专利摘要:
1499989 Surface active material TATE & LYLE Ltd 30 Sept 1975 [17 Oct 1974 18 April 1975] 45122/74 and 16222/75 Addition to 1399053 Heading C2C A process for the preparation of a surface active material comprises the reaction of solid particulate sucrose with at least one (C 1 -C 6 ) alkyl ester of a (#8 C) fatty acid in the presence of a basic esterification catalyst, e.g. an alkali metal carbonate or alkoxide, at a temperature of from 110‹ to 140‹ C. at atmospheric pressure and in the absence of any solvent. The reaction is preferably performed with high-shear mixing and in the presence of a surfactant.
公开号:SU906383A3
申请号:SU752184053
申请日:1975-10-17
公开日:1982-02-15
发明作者:Джеймс Кеннет
申请人:Тейт Энд Лайл Лимитед (Инофирма);
IPC主号:
专利说明:

3906 using the solvent, since the use of vacuum is considered an essential condition, taking into account that the equilibrium in the transesterification reaction does not favor the formation of ester sucrose and goes in the right direction with careful removal of the alcohol by-product. It was quite unexpectedly established that carrying out the process of transesterification under atmospheric pressure leads to an increase in the yield of the target product. Lower alkyl esters of fatty acids with 8 carbon atoms, in particular about 10-22, and more, in particular, preferably 16-18 carbon atoms, can be used in the proposed process. It is advisable to use methyl eOirs. It is usually convenient to use lower alkyl esters obtained from naturally occurring mixtures of triglycerides, for example methyl talloate, which includes methyl esters of stearic, palmitic and oleic acids, but lower alkyl esters derived from other triglycerides of fats and oils, such as porcine, can be used. lard, palm oil, cottonseed oil, soybean, olive, peanut oil, cottonseed, castor and linseed oil. However, it is usually less desirable to use lower alkyl esters of highly unsaturated fatty acids, for example, those obtained from so-called drying oils, such as linseed oil, because they can be oxidized and discolored during the proposed process and the product has relatively worse surface-active properties, it is generally preferred to use lower alkyl esters of acids containing no more than one double bond. The presence of a hydroxyl group in the acid chain may also harm the surface-active properties of the product. Figure 1 shows the composition of some fat triglycerides and fatty acid names from which they are derived and the number of carbon atoms in the acid chain, from which the corresponding lower alkyl esters (formed and suitable for use in this process, k) can also be used for ethyl and programme or butyl esters. Lower alkyl ester and sucrose are conveniently used in ec3 of vimopry quantities, although these proportions are not critical. The catalyst used in the process may be any alkaline compound commonly used as a transesterification catalyst, but carbonates and alkali metal alkylates, such as potassium carbonate and sodium methoxide, have been found to have good results. Other basic compounds such as tertiary or quaternary organic bases, silicates and borates can also be used. The concentration of the catalyst is not critical, but it is usually desirable to use at least 2% of the catalyst in order to achieve a satisfactory reaction rate and thus obtain a surfactant in a relatively short period of time. The reaction can be accelerated by using a higher concentration of about., Preferably 10. In general, no additional benefit is achieved with a further increase in catalyst concentration, levels above 20 are not recommended for use in practice. (All percentage concentration by weight relative to the weight of the reaction mixture). In the process, the sucrose and alkaline catalyst can be added to the alkyl ester and the resulting suspension is heated with stirring, causing the transesterification reaction. Alternatively, the alkyl ester is first heated with only the catalyst, thus partially washed, and then sucrose is added to the reaction mixture in order to undergo transesterification. However, this initial saponification stage is usually not needed when using the PLV obtained by the proposed method. Hot not. no solvent is used in the proposed process, the reaction is carried out at a temperature significantly below the melting point of sucrose in the region near PO-YO C. The preferred temperature region is 120130 ° C and the reaction is most expediently carried out at (for all these values -retmeparyp are inside the reaction mixture. Usually the reaction takes place at a temperature below 110 ° C while charring occurs at a temperature higher and the product does not have satisfactory surface-active properties. The reaction mixture can be heated until needed In any usual way, for example, by equipping the reaction vessel with an external jacket through which steam 8 passes, in some cases, especially if energetic mixing of the reaction mixture is used, it may be necessary to cool the reaction mixture during the reaction in order to maintain the desired temperature, for example, by passing water through an outer jacket. The process is carried out at atmospheric pressure in a simple open reaction vessel equipped with suitable heating and stirring devices. You can use a suitable type of mixer with a motor, but in order to ensure uniform mixing and to maintain the temperature constantly throughout the reaction mixture, especially in a large vessel, it is sometimes desirable to use a high-speed stirrer that makes several thousand revolutions per minute. No special conditions are required for the isolation of alcohol intermediates. The sucrose used in the proposed process is usually in the form of refined sugar particles, such as cooked sugar. The sizes of the sucrose particles are not critical, but very large particles are difficult to evenly distribute in the reaction mixture and, therefore, sucrose with a particle size of less than 250 microns is better used. Sucrose can be ground and sieved before use so that the desired particle size is obtained, but if a high-grade stirrer is used to stir the reaction mixture, it also slowly crushes the sucrose particles. The duration of the reaction is protected by the nature of the alkyl ether, the amount and type of catalyst, the efficiency of mixing, and the reaction temperature used. The reaction is complete when the mixture becomes very viscous with uniform stirring. The reaction can be completed in 6 hours, but usually it takes more than 6 hours for the lady to get optimal surfactant yields. The progress of the reaction can be observed, for example, by subjecting the samples of the reaction mixture to chromatography at regular intervals. It is most expedient to carry out the process in the presence of PLV, in particular the surface-active product obtained by the proposed method from triglyceride. It is added in an amount of wt% based on the total weight of the reaction mixture. Other effective surfactants that can be added in the same amounts are diglycerides and monoglycerides, the former being more effective than the latter. Either, such as sodium stearate, is less effective for these purposes. These additives act as a physical catalyst in a heterogeneous solid liquid reaction system used in the proposed process. The use of a surfactant is thus very advantageous when the alkaline transesterification catalyst is used in low concentrations. If a small amount of surfactant, diglyceride or monoglyceride is added to the reaction mixture, the reaction time is significantly reduced. The main product contains a mono-ester of sucrose fatty acid together with unreacted starting and intermediate products. It has significant surface-active properties and can be used, in its crude form, as a biodegradable, non-toxic surfactant for many cleansing purposes. Most of the product consists of sucrose monoesters, which are extremely valuable as surfactants. The reaction product solidifies upon cooling and various compositions can be obtained from it, for example, mixed with suitable excipients and auxiliaries to obtain an f / cel powder composition. Formulations for other purposes, such as cosmetics, agricultural chemicals, and animal food, can be prepared in a known manner. No solvents are used in the proposed process, therefore the costly and complex stages of solvent recovery and product purification are completely eliminated. A mixture of g of methyl talloate, 17 g of sucrose, 5 g of potassium carbonate and 2.5 g of 79063 surfactant obtained from sucrose and solid fat is stirred for about 11 hours at. The resulting turbid, waxy product hardens into a fragile substance s when cooled. Yield 4 g. The product has good surface-active properties and contains ./ 30 wt.% Sucrose iono esters, with some diesters and higher esters, 3 Characteristics of surfactants obtained by the reaction of methylolate with sucrose using potassium carbonate as a catalyst, presented 8 table. 2. The use of various fatty acid complex alkyl esters in the reaction with sucrose in the presence of a potassium carbonate based catalyst is presented in Table 3,
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权利要求:
Claims (1)
[1]
906383 T Bleach "2 1590 Claim Method A method for producing a surfactant containing sucrose fatty acid nonoesters, diesters and higher complex, by reacting a mixture of particles and sucrose, alkyl complex) 0 ,. fatty acid having a carbon atom of l. a. alkyl radical and Q-22 carbon atom in the fatty acid radical, with the main transesterification catalyst at 110–140 ° C, which is so as to increase the yield of the target product The method is carried out at atmospheric pressure. Sources of information taken into account in the examination 1. Patent ША VP 3558597, cl. 260-23, pubic. 1971 (prototype)
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同族专利:
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引用文献:
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法律状态:
优先权:
申请号 | 申请日 | 专利标题
GB45122/74A|GB1499989A|1974-10-17|1974-10-17|Production of a surface active material containing sucrose esters|
GB1622275|1975-04-18|
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