Production of esters sorbitan and fatty acids as surfactants

 

(57) Abstract:

The invention relates to a method for producing esters of fatty acids and sorbitan and/or their alkoxysilane derivatives by reacting fatty acids directly with sorbitol in the presence of catalytic systems. The catalytic system comprises a phosphorus-containing hydroxy (Aha), including restoring the hydroxy acid and the strong base is an alkaline or alkaline-earth metal. The molar ratio of acid to base is 0.9:1 to 1.7:1. The concentration of the catalytic system is 1.5 - 30% by weight based on sorbitol. The method optionally includes the interaction of the obtained esters with alkalization. Effect: improved product quality and process simplification. 13 C.p. f-crystals, 2 tab.

The present invention relates to an improved method for producing a surface-active esters, mainly esters sorbitan and fatty acids, to use the target esters as surfactants for the production alkoxycarbonyl, mainly ethoxylated surfactant esters, in particular ethoxylated esters scachetti surface-active substances.

Esters sorbitan and fatty acids, selling various ICI companies under the trade mark "Span", are widely used as surfactants and as intermediate reactants in the production of relatively more hydrophilic surface-active substances alkoxycarbonyl, mainly ethoxycarbonyl Polysorbate surface-active substances, for example, available on the market various ICI companies under the trademark "Tween". Usually esters sorbitan and fatty acids belong to the large-scale production of products obtained by the reaction of sorbitol and fatty acids in the presence of a catalytic composition, promoting the reaction of the formation of ester, as well as catalyzing intramolecular ether rearrangement with the conversion of sorbitol in sorbitan. In most cases, the reaction of formation of simple ether is desirable only to obtain the monocyclic product, although it is possible to implement the second reaction internal simple esterification to obtain isosorbide balance. It is believed that the reaction of the internal simple esterification proceeds after the reaction receipt of ester, but it is insignificant at large is one of esterification and internal simple esterification different, products usually represent a mixture of isomers. The possibility of additional changes in the molecule occurs due to mnogotomnoi alcohol and the existence of a large number of complex reactions of esterification. Somerest molecules, probably well known to experts in the field of production and application of such surface-active substances.

In principle, the reaction of the formation of esters is acidic and basic catalysis, whereas the reaction of formation of simple ether is usually catalyzed by acids. Usually when getting esters sorbitan and fatty acids are used in catalytic systems comprising a mixture of acidic and basic catalysts. It is generally accepted that the base catalyzes the reaction of formation of esters, acid catalyzes a simple esterification. In the presence of the water system, as a result of either its receipt with aqueous solutions of reagents, or education in the reaction, as expected, the acid and base react with the formation of salts. This may mean that the actual catalyst is a salt or a mixture or acids or bases and salts. Usually the reaction temperature is approximately 240oWith, and catalysts using the conventional catalytic systems include NaOH as the base and phosphorus oxyacids as acid. Various phosphorus oxyacids can successfully be used as acid components of the catalytic system, but historically the preferred phosphorus-containing unfused to the hydroxy acid, such as phosphoric acid. Usually basic and acid components of the catalyst (for a typical system NaOH/phosphoric acid) used in a mass ratio of about 1:1, which corresponds to a molar ratio of about 1.3:1, and when the total content of 0.6 - 0.8 wt.% acid and sorbitol reagents equivalent to from about 2.3 to 3 wt.% sorbitol reagent.

When elevated, a commonly used reaction temperatures must be observed precautions to avoid excessive oxidation of the reagents, and usually the reaction vessel is rinsed with nitrogen. In spite of this usually there is some oxidation and/or pyrolysis (possibly oxidative pyrolysis), and made efforts to reduce the extent and/or impact of these undesirable side reactions on the properties of products. The most obvious effect of the product is its color. Improved process for the reduction or removal of colored by-products is the inclusion in the reaction medium, Pleroma phosphorus-containing acids, in particular phosphor and/or hypophosphoric acids (posterolateral) to make the reaction medium is less oxidation (possibly using restorative acid that acts as a sacrifice antioxidant). Often after separation of the activated carbon from the reaction product perform additional discoloration by bleaching. Even with such improvements color, normally liquid product (pure substance) usually corresponds to 8 units of Gardner, which corresponds to a dark brown color. In the absence of such improvement processes coloring can reach more than 10 units of Gardner. Unit Gardner based on the visual comparison, and in this context are probably approximately logarithmic values in the scale concentrations of colored by-products.

Known to produce very pure esters sorbitan and fatty acids by the use of specially purified reagents and separation reactions obtain the esters and ethers, for example, as described in JP 62 - 142141A. However, such methods are rarely implemented in large-tonnage production of esters sorbitan and fatty acids, as multiple stages of purification and reactions does fatty acids, especially Polysorbate type, usually obtained by the reaction of the corresponding complex ester sorbitan with alkalization, in most cases, with ethylene oxide, generally under alkaline catalysis.

The present invention is based on the discovery that the use of a catalytic system in which the relative content of the acid is greater than commonly used, allows to obtain the target ester sorbitan and fatty acids, which has significantly better purity, especially improved color (less than one color on the Gardner) and aroma, even when the reaction system does not add charcoal. Moreover, the use of such a modified catalytic system allows the use of higher concentrations of catalyst, ensure the reduction of the period of reaction at lower temperatures, or a combination of both factors could further improve product characteristics. Esters of fatty acids can be alkoxysilane, in particular ethoxycarbonyl, obtaining product type polysorbates, also with improved color and aroma compared to other similar products obtained by applying the standard proposes a method of obtaining esters sorbitan and fatty acids, which includes the reaction of the fatty acid directly with sorbitol in the presence of a catalytic system, which contains a phosphorus-containing hydroxy (Aha), including restoring the phosphorus-containing acid and a strong base is an alkaline or alkaline-earth metal molar ratio of acid to base is from 0.9:1 to 1.7:1 and when the concentration of the catalytic system from about 1, about 5 to about 30 wt.% from sorbitol.

The invention additionally allows you to get alkoxysilane esters sorbitan, in particular Polysorbate compounds with improved properties, and the invention accordingly includes the use of esters sorbitan and fatty acids, obtained by the method according to the present invention, in the production of relevant alkoxycarbonyl esters sorbitan, in particular Polysorbate substances, by alkoxysilane, in particular ethoxycarbonyl, esters of fatty acids and sorbitan manufactured according to the present invention. Specifically, the invention includes a method of obtaining alkoxycarbonyl esters sorbitan, in particular Polysorbate compounds comprising the reaction of a fatty acid neposredno the phosphorus-containing hydroxy (Aha) as a reducing agent, and a strong Foundation of alkaline or alkaline-earth metal molar ratio of acid to base is from 0.9:1 to 1.7:1 and when the concentration of the catalytic system from about 1.5 to about 30 wt.% from sorbitol with obtaining a complex ester of sorbitol and fatty acids; then alkoxysilane, in particular amoxilonline of ester of sorbitol and fatty acids through the implementation of the reaction of ester with alkalization, mainly ethylene oxide.

Molar ratio of acids and bases correspond to the ratio of the nominal concentrations of N+and HE-the considered compounds (and are, thus, essentially, the work is equivalent to the ratio of the corresponding acids and bases). These ratios for the phosphorus-containing hydroxy acids account for the many possible available protons, so that, for example, phosphorus-containing acid is treated as Dwuosobowy acid.

The catalytic system used in the production method of esters of fatty acids in accordance with the present invention, is a combination of a strong base, alkaline or alkaline-earth metal and acid. The base is a strong alkali and usually represents the second metal, especially sodium hydroxide and/or potassium. The acid portion of the catalyst system includes a phosphorus-containing hydroxy (Aha). At typical elevated temperatures of the reaction it is desirable that the acid catalyst at the temperature of the reaction did not evaporate, and usually acidic part of the catalytic system is completely composed of phosphorus-containing hydroxy acids. Phosphoric oxicology part of the catalyst includes at least some amount of healing fosforsoderzhashchie hydroxy acid (hydroxy acids), such as phosphorus-containing hydroxy (Aha), which acts as a reductant in the reaction conditions receipt of ester. Preferably, reducing phosphorus oxyacids include hypophosphoric acid and/or and especially phosphorous acid. Found that phosphorous acid is significantly more effective hypophosphoric acid, although the reason is not clear. Any phosphorus-containing hydroxy acid is preferably a reducing agent, especially phosphoric acid, but can be used a mixture of restoring fosforsoderzhashchie acid with one or more non phosphorus oxyacids (oxicology), mainly phosphoric Ki the th oxyacids, mainly phosphorous acid was at least 5%, but usually at least 25%, especially at least 50% and typically up to 95% of all fosforsoderzhashchie oxyacids.

Use in a catalytic system hydroxide of an alkali metal and phosphorous acid determines specific feature of the invention, which accordingly includes a method of obtaining esters sorbitan and fatty acids, which includes the implementation of the direct reaction of fatty acids with sorbitol in the presence of a catalytic system, which contains phosphoric acid and alkali metal hydroxide in a molar ratio of phosphorous acid to the alkali metal hydroxide in the range from 0.9:1 to 1.7:1 and when the concentration of the catalytic system from about 1.5 to about 30 wt.% by weight of sorbitol.

The molar ratio of acid and base in the catalytic system used in the production of esters of fatty acids in accordance with the present invention is in the range from 0.9:1 to 1.7:1, in most cases from 1: 1 to 1.5:1, preferably from 1.1:1 to 1.3:1 and especially about 1.2:1. In addition to improving the color target of ester of fatty acids in the use of specific ratios kislota catalyst, increasing the reaction rate in comparison with the known catalytic systems. The reaction rate of obtaining esters of fatty acids can be further increased by use of higher concentrations of catalyst than the commonly used, without causing strengthen the color of the product. We achieved very good results when using up to about 6, especially up to approximately 5 - and mainly up to about 3-fold amount (typically about 2.3 wt.%) of catalyst per sorbitol, which is generally accepted. Thus, in the present invention the catalyst is used in amounts of from about 1.5 to about 30%, in particular from about 3 to about 12% and is mainly about 3 to 8 wt.% catalytic system based on sorbitol. The concentration of the catalyst is expressed in terms of weight of sorbitol, which avoids the obvious differences due to differences in molecular mass are used in different fatty acids, and to some extent compensating for the relatively low concentrations of catalyst (based on the reaction mixture as a whole), usually used for higher esters sorbitan, for example (Tr and fatty acids depends on the inclination of the applied acid oxidation in the process of formation of ester/simple ether. So, it is well known that industrial varieties of sorbitan of monooleate more dark than the corresponding varieties of sorbitan of monostearate and, apparently, it is called unsaturated oleic acid. The invention is particularly applicable for the synthesis of esters of unsaturated fatty acids, but can be successfully applied to obtain esters of saturated fatty acids, although the effect of the relative improvement in color is likely to be less than in the case of unsaturated acids, such as oleic acid. Typically, the fatty acids which can be used in the method according to the present invention include unsaturated fatty acids such as oleic, linoleic, linolenic acid and saturated acids, such as lauric, myristic, palmitic, stearic and Baganova acid. Such fatty acids are usually produced in the form of mixtures of fatty acids with the same carbon chain, which is found in the natural source from which they receive (or simulated synthetic analogs), such as fatty acids of coconut oil (COFA), and are mostly a mixture WITH12and C14acids, fatty acids of palm oil is mainly palmitic acid and hydrogen the method according to the present invention as a source of fatty acids.

Used a variety of sorbitol can also define a color target of ester of fatty acids. It is desirable to apply a variety with a low content of reducing sugars, containing aldehyde or ketone, as it is recognized that the carbonyl group is very easily converted into colored products during pyrolysis, mainly by oxidative pyrolysis. However, the method of obtaining esters of fatty acids in accordance with the present invention can provide significant benefits even when using varieties of sorbitol, which is very low in reducing sugars. In the method according to the present invention the color of the product can be moderately improved by the inclusion of metabisulfite, such as sodium metabisulfite added to the reaction mixture in the form of solids or in aqueous solution. Can be improved with the introduction of metabisulfite is achieved through education metabisulfite adduct with an aldehyde or ketone groups of reducing sugars, which reduces the system sensitivity to the staining in the reaction of obtaining a complex ester of fatty acids. The applied amount of metabisulfite is usually 0.1 to 10 wt.% from sorbitol - number, in most tavoy index of about 0.5 to 1 unit of Gardner in the target complex ester of fatty acids.

The target ester fatty acid may be a mono - or higher ester as sorbitane usually there are four free hydroxyl groups. Typically, esters of mono-, Sesqui-, di - and tri - fatty acids and sorbitan issued by the industry, and a similar product can be prepared by the method according to the present invention. In the industrial manufacture of products produced in accordance with production rules, as they are commercial products, and although they are often referred to as the terms applicable to relatively pure compounds, the products often will not match the integer ratios sorbitan and fatty acid residue. For example, a product commonly marketed under the name of sorbitan monooleate contains an average of from 1.4 to 1.5 residues of oleic acid on the balance sorbitan. Having in mind the above, for the lower esters are typically used fatty acid and sorbitol in equimolar ratio, and the reaction will be carried out substantially to completion. When you need higher esters, some fatty acids may react with sorbitane and as triolein typically contains about 10% unreacted oleic acid.

The method according to the present invention can provide the target esters of fatty acids without the use of activated carbon, with color index greater than that obtained in other similar known methods, in which activated carbon is used. The use of activated carbon is not excluded in the method according to the present invention, but its use does not provide any significant additional benefits. Of course, the non-use of activated charcoal can be considered as an advantage of the method, since coal is difficult or impossible to filter from the target complex fatty acid ester, and prefer to leave on the filter a certain amount of product, typically a few percent of the total output, in a form that is not easily separated from the coal.

Similarly, in a typical known method for obtaining relatively malaekahana product of ester of fatty acid, it is usually subjected to bleaching, for example, hydrogen peroxide. In accordance with the present invention the products of good color can be obtained without bleaching. Moreover, additionally improved color can be achieved by bleaching prognolo care it may be preferable to use unbleached ester products of fatty acids, that avoids any risk of contact residues whitening substances or by-products of bleaching in the final products.

The reaction of obtaining esters of fatty acids is usually carried out in an atmosphere of inert gas, usually nitrogen atmosphere to minimize oxidation decomposition of the initial reactants or products, and at temperatures high enough to evaporate the water present in the reagents or formed in the reaction of obtaining a simple ester and ether complex. Typically, the reaction mixture is heated to the maximum temperature after mixing of the reactants and a catalyst. The generally accepted maximum reaction temperature of about 240 - 250oSince, however, it is established that can be used to lower the temperature. Thus, in accordance with the present invention, the peak reaction temperature typically ranges from 150 to 250oWith, but in most cases, from 170 to 230oC. the Use of reaction temperatures below those generally accepted, particularly preferably with the use of higher concentrations of catalyst. At concentrations of catalyst above the conventional 2 - 3 times may apply temperature Raccordo 6-fold, the generally accepted level of the reaction temperature, if necessary, can be reduced to about 170oC. lowering the temperature of the reaction, obviously, provides an additional advantage in the color and purity of the product. Even at relatively low temperatures, the duration of response for the proposed method may be shorter than the conventional one. The inventors have achieved a satisfactory degree of conversion during the reaction period of 5 hours and a maximum reaction temperature of 220oWith against reaction period of 8 hours at a maximum temperature of 245oWith, in case, similar to the conventional catalytic system (about 1.3:1 (mol.) sodium hydroxide to phosphoric acid at 0.7 wt. %).

Less colored esters of fatty acids, which can be obtained by the method according to the present invention, particularly acceptable as dispersants and/or emulsifiers for inclusion in products for personal care. Specific end use is usually associated with a particular esters, so sorbitan palmitate, sorbitan stearate, sorbitan beginat particularly used in creams type emulsion oil-in-water, dairy products and liquid cosmetic and liquid cosmetics and massage oils and oils for baths, in water washable ointments and cosmetics, in particular in lipstick, blush and other items for make-up, especially as a pigment dispersant, and laurate in mud packs, especially as a dispersant, and in children's shampoos, especially as air conditioning.

In addition to the advantages of less coloring arbitarily ester of fatty acids, manufactured by the method according to the present invention, has less odor, usually less than desirable odor than conventional materials. So, the smell is usually more similar to the smell of butterscotch than with smells burnt or foul odor associated with conventional sorbitan esters, currently commercially available. An additional advantage is particularly suitable for use in personal care products is that esters synthesized by the method according to the present invention, need not and usually do not contain residues of bleaching components, because bleaching components are not applied (as described above they are not needed). This makes these materials particularly attractive for personal care products such as cosmetics, which ispolzuetsyaprintsip care, especially species mentioned above, containing one or more esters of fatty acids, obtained by the method according to the present invention as dispersants and / or emulsifiers, and the application contains one or more esters of fatty acids, obtained by the proposed method, as dispersants and / or emulsifiers in personal care products.

Improving the color and odor also allows to synthesize alkoxysilane products, in particular ethoxylated products Polysorbate type with improved color and odor, and as mentioned above, the invention includes obtaining alkoxysilane, in particular ethoxylated esters sorbitan and fatty acids, and the use of esters sorbitan and fatty acids, obtained by the method according to the present invention, in the production of alkoxysilane, in particular, ethoxylated, sorbitan esters of fatty acids (polysorbates). The reaction alkoxysilane sorbitnogo of ester is typically carried out at a temperature substantially above ambient temperature, for example at about 125 - 175oSince, typically, using a basic catalyst, in most cases hydroxide selecing is from. The reaction is carried out until the desired degree of alkoxysilane, usually defined as the number of HE (mg KOH equivalent per gram of product). At the end of the reaction, a basic catalyst is neutralized with getting unbleached product. Improved color esters sorbitan and fatty acids allows you to omit the usual stage postalcodenumber bleaching in the production of such alkoxysilane products, it is particularly advantageous for products personal care for which you want to minimize the content of bleaching residues (preferably, to achieve their full absence). Improvement of smell is also appropriate for consumers of personal care and consumer food additives. If necessary the product even less color, then ethoxylated materials can otmelivatsja in a standard way, for example hydrogen peroxide.

Such ethoxylated, especially ethoxylated derivatives of esters sorbitan, are used as emulsifiers and dispersants in emulsions of the type oil-in-water creams, especially as solubilization perfume and flavouring substances in products for personal care and PI is about care and food product and/or additives, especially the above-mentioned types, including one or more alkoxycarbonyl(s), in particular ethoxylated(s) ester(s) sorbitan and fatty acids, obtained by the method according to the present invention as dispersants and/or emulsifiers and/or solubilization and application alkoxysilane(s), in particular ethoxylated(s) of ester(s) sorbitan and fatty acids, obtained by the method according to the present invention as dispersants and/or emulsifiers and/or solubilization in personal care products, and/or in food products, and/or supplements that you take.

Improved color colored sorbitan esters and alkoxysilanes, mainly the ethoxylated sorbitan esters obtained by the method according to the present invention, can enhance the color during storage, especially if you are not taking special precautions. In order to make the products less prone to deterioration, it may be appropriate to include in the ester products are a small portion, for example from 0.01 to 0.25 wt.% antioxidant, such as 2,6-di-tert-butyl-4-METHYLPHENOL.

The following examples illustrate the present invention. If specially the second acid - Priolene 6900, ex Unichema;

lauric acid - rated lauric acid is a COFA - fatty acids derived from coconut oil (a mixture of C12- C14mainly saturated fatty acids);

sorbitol - Sorbidex 130 ex Cerestar;

dicalite - additive diatomaceous earth to filter ex Redland Minerals.

Test methods:

color is measured using a Gardner colorimeter; the results are expressed in units of Gardner (GU);

acid number is measured by the ASTM D974-92; results expressed in mg (KOH equivalent) g (samples)-1;

hydroxyl number measured by the ASTM E326-85; the results are expressed in mg (KOH equivalent) g (samples)-1;

the saponification number is measured according to the method CAPAR4/1; the results are expressed in mg (KOH equivalent) g (samples)-1.

Example 1.

As a laboratory reactor for the production of ester by the esterification use flat-bottomed glass flask of 1 liter, equipped with a supply of nitrogen, a thermometer (thermocouple), mechanical Teflon stirrer, a column of Vigreks side capacitor associated with the team of the bulb, and the outer jacket. In the flask is charged with oleic acid (416 g; 1,47 mol), sorbitol (184 g; 1 mol, in the form of a 70% aqueous rest the tion of 1.2:1), the mixture was thoroughly otdovat nitrogen (and during the reaction) and continuously raising the temperature to 110oWith, in which water (from a solution of sorbitol) begins to Athanasia from the reaction mixture. The temperature is slowly increased to 130oTo halt the removal of free water and then raised to 245oC for 30 minutes. In the course of the reaction periodically take samples for analysis on the acid number to his fall below 10 and then on the hydroxyl number to decrease in the range 210 - 185. The amount of water condensate from the reaction is also used for indicating the reaction. The reaction mixture was then filtered through filter paper with medium flow using 1 wt.% (calculated on the weight of the reaction mixture) Dicalite as filtration media. Repeat this example as a comparative example 1C except that the used catalyst at a concentration of 2.3 wt.% a mixture of NaOH and phosphorous acid in a molar ratio of acid : base of 0.8:1. Product properties are given in table.1.

Examples 2 to 9.

Repeat example 1, using different molar ratios of acids and bases and different concentrations of catalyst. In table. 2 shows the ratio and centerantalya example 4C is used phosphoric acid, that is no healing phosphorus-containing hydroxy acid is not used.

Example 10.

Repeat example 1 except that to obtain (nominally) trioleate sorbitan apply the molar ratio of oleic acid to sorbitane about 3: 1 and the concentration of catalyst 5.7 wt.% from sorbitol at a molar ratio of acid to base of 1.2:1. Comparative example 10C is similar to example 10, but using a molar ratio of acid to base is 0.8:1 and a concentration of about 2.8%. The results are shown in table. 2.

Example 11.

Repeat example 1 except that instead of used in example 1 oleic acid is used lauric acid (COFA) and the catalyst at a concentration of 3.2 wt. % when the molar ratio of the acid to the base of 1.2:1. Comparative example 11C is similar to example 11 except that the molar ratio of acid to base is 0.8:1 at a concentration of catalyst of 1.6%. The results are shown in table.2.

Example 12.

Repeating example 5 except that the reaction mixture include activated carbon (6.7 g; 1.8 wt.%). Product color corresponds to 3 units Gardner, the same as in example 5.

Example 13.

Example 14.

Repeat example 7 except that instead of phosphorous acid according to example 7 is used hypophosphoric acid (0.26 wt.% when the molar ratio of the acid to the base of 1.2: 1). Product color corresponds to 5 per Gardner, 2 units worse than the product in example 7.

Example 15.

Example 4 is repeated on a pilot installation with getting about 25 kg target of ester. At the end of the reaction receipt of ester color of the product is 5% Gardner. Procedural ester maintain the reactor in a stream of nitrogen over an extended period of time, at the end of which color is enhanced to 8% Gardner (because of the additional decomposition of the cooling-off period).

Example 16.

A sample of the product from example 15 amoxilbuy in 19-liter autoclave, equipped with a top paddle stirrer. Charged to the reactor, sorbitan monooleate (about 1500 g; about 3.4 mol) and vacuum at ambient temperature. The temperature was raised to 90oAnd add the sodium hydroxide. The mixture is optionally heated to 120oWith and removed under vacuum to 5 bar, until the hydroxyl number of the product will not show almost full completion of the reaction, and the system give the possibility to continue the reaction after the addition of ethylene oxide up to a decrease of pressure to a constant level. Ethoxylated product was then cooled and vacuum outgassing keep the temperature above 100oWith the addition cool and add acid to neutralize the catalyst. The color of the unbleached ethoxylate corresponds to 7% Gardner. Color correction of this product in order to reduce the magnitude of the color index for complex ether (from the exposure time at elevated temperature) allows to reach about 3.5 - 4 units of Gardner.

The whitening effect of this product check the effect on the sample with hydrogen peroxide at 90. The color of the bleached product is equivalent to 5 units of Gardner. Color correction of this product in order to reduce the heightened color in complex ether (from the exposure time at elevated temperature) achieves an approximately 2 - 3 units Gardner.

Comparative testing is also carried out under the conditions of example 16, using industrial sorbitan monooleate (Span 80 ex ICI Surfacants), the color of which corresponds to 8% Gardner. Color neotv the RA.

1. The method of obtaining esters of fatty acids and sorbitan and/or their alkoxysilane derivatives, including interaction of the fatty acids directly with sorbitol in the presence of a catalytic system comprising phosphorus-containing hydroxy (Aha), including restoring phosphorus containing the hydroxy acid and the strong base is an alkaline or alkaline-earth metal molar ratio of acid to base of 0.9: 1 to 1.7: 1 and when the concentration of the catalytic system 1.5 to 30 wt. % (based on sorbitol and possibly subsequent interaction of the obtained esters with alkalization.

2. The method according to p. 1, characterized in that healing phosphorus-containing acid is or includes phosphorous acid.

3. The method according to p. 1 or 2, characterized in that the main component of the catalytic system is an oxide, hydroxide or carbonate of alkali or alkaline-earth metal.

4. The method according to p. 3, characterized in that the base used is sodium hydroxide and/or potassium.

5. The method according to p. 1, characterized in that the use of the catalytic system, which includes phosphorous acid and the alkali metal hydroxide in a molar system 1.5 to 30 wt. percent, based on sorbitol.

6. The method according to any of paragraphs. 1-5, characterized in that the catalytic system, the molar ratio of the acid to the base is in the range of 0.9: 1 to 1.7: 1.

7. The method according to p. 6, characterized in that the molar ratio of the acid to the base is in the range from 1.1: 1 to 1.5: 1.

8. The method according to any of paragraphs. 1-7, characterized in that the concentration of the catalytic system is equal 3-12 wt. % (based on sorbitol.

9. The method according to p. 8, characterized in that the concentration of the catalytic system is equal 3-8 wt. % (based on sorbitol.

10. The method according to any of paragraphs. 1-9, wherein the reaction mixture additionally contains metabisulfite.

11. The method according to p. 8, characterized in that as metabisulfite is used metabisulfite sodium.

12. The method according to p. 10 or 11, characterized in that the concentration used metabisulfite 0.1-10 wt. % (based on sorbitol.

13. The method according to any one of paragraphs. 1-12, in which the reaction is carried out at a temperature in the range 170-230oC.

14. The method according to p. 13, characterized in that as alkalinized used ethylene oxide.

 

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1 cl, 1 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: described is a cosmetic composition in form of a Pickering type "oil-in-water" emulsion for skin or hair, containing a "core-shell" type microgel emulsifier, oil phase ingredients and aqueous phase ingredients, where "core-shell" type microgel emulsifier consists of a copolymer, typically obtained by polymerising polyethylene oxide macromonomers of following formula (1), hydrophobic monomers of following formula (2) and cross-linking monomers of following formula (3) in following conditions (A) and (B): (A) molar ratio of initial molar amount of said polyethylene oxide to initial molar amount of hydrophobic monomers is 1:10–1:250, (B) initial amount of said cross-linking monomers is 0.1–1.5 wt% with respect to initial amount of said hydrophobic monomers; (1), where R1 denotes alkyl having 1–3 carbon atoms, and n is an integer from 8 to 200, X denotes H or CH3; (2), where R2 denotes alkyl having 1–3 carbon atoms, and R3 denotes alkyl having 1–12 carbon atoms; (3), where R4 and R5 each independently denotes alkyl having 1–3 carbon atoms, and m is a number from 0 to 2, where amount of "core-shell" type microgel emulsifier is 0.01–10 wt% with respect to total amount of composition in form of Pickering emulsion. Also described is a method of producing said cosmetic composition in form of a Pickering type "oil-in-water" emulsion, which includes: mixing and dispersing "core-shell" type microgel emulsifier in water or aqueous phase ingredients, adding oil phase ingredients and other ingredients, and emulsifying mixture by mixing and applying a shear force. Invention also describes use of said "core-shell" type microgel emulsifier for producing a cosmetic composition in form of Pickering type "oil-in-water" emulsion for skin or hair.

EFFECT: obtaining a composition in form of emulsion with improved emulsification stability, with low skin irritation and low sensation scratchiness and powderiness.

5 cl, 1 dwg, 14 tbl, 20 ex

FIELD: chemistry.

SUBSTANCE: in the proposed method for producing fatty acid and sorbitan esters, vegetable oils interact directly with sorbitol in the presence of a catalytic system consisting of hydroxy acid and sodium hydroxide at the molar ratio of 0.8:1.2-1:2 and at the concentration of the catalyst system of 2-4 wt % in terms of sorbitol.

EFFECT: efficient method for producing sorbitan and fatty acid esters.

3 cl, 1 tbl, 32 ex

FIELD: organic chemistry, chemical technology, pharmacy.

SUBSTANCE: invention relates to the improved method for isolating and purifying pravastatin or its pharmacologically acceptable salt from impurities of pravastatin analogues. Method involves extraction of pravastatin or its pharmacologically acceptable salt comprising impurities of pravastatin analogues with organic solvent of the formula: CH3CO2R wherein R represents alkyl comprising 3 or 4 carbon atoms. Also, invention relates to the improved method for isolating or purifying pravastatin or its pharmacologically acceptable salt that involves decomposition of impurities by using inorganic acid or that involves removing compound of the formula (I): by using inorganic solvent. Also, invention relates to the composition comprising pravastatin sodium salt and compound of the formula (I) taken in the amount 0.1 wt.-% or less with respect to the amount of pravastatin sodium salt. Method provides preparing the end product of the high purity degree.

EFFECT: improved purifying method.

18 cl, 1 tbl, 8 ex

FIELD: chemistry.

SUBSTANCE: in the proposed method for producing fatty acid and sorbitan esters, vegetable oils interact directly with sorbitol in the presence of a catalytic system consisting of hydroxy acid and sodium hydroxide at the molar ratio of 0.8:1.2-1:2 and at the concentration of the catalyst system of 2-4 wt % in terms of sorbitol.

EFFECT: efficient method for producing sorbitan and fatty acid esters.

3 cl, 1 tbl, 32 ex

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