• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    L'invention concerne la préparation de suspensions ou de poudres stables de microcapsules stables et d'une porosité variable, contenant au moins une matière active, préparation comprenant les stades de préparation d'une émulsion "huile dans l'eau" à partir de gélatine colloidale et de gomme d'acacia et d'une émulsion, solution ou dispersion huileuse de la matière active, de coacervation et microencapsulation des gouttellettes émulsionnées, de réticulation des parois des microcapsules puis de formulation, préparation caractérisée en ce que l'on ajoute à l'émulsion "huile dans l'eau" une quantitité variable d'éthyl hydroxyéthylcellulose organosoluble, l'on fait agir après coacervation de l'aldéhyde glutarique et du tanin, l'on additionne d'éthyl hydroxyéthylcellulose hydrosoluble ou d'un véhicule solide, pour obtenir une suspension ou une poudre. L'invention concerne également les suspensions ou poudres ainsi obtenues.
    公开号:SU1655294A3
    申请号:SU802969269
    申请日:1980-08-29
    公开日:1991-06-07
    发明作者:Сюглиа Жан-Клод；Мейнар Коллетт
    申请人:Руссель-Юклаф (Фирма)；
    IPC主号:
    专利说明:


    cm
    You will relate to the technology of producing microcapsules containing an active substance that can affect the environment.
    The purpose of the invention is to change the duration of the prolongation.
    Example 1. Preparation of an aqueous suspension of microcapsules of weak porosity containing (S) pЈ-cyano 3-phenoxybenzyl ester 1 R, cis-2,2-dimethyl 3- (2,2-dibromovinyl) cyclopropane-1-carboxylic acid or decamet - rin (product A).
    20 g of gelatin and 20 g of acacia gum in 760 ml of desalinated water in the presence of 0.5 g of secondary octanol are stirred at 500 rpm at 50 ° C. Get the first solution (I).
    A second solution (II) is prepared, stirring at 500 rpm at 50 ° C / 15 g of compound A, 46.4 g of xylene, 96.6 g of dimethyl phthalate, 4.0 g of secondary octanol, 6.5 g of water soluble ethylhydroxyethylcellulose (NES) (16.25% of the total mass of gelatin and acacia gum), 0.8 g of anionic surfactant based on alkylaryl sulfonate — gahoryl EM 520, and 0.2 g g. mariel EM 60 — an oxide condensation product ethylene with a hydroxyl-containing polyester.
    Prepare emulsion oil in water, slowly add solution II to solution I at a stirring speed of 500 rpm and 50 ° C.
    j
    The resulting emulsion thus contains 2.51% by weight of compound A and 4.02% by weight of colloid-gelatin and acacia gum.
    When the oil-in-water emulsion is obtained, the pH of the reaction medium is adjusted to 4.2-4.4 by adding a 10% acetic acid solution, and then the temperature is slowly reduced to 20 ° C over about 1 hour.
    Then 5 ml of a 25% glutaraldehyde solution are added with stirring (500 rpm). Then, also with stirring at a speed of 500 rpm, after about 1 hour, 10 g of a 15% aqueous solution of tannin is added.
    The reaction mixture with stirring at a speed of 500 rpm is maintained at room temperature for 3 hours (approximately). Thus, microcapsules with a cross-linked structure are obtained, the diameter of which is not less than 30 microns
    To the resulting emulsion of crosslinked microcapsules, 1 g is successively added.
    five
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    five
    secondary octanol, 119 g of calcium chloride (in small fractions, or 11.95% by weight based on the mass of the microcapsule emulsion), 10 g of water-soluble ethylhydroxyethylcellulose (or 1% by weight of the amount of the microcapsule emulsion), 12 g Galoryl EM 42 and 0 , 04 g Rhodamine B, and then continue stirring for about 3 h and pass the resulting suspension through a sieve. This suspension contains 98.1% of the original active ingredient.
    PRI me R 2 (comparative). Preparation of an aqueous suspension of microcapsules with strong porosity containing compound A.
    The method is carried out as in Example 1, using the same amounts of components, but without using water-insoluble ethyl hydroxyethylcellulose in fl solution, a suspension of microcapsules is obtained, which have an increased porosity. This suspension contains 98.7% of the original active ingredient.
    PRI me R 3. Preparation of powder on the basis of microcapsules.
    The microcapsules obtained in examples 1 and 2 can also be isolated as a powder. In order to obtain such a powder, with stirring at 500 rpm, they are added to the total reaction mixture obtained after forming the crosslinked structure of the coacervate of Example 1 or 2, 110 g (or 11.05% by weight of the microcapsule emulsion) of talc , maintain stirring for about 15 minutes, pass the suspension through a sieve, suction the microcapsules and dry.
    The resulting powder can then be conditioned by conventional methods, for example, in the form of baits.
    PRI me R 4. Obtaining powder on the basis of microcapsules containing the virus Heliothis Nuclear Polyhedrosis.
    Under stirring at a speed of 500 rpm at 50 ° C, a first solution is prepared from 20 g of gelatin and 20 g of acacia gum in 760 ml of desalted water.
    Prepare a second solution (II) with stirring at 500 rpm, starting with 25 g of Heliothis Nuclear Polyhedrosis virus powder, 46.4 g of xylene, 96.6 g of dimethyl phthalate, 0.8 g of Galoril EM 520 and 0.2 g Galorila EM 60.
    An oil-in-water emulsion is prepared, slowly introducing solution II into solution I with stirring (500 rpm, 50 ° C).
    After an oil-in-water emulsion is obtained, the pH of the reaction medium is adjusted to 4.2-4.4 by the addition of a 10% acetic acid solution, and then the temperature is reduced to 20 ° C over about 1 hour.
    Then, at a stirring speed of 500 rpm, 5 ml of a 25% glutaraldehyde solution is added. After about 1 hour, with constant stirring at 500 rpm, 10 g of a 15% aqueous solution of tannin is added. The reaction mixture is kept under stirring at 500 rpm at room temperature for 3 hours (approximately). In this way, cross-linked microcapsules are obtained with a diameter of 30 jti (maximum).
    ten
    roval paper. An equivalent amount of non-micronized encapsulated naphthalene is placed as a control. The study is conducted in the dark, with an average relative humidity of 60%, in a stream of air at a speed of 143 m3 / h.
    Naphthalene sublimate determination is carried out on a chromatography apparatus in the vapor phase and after 24 hours, 7 and 28 days.
    Naphthalene, which is not microencapsulated, turned out to be completely sublimated after
    h, while micro15 capsules of samples A, B, and C gave lost naphthalene depending on the time and amount of organic soluble hydroxyethylcellulose (CNPC) present. in the walls of microcapsules (see tab. 2). 20 Based on these measurements, it can be determined that the difference in porosity of the microcapsules depends on the concentration of EHEC in the walls.
    So, changing the concentration of the organo. After the formation of crosslinked microcapsules of soluble ethyl hydroxyethylcellulose, is added with stirring at a speed of 500 rpm to the total reaction mixture obtained after forming the crosslinked structure of the coacervate,
    content in the microcapsule to control the porosity from the microcapsule, depending on the encapsulated active
    110 g of talcum powder (or 11.17% of the mass of the substance and of its use.
    microcapsules), keep stirring for 15 minutes (approximately) pass the suspension through a sieve, suction the microcapsules and dry them.
    The resulting seaweed can then be conditioned by conventional methods, for example, in the form of bait.
    The proposed method provides microencapsulation of the virus without destroying it.
    Froze The study of the porosity of the microcapsules obtained by the proposed method.
    To study the porosity of microcapsules, they were prepared according to the method described in examples 1 and 2, but they chose naphthalene as the microencapsulating substance, and not compound A.
    The concentration of organic-soluble ethylhydroethylcellulose solution I varies depending on the test (see Table 1).
    1i) 0 mg of the obtained microcapsules containing naphthalene, taken from samples A, B and C, are collected in filter cups. Figure 6 is the study against light radiation baked by microcapsules (prepared by the proposed method)
    to him the substance.
    Photosensitive compound, for example, 5-benzyl-3-furylmethyl ether (1R, 3S, E) 2,2-dimethyl-3 oxo-2,3,4,5-terahydro-3-thiophe
    40 idenmethyl) cyclopropanecarboxylic lots or cadetrin (the compound is microencapsulated and the microcaps are introduced into the suspension according to the previous method. This suspension and
    A 45 doped concentrate based on the same photosensitive compound and at the same concentration is subjected to the same effect reproducing solar radiation.
    50 range. The average temperature and humidity are corresponding to 25 ° C and 75%.
    55
    The determination of the activity loss (compound B) was made after 24 hours, 7 and 14 days of expiration under illumination and by means of chromatography in liquid pressure and high pressure.
    roval paper. An equivalent amount of non-micronized encapsulated naphthalene is placed as a control. The study is conducted in the dark, with an average relative humidity of 60%, in a stream of air at a speed of 143 m3 / h.
    Naphthalene sublimate determination is carried out on a chromatographic apparatus in the vapor phase and after 24 hours, 7 and 28 days.
    Naphthalene, which is not microencapsulated, turned out to be completely sublimated after
    h, while microcapsules of samples A, B, and C gave lost naphthalene depending on the time and amount of organic soluble hydroxyethylcellulose (CNPC) present. in the walls of microcapsules (see tab. 2). Based on these proo can be established that the difference in porosity of the microcapsules depends on the concentration of EHEC in the walls.
    So, by changing the concentration of organose in microcapsules, the porosity of the microcapsule walls can be controlled depending on the nature of the active veggie encapsulated II Figure 6: Study of protection against light radiation provided by the microcapsules (prepared by the proposed method) to the active substance.
    A photosensitive compound, such as (1R, 3S, E) 5-benzyl-3-furylmethyl ester (2,2-dimethyl-3- (2-oxo-2,3,4,5-terahydro-3-thiophenylidenemethyl) cyclopropanecarboxylic acid or cadetrin (compound B), microencapsulated and microcapsules are introduced into the suspension according to the previous method. This suspension and emulsifiable concentrate based on the same photosensitive compound and at the same concentration are subjected to the same illumination reproducing the sun.
    spectrum. The average temperature and relative humidity are respectively 25 ° С and 75%.
    The losses of the active substance (Compound B) were determined after 24 hours, 7 and 14 days of operation under illumination and by means of a chromatography apparatus in the liquid phase at high pressure.
    The results of these tests are given in table. 3
    These results prove the effectiveness of protecting the microencapsulated active substance.
    Example 7. The study of the preservation of the biological activity of micro-encapsulated active substance
    Compound A (decamethrin) is micro-encapsulated and injected into suspension or conditioned as granules, starting from the powder of these microcapsules. This suspension and these granules are compared with an emulsifiable concentrate based on this product A at the same concentration.
    The study of the biological activity of the suspension of microcapsules and emulsifiable concentrate.
    The insect used for this biological sample is SPODOP-TERA LITTORALIS. The microcapsule suspension and the emulsifiable concentrate are diluted with water, then both diluted aqueous solutions containing product A are sprayed in an amount of 1) ml per. 4 seedlings of beans (3 leaves). 20 caterpillars (stage L4) are planted on each sapling after 0.3.5.7 and 14 days after treatment. Controls are performed 24 and 48 hours after invasion. The results are shown in Table. 6
    .Dan table. 6 show that the emulsifiable concentrate shows a marked decrease in activity after the 3rd day, while the suspension of microcapsules still has some activity after the 4th day.
    Investigation of the biological activity of a microencapsulated substance and then conditioned as bait in granules.
    These baits in the form of granules are obtained from individual microcapsules that are in powder form and contain product A as the active substance.
    They are scattered on the ground for protecting lettuce from the invasion of caterpillars (SPODOPTERA LITTORALIS). It has been previously found that product A, introduced directly into bait, without microencapsulation, deteriorates very quickly and quickly loses its biological activity.
    The cultivated area contains twenty lettuce in a stage of 2-3 leaves, transplanted in 4 lines.
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    20 caterpillars are put on the ground. Control is carried out 19 days after infection. The results of the control are given in table. four.
    The consequence of two types of microcapsules.
    Insect test: caterpillars of Spodoptera littoralis (4th stage: 1.5-1 cm).
    Processing method: direct spraying.
    The amount of solution used: 10 ml of aqueous toxic solution for 5 cotton plants.
    Processed base: 4 cotton plants.
    Infection: day 0, day 1, day 2, day 3, day 4, day 5, day 6 with the help of 20 individuals.
    Control: 24 and 48 hours after infection.
    Doses MA, g / l: 0.1 g MA / l.
    The results are shown in Table. five.
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    The method of obtaining microcapsules by preparing an oil-in-water emulsion when mixed at a speed of 500 rpm and at 50 ° C a solution containing 2.51% of the total mass of the emulsion of the biologically active substance as a core material and an organic solvent, with an aqueous solution containing 4, 02% of the total mass of the emulsion of colloid - gelatin and acacia gum at an equal ratio, in the presence of an emulsifier, lowering the pH of the reaction medium to 4.2-4.4 and temperature to 20 ° C for 1 hour while maintaining the same stirring speed and stitched shell mic capsules, characterized in that, in order to regulate the prolongation of the action of the biologically active substance, 0.4% of the total mass of the emulsion of secondary octyl alcohol is used as an emulsifier in the presence of a mixture of an alkyl aryl sulfonate anionic surfactant with a non-ionic surfactant on the basis of the condensation product of ethylene oxide with a hydroxyl-containing polyester, 5.0–16.25% of the weight of the colloid of water-insoluble ethyloxyethylcellulose is additionally introduced into the emulsion, shivka is performed sequentially
    processing the microcapsules, 25% glutaraldehyde solution for 1 hour and an aqueous solution of tannin for 3 hours with stirring at 500 rpm, then 11.95% by weight are added to the resulting emulsion of crosslinked microcapsules with variable porosity
    Orgon-soluble ethylhydroxyethylcellulose
    Compound
    Naphthalene non-microcapsulated Microcapsules with 0% EHEC Microcapsules with 5% EHEC Microcapsules with 10% EHE
    emulsions of calcium chloride and 1% water-soluble ethyl hydroxyethyl cellulose to obtain a suspension of microcapsules or 11.17–11.65% by weight of talc emulsion with slow mixing at 7.0 ° C, followed by drying and separation of the powder of microcapsules. I Table 1
    ten
    Table 2
    Sublimation%, in terms, days
    1 (7.4 h) 1
    28
    100
    28
    thirty
    sixteen
    22
    24
    Table3
    10 10
    95 1:10 90 9 (1 75 80 65 140 100 5 15 5 5 П
    Table4
    T a b l and c a 6
    30 5
    45
    YU
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    同族专利:
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR7921743A|FR2464093B1|1979-08-30|1979-08-30|
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