composition 4th (with maltodextrin only)
    Urea and maltodextrin (DE <6) are added to water at respective concentrations of 1 gL -1 and 57 gL -1 and solubilized with stirring (about 400 rpm) in about 1 minute.
    Crushed rapeseed meal is then added to the water-urea-maltodextrin mixture in about 3 minutes by successive addition of small amounts, at a stirring rate ranging from 400 to 500 rpm depending on the increase in viscosity ( that is to say that at the time of adding a new quantity of crushed cake, the stirring speed is increased to 500 revolutions / min), until a homogeneous suspension is obtained. The amount of cake added by weight relative to the total weight of water and cake is 25% w / w.
    This suspension of cake milled in aqueous medium is then mixed with a urea-formaldehyde resin, added gradually with very vigorous stirring (about 1200 revolutions / minute). The quantity of resin added is 94.43 g per 100 g of adhesive composition, the weights being indicated in dry weight. Stirring is maintained for 2 to 3 minutes to thoroughly homogenize the mixture.
    The solids content of the adhesive composition is finally adjusted so that the viscosity of the adhesive formulation remains constant with respect to that measured on an adhesive formulation without cake. d) Comparative composition 4b (without maltodextrin or silicone)
    Urea is added to water at a concentration of about 1 g.L'1 and solubilized with stirring (about 400 rpm) in about 1 minute.
    Crushed rapeseed cake is then added to the water-urea mixture in about 3 minutes by successive addition of small amounts, at a stirring rate ranging from 400 to 500 rpm as a function of the viscosity increase. that is to say that at the time of adding a new quantity of crushed cake, the stirring speed is increased to 500 rpm), until a homogeneous suspension is obtained. The amount of cake added by weight relative to the total weight of water and cake is 25% w / w.
    This homogeneous suspension of ground cake in water is then mixed with a urea-formaldehyde resin, added gradually with very vigorous stirring (about 1200 revolutions / minute). The quantity of resin added is 89.35 g per 100 g of adhesive composition, the weights being indicated in dry weight. Stirring is maintained for 2 to 3 minutes to thoroughly homogenize the mixture.
    The solids content of the adhesive composition is finally adjusted so that the viscosity of the adhesive formulation remains constant with respect to that measured on an adhesive formulation without cake.
    When using this composition as an adhesive composition, wax is added to this composition. e) Summary table of compositions
    Table 1: Summary of compositions 4b to 4e expressed in percentage by dry weight of each ingredient on the total dry weight of composition. 2.3. Characterization of the compositions obtained The compositions 4b to 4e can be used as adhesive compositions and have been characterized by:
    The measurement of the dry extract using a halogenated balance (105 ° C, stabilization time of 20 seconds),
    Measurement of flow time using Elcometer 2215 Lory Viscosity Cup (non-standard test),
    The measurement of the freezing time by monitoring the evolution of the viscosity with Trombomat (test temperature 180 to 200 ° C., this temperature range corresponding to those used during the heat transition of a composite wood panel ). 3. Results
    The results of the viscosity measurements and the gel time of the compositions are shown in Table 2 below and in FIG.
    * Vcu: Viscous Coupling Unit
    Table 2: Viscosity and gel time of the compositions (without the wax for test 4b).
    As can be seen in Figure 2, the gel time of the adhesive composition is significantly reduced with the introduction of maltodextrin and little affected with the introduction of silicone. However, a synergistic effect of reducing the gel time of the composition is observed with the introduction of maltodextrin and silicone.
    Reduction of the gel time can result in premature pre-hardening of the resin. An expected benefit of this accelerated hardening of the resin is a limitation of the temperature drop encountered during the drying in temperature. This effect makes it possible in particular to reduce the filtration of the adhesive composition through the material coated with this composition, for example through the pores of the wood particles. The adhesive composition thus remains more on the surface, for example wood particles and can better ensure its role as a binder.
    Example 3: Preparation of chipboard
    Sintered wood panels were prepared on a laboratory scale from adhesive compositions prepared in a manner similar to that of Example 2. For reasons of dimensioning, the panels were prepared in a layer, based on chips. fine (corresponding to the inner layer of a conventional panel). 1. Material 1.1. Adhesive compositions
    The adhesive compositions 1c to 1f used in this Example are prepared in identical ways to the compositions 4b to 4e respectively, prepared in Example 2.
    Compositions 1a and 1b are prepared from UF resin and optionally water and milled rapeseed cake as described in the material of Example 2. The preparation of these compositions is more fully detailed below. 1.2. Particles of wood
    The particles (in this case, chips) of fine wood come from Kronofrance. 2. Method 2.1. Preparation of the composition 1 a
    UF resin is mixed with wood chips. To do this, it is usually sprayed on the wood chips in a mixer. However, during these tests, the resin was manually mixed with the wood chips.
    When using this composition as an adhesive composition, wax is added to this composition. This addition is done manually after mixing the resin and wood chips. 2.2. Preparation of the composition 1b
    Crushed rapeseed meal is added to water in about 3 minutes by successive addition of small amounts, at a stirring rate ranging from 400 to 500 rpm as a function of the increase in viscosity (ie that is, when adding a new quantity of ground cake, the stirring speed is increased to 500 rpm), until a homogeneous suspension is obtained. The amount of cake added by weight relative to the total weight of water and cake is 25% w / w.
    This suspension of cake milled in aqueous medium is then mixed with a urea-formaldehyde resin, added gradually with very vigorous stirring (about 1200 revolutions / minute). Stirring is maintained for 2 to 3 minutes to thoroughly homogenize the mixture.
    The solids content of the adhesive composition is finally adjusted so that the viscosity of the adhesive formulation remains constant with respect to that measured on an adhesive formulation without cake.
    When using this composition as an adhesive composition, wax is added to this composition. This addition is done manually after mixing the resin and wood chips. 2.3. Summary table of the adhesive compositions 1 to 1
    Table 3: Summary of adhesive compositions 1 to 1 f expressed as a percentage by dry weight of each ingredient on the total dry weight of composition.
    2.4. Characterization of the compositions obtained The adhesive compositions 1a to 1f were characterized by:
    The measure of the dry extract,
    Measuring a flow time,
    The measurement of the freezing time, as described in Example 2. 2.5. Steaming wood chips The oven used is a conventional oven with ventilation.
    The chips are placed in an oven at 60¾ in aluminum trays with a capacity of about 100 g (which facilitates the placement of chips in the oven). They are left at least 6 hours at this temperature. The dry extract of chips used for wood panels composition is 97% (measured on a dry-matter scale).
    The chips are left in the oven until use. They came out of the oven shortly before the completion of the wood panel (about 10 to 15 minutes, maximum to avoid a recovery in moisture of the particles, and which correspond to the cooling time). 2.6. Preparation of the chipboards The panels were prepared as follows: (i) Manual mixing of the wood chips (after cooling after leaving the oven) with one of the adhesive compositions 1a to 1f at a temperature from 30 to 35 ° C and for 2 minutes; (ii) For the adhesive compositions 1a to 1c, adding the wax to the mixture obtained in step (i) and manual mixing for 1 min; (iii) Incorporation of the mixtures obtained in steps (i) (mixing from the adhesive compositions 1 d to 1 f) and (ii) (mixing from the adhesive compositions 1a to 1c) in a mold whose dimensions were calculated in order to to be able to fix the density of the panel at 650kg / m3 (the panels obtained measure approximately 250 x 350 mm2 for a final thickness of 7-8 mm); (iv) Incorporation of the molds containing the mixtures in an MI41 press from TechniHispania at 200 ° C. for 4 minutes. 2.7. Summary table of wood panels obtained from adhesive compositions 1 to 1
    *% by dry weight relative to the total dry weight of the chipboard
    Table 4: Summary of the compositions of the wood panels obtained from the adhesive compositions 1 to 1 2.8. Characterization of chipboards The chipboard panels are characterized by two parameters:
    The swelling with water: the measurement of swelling in thickness of the wood panel after total immersion in water (according to standard NF EN 317) is carried out at ambient temperature, the measurements of the thickness being carried out at tO, t + 2h, t + 24h, on average on 3 test tubes,
    The mechanical resistance: the measurement is carried out by a 3-point bending test to evaluate the maximum stress, and the bending modulus (MPa) This measurement is inspired by the NF EN 310 standard and is performed on MTS Criterion type traction machine (model43), with a 2 kN sensor, a test speed of 2 mm / min, averaged over 5 test pieces.
    The standards as indicated in this application are those in effect on the filing date. 3. Results 3.1. Results on the adhesive compositions The results of the viscosity measurements and the gel time of the compositions are shown in Table 5 below.
    * Vcu: Viscous Coupling Unit
    Table 5: Viscosity and gel time of adhesive compositions 1 to 1 (without the wax for tests a, b and c).
    The gel time of the adhesive composition is: significantly reduced with the introduction of cake and maltodextrin, and little affected with the introduction of urea.
    A synergistic effect of reducing the gel time of the composition is also observed with the introduction of maltodextrin and silicone. 3.2. Results on chipboard The results in terms of water swelling and strength are shown in Table 6 below and in Figure 3.
    Table 6: Mechanical properties and water resistance of chipboard prepared using adhesive compositions 1a to 1f
    The mechanical properties of the chipboard are significantly improved when it is prepared with the adhesive composition 1d, that is with the adhesive composition comprising in combination a maltodextrin and a silicone, namely maltodextrin and a siloxane, respectively.
    Indeed, as can be seen in Figure 3A, the stress resistance is the best for the wood panel prepared with a composition comprising both ground rapeseed cake, urea, maltodextrin and a siloxane.
    It is more particularly noted that the addition of cake and, to a lesser extent, the addition of urea significantly increase the resistance to stress, while the addition of maltodextrin or siloxane alone slightly reduces this resistance.
    However, unexpectedly, the combined addition of maltodextrin and siloxane significantly increases the stress resistance.
    Regarding the swelling with water, as can be seen in Figure 3B, the addition of cake significantly degrades the resistance of the wood panel swelling when immersed in water. This degradation is totally offset by the addition of urea. However, the addition of maltodextrin or siloxane
    each causes a very slight increase in the rate of swelling with water while, unexpectedly, the combined addition of maltodextrin and siloxane makes it possible to reduce this rate of swelling. The best result in terms of resistance to water swelling is thus obtained with an agglomerated wood panel prepared with a composition comprising both ground rapeseed cake, urea, maltodextrin and a siloxane.
    EXAMPLE 4 Effect of the Chemical Nature of Silicone on the Properties of the Chipboard 1. Material 1.1. Silicone
    Two polymers based on polydimethyl siloxane were tested, both provided by Evonik (Germany):
    Tegostab B8460: polyether-polydimethyl siloxane copolymer, and
    Tegoprotect 5000: polydimethyl siloxane functionalized hydroxy. 1.2. Adhesive compositions
    The adhesive compositions 3a and 3b used in this Example are prepared identically to the composition 4c of Example 2, the only difference between the compositions 3a and 3b being the nature of the silicone introduced into the composition. 1.3. Wood panels
    The chipboard is prepared as in Example 3. 1.4. Summary table of wood panels obtained from adhesive compositions 3a and 3b
    *% by dry weight relative to the total dry weight of the chipboard
    Table 7: Summary of the compositions of the wood panels obtained from the adhesive compositions 3a and 3b 2. Method 2.1. Characterization of the compositions obtained
    The adhesive compositions 3a and 3b have been characterized by:
    The measure of the dry extract,
    Measuring a flow time,
    The measurement of the freezing time, as described in Example 2. 2.2. Characterization of chipboard
    Sintered wood panels are characterized by two parameters:
    Swelling with water,
    Mechanical strength, as described in Example 3. 3. Results 3.1. Results on the adhesive compositions The results of the viscosity measurements and the gel time of the compositions are shown in Table 8 below.
    * Vcu: Viscous Coupling Unit
    Table 8: Viscosity and gel time of the adhesive compositions 3a and 3b 3.3. Results on chipboard
    The results in terms of water swelling and mechanical strength are shown in Table 9 below and in Figure 4.
    Table 9: Mechanical properties and water resistance of chipboard prepared using adhesive compositions 3a and 3b
    As can be seen in Figure 4A, the mechanical properties of the chipboard obtained with the two surfactants are similar. In contrast, the water resistance of the chipboard is improved when the wood panel is prepared with an adhesive composition comprising Tegostab B8460 relative to a wood panel is prepared with an adhesive composition comprising Tegoprotect 5000. However , the water resistance of the latter remains within the acceptable upper limit.
    权利要求:
    Claims (14)
    [1" id="c-fr-0001]
    A composition comprising: a crushed plant containing at least 3% protein, maltodextrin, and silicone.
    [2" id="c-fr-0002]
    2. Composition according to claim 1, wherein the amount of maltodextrin in the composition is between 0.1 and 20% by dry weight on the total dry weight of ground vegetable.
    [3" id="c-fr-0003]
    3. Composition according to one of claims 1 or 2, wherein the amount of silicone in the composition is between 0.5 and 30% by dry weight on the total dry weight of ground vegetable.
    [4" id="c-fr-0004]
    4. Composition according to any one of claims 1 to 3, wherein the crushed plant is one or more crushed plant meal (s) selected (s) from the group consisting of rapeseed, canola, sunflower cake , soy, cotton, flax, walnuts, olive, mustard, hemp, carnation, corn germ, rape, safflower, shea, sesame, castor oil, camelina, jatropha, peanut, oil palm, hazelnut, almond and copra kernels.
    [5" id="c-fr-0005]
    5. Composition according to any one of claims 1 to 3, wherein the crushed plant is obtained by grinding fruit and / or seeds of protein crops selected from the group consisting of pea, faba bean, lupine, lentils, fenugreek and beans.
    [6" id="c-fr-0006]
    6. A composition according to any one of claims 1 to 4, wherein the crushed plant cake is in the form of a powder having a median volume diameter D50 of between 1 and 250 μm.
    [7" id="c-fr-0007]
    7. Composition according to any one of claims 1 to 6, in the form of granules.
    [8" id="c-fr-0008]
    8. Process for the preparation of a composition according to one of claims 1 to 7 comprising the following steps: (i) the grinding of seeds and / or fruits of oleaginous and / or proteinaceous plants, (ii) the addition of maltodextrin and silicone milled plant obtained in step (i).
    [9" id="c-fr-0009]
    9. Preparation process according to claim 8, wherein the addition of maltodextrin and silicone carried out in step (ii) is carried out by the preparation of at least one aqueous solution comprising maltodextrin and / or silicone.
    [10" id="c-fr-0010]
    10. Preparation process according to claim 9, wherein the aqueous solution is sprayed on the ground material obtained in step (i).
    [11" id="c-fr-0011]
    11. Preparation process according to claim 9, wherein the ground material obtained in step (i) is suspended in the aqueous solution.
    [12" id="c-fr-0012]
    12. Adhesive composition comprising a composition according to one of claims 1 to 7, and one or more precursors of a resin selected from the group consisting of polymethylene diphenyl 4,4'-diisocyanate, urea-formaldehyde, phenol -formaldehyde and / or melamine-urea-formaldehyde.
    [13" id="c-fr-0013]
    An article comprising an adhesive composition according to claim 12 and a lignocellulosic material.
    [14" id="c-fr-0014]
    14. Use of a composition according to one of claims 1 to 7 for the preparation of an adhesive composition, a polyurethane foam, a cosmetic composition, a phytosanitary composition or a food composition.
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    同族专利:
    公开号 | 公开日
    FR3041966B1|2019-07-05|
    WO2017055557A1|2017-04-06|
    引用文献:
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    WO1998019652A1|1996-11-06|1998-05-14|The Boots Company Plc|Spray-dryed powder comprising at least one protein and one hydrolysed starch and its use for topical compositions|
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    WO2002045512A2|2000-12-05|2002-06-13|S.I.P.C.A.M. Societa' Italiana Prodotti Chimici E Per L'agricoltura Milano S.P.A.|Polyphosphate microbicide for pre- and postharvest crop protecion|
    US20090098387A1|2007-10-09|2009-04-16|Hercules Incorporated|Diluents for crosslinker-containing adhesive compositions|
    US20120247993A1|2008-11-14|2012-10-04|Unistraw Patent Holdings Limited|Probiotic Compositions, Methods and Apparatus for Their Administration|
    US20130224482A1|2012-02-27|2013-08-29|Hercules Incorporated|Diluents for crosslinker-containing adhesive compositions|
    EP2842607A1|2013-09-02|2015-03-04|Symrise AG|A skin and/or hair whitening mixture|
    CN109825247A|2019-03-07|2019-05-31|河南工业大学|A kind of composite modified sesame protein adhesive and preparation method thereof|
    IT201900011805A1|2019-07-15|2021-01-15|Agroils Tech S P A|FORMALDEHYDE-FREE BINDING COMPOUNDS AND METHODS FOR PRODUCING THEM|
    WO2021009210A1|2019-07-15|2021-01-21|Agroils Technologies S.P.A.|Formaldehyde-free binders and methods for producing the same|
    IT201900014370A1|2019-08-08|2021-02-08|Agroils Tech S P A|FORMALDEHYDE-FREE BINDING COMPOUNDS AND METHODS FOR PRODUCING THEM|
    法律状态:
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    2017-12-01| TP| Transmission of property|Owner name: EVERTREE, FR Effective date: 20171025 |
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    2021-10-29| PLFP| Fee payment|Year of fee payment: 7 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1559347A|FR3041966B1|2015-10-01|2015-10-01|COMPOSITION COMPRISING A PLANT BROYA, MALTODEXTRIN AND SILICONE|
    FR1559347|2015-10-01|FR1559347A| FR3041966B1|2015-10-01|2015-10-01|COMPOSITION COMPRISING A PLANT BROYA, MALTODEXTRIN AND SILICONE|
    PCT/EP2016/073431| WO2017055557A1|2015-10-01|2016-09-30|Composition comprising ground plants, maltodextrin and silicone|
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