SU1051068A1 - Process for preparing surfactant - Google Patents

Abstract

The formulation of a surface-active substance is determined by the fact that the mix is up to 18-20 atoms of the ugene and the highest aliphatic alcohol of the fraction with 10-18 atoms of the ugoropa, ipi popioetietipenoostoy, the most important component of the problem, I’ve been out of the problem, I’ve used the problem, I’ve used it. hydroxyethiene groups, and apanopamide synthetic fatty acids, 4 stocks, with a concentration of 2–12 wt.%, are subjected to saturation by gaseous cef oxide, and diluted with inert gas to 4–8% by volume, if necessary. The ratio of the initial reagents is 1: 1 - 1.2, respectively, at FROM 70 ° C with a gradual decrease to 36 ° C, followed by neutralization of the mass with an aqueous solution of sodium hydroxide to a pH of 7.5 - 9 at 20-60 ° C ;WITH. (L with

Description

O) 00 The invention relates to a method for acquiring a new surface-active substance (surfactant), which can be used as a component in washing composites for technical and quick purposes. A method for producing surfactants is known, according to which a mixture of 20% by weight of apanopamide fatty acids having 8-2O carbon atoms in the mixture and a BO% by weight of organic orthomerase having 8-26 carbon atoms, for example apkilbenzop, higher aliphatic alcohol, is prepared or high-aliphatic alcohol popioxyethipene ester with 2-12 oxyethylenes and groups in the molecule. Then the liquid J mixture is sulfated with chlorosulfonic acid, taken with a 5 mol.% Excess relative to the stoichiometric amount required. The suphatization process is carried out in a batch reactor with vigorous stirring and cooling of the reaction mass in such a way that its temperature remains constant during the whole process and is within 34-30 0. After the supply of the sulfating agent to the reactor, the reaction mass neutralized with an aqueous solution of sodium hydroxide. The yield of the target product (a mixture of anion-active surfactants i used as the combined active base of detergents) is 88 mop. Foaming ability of the product obtained, defined as the height of the foam column formed in the measuring cylinder when it is mixed with O, Vol% w / w aqueous solution, and measured immediately after stopping the mixing does not exceed 155 mm fl. However, the known method does not allow to swell up the combined active basis of washing means with high peeling ability. The reason lies in the fact that supatriation of a mixture of apanolamide acidic acids with alkylbetape, a higher aliphatic alcohol or a popioxyethylene ester of higher aliphatic alcohol, taken in a percentage ratio of 20:80, does not eliminate the sharp increase in the viscosity of the reaction mass during the suppressive process. When using the hydrogen sulfonate powder as a sulfating agent, this leads to a termination of the bubbling of gaseous reaction products and causes the formation of a foamed reaction mass in the reactor. This circumstance does not allow the process of sulphating the mixture to be completed, which reduces the yield of the target product and impairs its foaming capacity. The purpose of the invention is to develop a method of obtaining a new surfactant, which has a high perennial ability, and an increase in the yield of the target product. The delivered chain is achieved in that according to the method of obtaining a surfactant, a mixture of alkyl benzene with 18-2 O carbon atoms or a Shaped aliphatic alcohol fraction with 10-18 carbon atoms, or polyoxyethylene ether of a higher aliphatic alcohol fraction with 1 O-18 carbon atoms, containing 3-7 oxyethyl or new groups and alkali-amide of synthetic acids of 1H acids of fraction Сi. With a concentration of the latter 2-12 wt.%, It is subjected to sulfate treatment with gaseous sulfur trioxide, diluted with ishft gas to 4-8 vol.%, Or chlorosulfeic acid at a molar ratio of initial reagents, equals 1: 1 - 1.2, respectively, at 70 ° C with a gradual decrease to 36 C, followed by neutralization of the reaction mass with an aqueous solution of sodium hydroxide to pH 7.5 - 9 at 20-60 ° C. The yield is 91-99 mol.%, .. a foaming capacity of 160-1.95 mm. Enhance yield and peoreforming. The characteristics of the target product are achieved by noticing that when sulphating a mixture of apkilbevzop ipv prirta, or its popvoxyugene foam and apanopamid fatty acids, including 2 to 12 wt.% of the latter, there is no sharp increase in the viscosity of the reaction mass during the test. In addition, maintaining the sulfate reaction temperature higher than the limestone method also leads to a decrease in the viscosity of the reaction mixture and eliminates its foaming, which allows the sulphation process to be completed (thereby increasing the yield of the organic matter mixture). In turn, a decrease in the content of unsaturated raw materials in the product contributes to its higher foaming capacity. The reduction in the temperature of the supipatriation reaction in the range of 70-36 ° C eliminates the

side reactions of oxidation and dehydration of organic umberodorods, whose products reduce the foaming ability, detergents,

The boiled method of surfactant stoning, as a result of maintaining the high temperature of the sup-fatigue reaction and lowering the viscosity of the reaction mass, allows us to use it. as a sulfating agent, not only chlorosulfonic acid, yo and gaseous sulfur trioxide diluted with an inert gas. Due to this, the process of sulfation of the mixture can be carried out both in a batch reactor with a stirrer and in a continuous film reactor. Moreover, in the latter case, the energy consumption for mechanical mixing of the reaction of a different mass is excluded. Example 1. In a tsipindrice reactor with an inner diameter of 45 mm and a height of 110 mm, equipped with a bubbling tube, a paddle stirrer, cooling jacket, a thermal slide and fittings for supplying reagents to the outlet of the gaseous reaction products, 82.0 g of the mixture consisting of 2 wt. .% (1.64 f) of the myoethanepamide I synthetic fatty acids of the fraction. . CIQ-C g with average MOS. weighing 264 and 98 wt.% (8O, 36g) ve higher ali fatic alcohol fraction with an average mop.vesy 216.

Having established the initial temperature of the mixture at 70 ° C, sulfur trioxide gas diluted with dried air to a concentration of 4 vol% sulfur trioxide is introduced into the reactor. Three-oxide consumption. Sulfur 1.65 g / min. Time of sulfation 21 minutes The molar ratio of sulfur trioxide to the mixture subjected to sugatirovanie 1.15: 1.0. Simultaneously with the start of the supply of sulfur trioxide to the reactor, the temperatures of the reaction mass 1 are gradually reduced to. the end of the suprapatsion reaction. After stopping the supply of sulfur trioxide to the reactor for 15 minutes, continue stirring the reaction mass until the gaseous products of the reaction are stopped, after which it is neutralized to a pH of 7.5-8.0. 113 g of sodium hydroxide sodium hydroxide solution 20-60 0. Take 228 g of the neutralized reaction mass.

The yield of the target product, determined by the method of extraction of anion-active

The PDV with isopropyl alcohol is 125.0 g (98 mop.%). The foaming capacity of the surfactant obtained is 172 mm.

Example 2. A mixture of organic substances with a total weight of 82.0 g, consisting of 5% by weight (4.10 g) of synthetic fatty acid monoethanolamide of the C | o-C fraction with an average mol. weighing 264 and 95% by weight (77.9Og) of the higher aliphatic alcohol fraction С fo - with an average mol. weighing 216, sulfatirovat and neutralized under the conditions of example 1. Get 227 g of the neutralized reaction mass.

The yield of the target product is 121.2 g (96 mol.%). Foaming capacity 180 mm.

Example 3. A mixture of organic substances with a total weight of 82.0 g, consisting of 12% by weight (9.84 g) of monoethanolamide synthetic fatty acid frac; tion with an average mol. weighing 264 and 88 wt.% (72.16 g) of the higher aliphatic alcohol fraction. With a mean mol. weight 216, supiphate and neutralize under conditions of example 1. Obtain 228 g of the neutralized reaction mass.

The yield of the target product 116,0 g (91 mol.%). Foaming capacity is 16 mm.

PRI me R 4. A mixture of organic substances with a total weight of 82.0 g, consisting of 10 wt.% (8.2 g) of synthetic fatty acid monoethanolamide C fraction (QC with an average molecular weight of 264 and 90 wt. .% (73.8 g) from the higher aliphatic alcohol fraction with an average molecular weight of 216, sufate chlorosulfonic acid, followed by neutralization under the conditions of example 1, but at a molar ratio, the sulfate of the binding agent to the mixture of organic substances 1, O5: 1, Chlorosglonic acid consumption is 1.89 g / min and the sulfation time is 24 minutes. Receives 223 g of neutralized reaction mixture ssy;

the yield of the target product 119,0 g (92 mol.%). Foaming capacity is 165 mm.

Example 5. In a vertical reactor of film-based TVP with an internal diameter of 5 mm and the length of the reaction zone; 800 mm, equipped with a cooling bushing, supplying nipples in the upper part of the reactor and a discharge pipe to the lower part of which, a mixture of organic substances is continuously fed, consisting of 10% by weight of mono-ethanopamide C synthetic fatty acid (g average MOP. weight 264 and 9O wt.% of the highest apiphagic alcohol fraction with an average mop weight 216. Consumption of a mixture of these organic substances 6.2 g / min Suffering agent - gaseous sulfur trioxide diluted with dried air to a concentration of 6 vol. % trioxide, also not At a rate of 2.48 g / min, the molar ratio of sulfur dioxide to the mixture of organic substances 1.10: 1.0 is supplied discontinuously to the upper part of the reactor, and the temperature of the sufatation process is fed countercurrent to the direction of movement of the reactor. cooling water. At that, the temperature of the mixture of organic substances at the entrance to the reaction zone is 70 ° C and the reaction mass at the outlet. The reaction mass leaving the reactor is degassed in a cyclone and neutralized to pH 7.5 - 9.0 by adding to her 7.4 g / min 1 5% of an aqueous solution of sodium hydroxide at 2 ° -6 ° C. Output of the neutralized reaction mass 15.8 g / min. The yield of the target product is 9.8 g (94 mol.%). Foaming capacity is 175 mm. Example 6. A mixture of organic substances consisting of 10% by weight of monoethanolamide synthetic fatty acids of the CY - C fraction (with an average mol. Weight of 201 and 9O% by weight of higher aliphatic alcohol 4 Acioia Cio-Cj with the average mole. weighing 2U2, they are continuously sufatized and neutralized under the conditions of Example 5, but with a consumption of a mixture of organic substances 5.8 g / min. The flow rate of gaseous sulfur trioxide diluted with nitrogen to a concentration of 8 vol.% sulfur trioxide, 2.56 g / min. The temperature of the inlet in the reaction of organic substances in the oning zone is 48 C, and the reaction mass at the outlet is 36 C. The output of the neutralized reaction mass is 15.2 g / min, the yield of the desired product is 8.6 g (95.5 mol.%). The foaming ability is 178 mm. Example 7. A mixture of organic substances consisting of 5 wt.% of. synthetic fatty acid monoethanopamide C | oC; f6 with an average molecular weight of 264 and 95% by weight from a dodecylbenzop with a molecular weight of 244, is continuously fed and neutralized under the conditions of example 5, but at a sulfur trioxide consumption of 2.22 g / min and consumption of a 15% aqueous solution of sodium hydroxide 6.7 g / min. The output of the neutralized reaction mass 13.9 g / min The yield of the chain product 9.1 g {98 mol.%). Foaming capacity is 172 mm. Example 8. A mixture of organic substances with a total weight of 82.0 g, consisting of 8% by weight (6.6 g) of mono-ethanopamide synthetic fatty acids, fractions with an average mol. weighing 201 and 92 wt.% (75.4 g) of tetradecylbenzene, mol. weighing 272, sulphate chlorosulfonic acid in the reactor of example 1. Consumption of chlorosulfonic acid 1.83 g / min. Sulfation time 20 min. The molar ratio of the sulfating agent to the mixture of organic substances is 1.02: 1. Simultaneously with the start of the delivery of chlorosulfonic acid to the reactor, the temperature of the sulfation reaction is lowered from 46 ° C at its beginning to 36 ° C at its end. After stopping the delivery of the Hprsulfonic acid to the reactor for 15 minutes, the reaction mixture is continued until the gaseous reaction products are completely released, and then neutralized to pH 7.5-8.0 by adding to it 68.5 g of a 25% aqueous caustic solution. sodium at 2060 ° C. Obtain 175.2 g of the neutralized reaction mass. The yield of the chain product is 112 g, (95 mol.%). Foaming capacity is 168 mm. Example 9. A mixture of organic substances consisting of 4% by weight of monoethanolamide synthetic fatty acids of the Cfo-C fraction (, with an average molecular weight of 264 and 96% by weight of polyoxy-type ester aliphatic alcohol fractions with 3 oxyethylene groups in the molecule and an average molecular weight of 308, iHonpejaJBHo is sulfated and neutralized under the conditions of Example 5, but with a three-oxime consumption of 1.25 g / min and a 15% aqueous solution of caustic sodium hydroxide 5.5 g / min. the reaction mass of 12.9 g / min. The yield of the target product 8.4 g LLC mol.%). The foaming capacity is 195 mm. Example 10. A mixture of organic substances weighing 82.0 g, consisting of 1% by weight (8.2 g) of synthetic fatty acid monoethanolamide of the C-f-CiQCo fraction, mol, weighing 201 and

90 wt.% (73.8 g) from the popioxyethiophene ester of the highest apiphatic alcohol fraction with 7 hydroxyethiene groups in the molecule and the average mop. weighing 5.24, is sulfated and neutralized under the conditions of Example 8, but at a flow rate of 1 × 8 g / min, a time of 18 mive and an aqueous solution of sodium hydroxide is 52.0 g / min.

Obtain 148.7 g of the neutralized reaction mass. The yield of the chain product is 112 g (92 mop.%). Foam quality is 190 mm.

Thus, the proposed method, compared with the known one, by suppressing a mixture of organic substances and fatty acid alkanopamide with a concentration of the latter 2-12 wt.%, Calculated on the total weight of the mixture, and also by maintaining a higher and variable sulphate reaction temperature, yield and foaming ability of the target product.

Comparative indicators of the previous, known and known methods are given in the following table. one.

ITe, b p and c a 1

As can be seen from the table. 1, the proposed 45 method, in comparison with the known one, allows increasing the yield of the target product by 3–11 mol% and obtaining a surfactant with a significantly higher: gpeneproduc tion) ability. 50

New surfactant can be used as a component in the wash compositions.

The test was carried out in a synthetic detergent (CMC) surfactant, 55 obtained according to the proposed test method was carried out according to the test method by comparing the detergent action

CMC, including a new surfactant with the action of CMC on the basis of lauryl sulfite.

For tests, samples of universal CMC of the following composition are prepared, wt.%:

. PAV20,0

Trishylphosphate sodium 4O, 0 Carboxymegycellulose 2,0 Silicate Vatrv 8.0

Stream sulfate 10.0

Vodado 10O, 0

Determination of the detergent action carried out in a paundermeter piece

Claims (1)

METHOD FOR PRODUCING SURFACE ACTIVE SUBSTANCE? characterized in that a mixture of alkvlbenzop with 18-20 carbon atoms or a higher aliphatic alcohol fraction with 10-18 carbon atoms, or a polyoxyethylene ester of a higher aliphatic alcohol fraction with 10-18 carbon atoms containing 3-7 hydroxyetipene groups, and synthetic apcanopamide of fatty acids of the C ^ -C ^ fraction with a concentration of the latter of 2-12 wt.% is subjected to sulfation with gaseous three <sulfur dioxide, diluted with an inert gas to 4-8 vol.%, or with horsulfonic acid at a molar ratio of mating reagents equal to but 1: 1 - 1.2, at from 70 ° C with a gradual decrease to 36 ° C, followed by neutralization of the mass with an aqueous solution of sodium hydroxide to pH 7.5 - 9 at ® 20-60 ° C. 1 1051068 2