CN111087328A - Preparation method of fatty alcohol sulfosuccinic acid monoester disodium salt - Google Patents
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Abstract
The invention relates to a preparation method of fatty alcohol sulfosuccinic acid monoester disodium salt. The method comprises the following steps: (1) mixing fatty alcohol, an alkaline catalyst and maleic anhydride, and reacting at 70-90 ℃; (2) mixing the reaction product obtained in the step (1) with a washing solvent, heating to 40-80 ℃, and separating to obtain upper-layer liquid; (3) mixing the upper layer liquid with an aqueous solution of sodium sulfite, and reacting at 70-90 ℃; the washing solvent is water, an aqueous solution of an inorganic salt or an aqueous solution of a weakly basic metal organic non-carbonate salt. The method washes a reaction product of fatty alcohol and maleic anhydride by using a washing solvent at a specific temperature, and then reacts with sodium sulfite to obtain the fatty alcohol sulfosuccinic acid monoester disodium salt simply, efficiently and highly-purely.
Description
Technical Field
The invention relates to the field of organic synthesis, in particular to a preparation method of fatty alcohol sulfosuccinic acid monoester disodium salt.
Background
The quality of the common fatty alcohol in the market is poor, the less the number of carbon atoms in the fatty alcohol, the stronger the water absorption and the higher the moisture content, and the influence along with the preservation mode of the fatty alcohol and the climate environment is larger, when the fatty alcohol is used for producing the fatty alcohol sulfosuccinate disodium salt, the maleic anhydride and the water in the fatty alcohol are difficult to avoid reacting to generate maleic acid, and then the maleic anhydride and the water in the fatty alcohol are further sulfonated to generate the sulfosuccinate. On one hand, the quality of the product is difficult to improve, strong competitiveness is lacked in the international market, on the other hand, the consumption of the sulfonating agent sulfite in the subsequent sulfonation reaction is wasted, and then unnecessary byproducts are introduced, so that the product does not meet the original purpose of green chemistry advocated by the current society.
During the synthesis of the sodium dodecyl alcohol allyl succinate sulfonate (Zhang Zhenhua, Liuchang, school report of southern Hua university, 18 vol.4 in 2004), the intermediate dodecyl alcohol maleic acid monoester is synthesized, and acetone is adopted to recrystallize for 3 times, so that a pure intermediate is obtained. The organic solvent acetone is adopted, so the cost is high, and the method is not suitable for industrial production. Patent application CN106748911A discloses a method for efficiently synthesizing sulfosuccinic acid ethoxy ether fatty alcohol monoester disodium salt, which adopts an alkaline mixed catalyst to improve the conversion rate of alcohol ether in esterification reaction and reduce the by-product of fatty alcohol polyoxyethylene ether maleic diester. The references of pilot study on synthesis of alcohol ether sulfosuccinic acid monoester disodium salt (Guangzhou chemical industry, No. 11 of No. 38 2010), research progress of sulfosuccinate surfactant (Zhang Jun, Huaping, Jiangsu chemical industry, No. 6 of No. 29 of No. 2001: 16-26) and the like adopt a method of excessive maleic anhydride for synthesis, and then are used for the next sulfonation reaction after detection of constant acid value. Almost neglects the by-product and catalyst residue which are finally sulfonated to generate sulfosuccinate caused by maleic anhydride residue, and the by-product, catalyst and the like in the product have a growing trend along with the increase of the standing time, color, smell and various physicochemical indexes, thus greatly reducing the purity and quality of the final product and seriously hindering the application of the product.
Therefore, the preparation method of the fatty alcohol sulfosuccinic acid monoester disodium salt, which has the advantages of simple process, easy realization of large-scale production and high purity, has important significance.
Disclosure of Invention
Based on the above, the invention aims to provide the preparation method of the fatty alcohol sulfosuccinic acid monoester disodium salt, which has the advantages of simple process, easy realization of large-scale production and high purity.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of fatty alcohol sulfosuccinic acid monoester disodium salt comprises the following steps:
(1) mixing fatty alcohol, an alkaline catalyst and maleic anhydride, and reacting at 70-90 ℃;
(2) mixing the reaction product obtained in the step (1) with a washing solvent, heating to 40-80 ℃, and separating to obtain upper-layer liquid;
(3) mixing the upper layer liquid with an aqueous solution of sodium sulfite, and reacting at 70-90 ℃;
the washing solvent is water, an aqueous solution of an inorganic salt or an aqueous solution of a weakly basic metal organic non-carbonate.
Compared with the prior art, the invention has the following beneficial effects:
the method of the invention obtains the fatty alcohol sulfosuccinic acid monoester disodium salt simply, efficiently and highly-purity by washing the reaction product of the fatty alcohol and the maleic anhydride with a washing solvent at a specific temperature and then reacting the reaction product with sodium sulfite. In the invention, a large number of experimental researches show that water, an aqueous solution of inorganic salt or an aqueous solution of alkalescent metal organic non-carbonate is selected as a washing solvent, and the washing solvent can selectively dissolve residual impurities such as catalyst, byproducts and the like at 40-80 ℃. Furthermore, the maleic acid fatty alcohol monoester is in a molten state at 40-80 ℃, and is hardly soluble in a washing solvent. Therefore, impurities dissolved in the washing solvent can be separated from the intermediate maleic acid fatty alcohol monoester to form two incompatible phases, so that the impurity content in the intermediate maleic acid fatty alcohol monoester is greatly reduced, and the high-purity maleic acid fatty alcohol monoester is obtained. And the reaction conditions of the esterification reaction and the sulfonation reaction are optimized further, so that the purity of the target product, namely the fatty alcohol sulfosuccinic acid monoester disodium salt is improved obviously.
Drawings
FIG. 1 is an infrared spectrum of disodium lauryl sulfosuccinate prepared in example 1;
FIG. 2 is an HPLC chromatogram of disodium lauryl sulfosuccinate prepared in example 1 (wherein 2.80min is the sodium ion peak of the product);
FIG. 3 is an HPLC chromatogram of disodium lauryl sulfosuccinate prepared in comparative example 1 (wherein 2.80min is the sodium ion peak of the product).
Detailed Description
In order that the invention may be more readily understood, reference will now be made to the following more particular description of the invention, examples of which are set forth below. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. These embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
A preparation method of fatty alcohol sulfosuccinic acid monoester disodium salt comprises the following steps:
(1) mixing fatty alcohol, an alkaline catalyst and maleic anhydride, and reacting at 70-90 ℃;
(2) mixing the reaction product obtained in the step (1) with a washing solvent, heating to 40-80 ℃, and separating to obtain upper-layer liquid;
(3) mixing the upper layer liquid with an aqueous solution of sodium sulfite, and reacting at 70-90 ℃;
the washing solvent is selected from water, aqueous solutions of inorganic salts or aqueous solutions of weakly basic metal organic non-carbonates.
The reaction formula of the invention is as follows:
fatty alcohol and maleic anhydride are subjected to esterification reaction under proper temperature conditions and catalysis conditions to obtain an intermediate maleic acid fatty alcohol monoester. And then the maleic acid fatty alcohol monoester is sulfonated to obtain fatty alcohol sulfosuccinic acid monoester disodium salt.
In this process, maleic anhydride and water inevitably produce maleic acid due to moisture in the fatty alcohol, which may be further sulfonated as a by-product to produce sulfosuccinate. In addition, in order to fully react the fatty alcohol, an excess of maleic anhydride is usually added, which can also form the final sulfosuccinate by-product. Residues of the esterification catalyst can also form by-products that affect the purity of the final product.
Through a great deal of experimental research, the inventor of the application finds that the intermediate maleic acid fatty alcohol monoester has a carboxyl group with high polarity and an alkyl chain with low polarity. When the temperature is controlled to 40 to 80 ℃, it can be formed in a molten state in the specific washing solvent of the present invention and is insoluble in the washing solvent. If the temperature is lower than 40 ℃, the maleic acid fatty alcohol monoester is easy to solidify into a solid state and is not easy to separate from a washing solvent. When the temperature is more than 80 ℃, part of the maleic acid fatty alcohol monoester starts to be hydrolyzed, resulting in a reduction of the final yield. And when the temperature is 40-80 ℃, the compatibility of the residual by-product and the catalyst with the washing solvent is greater than that of the maleic fatty alcohol monoester, so that the catalyst is easy to dissolve in the washing solvent. At this time, the maleic acid fatty alcohol monoester in a molten state is layered with a by-product dissolved in the washing solvent and the catalyst, and the maleic acid fatty alcohol monoester having a smaller density is located in an upper layer and the washing solvent having a larger density is located in a lower layer. The maleic acid fatty alcohol monoester with higher purity of the upper layer can be obtained by simple separation.
When the washing solvent is weakly alkaline metal carbonate, the carbonate in the heating and washing process can react and decompose to generate carbon dioxide gas, so that the upper-layer liquid is not convenient to separate, impurities cannot be effectively removed, and the purity of the final product is greatly reduced.
In some of these embodiments, the inorganic salt is selected from at least one of sodium chloride, potassium chloride, sodium sulfate, disodium hydrogen phosphate, and potassium sulfate; and/or the weakly basic metal organic non-carbonate is disodium citrate.
In some of these embodiments, in step (2), the reaction product is mixed with a washing solvent and heated to 45-55 ℃.
In some of these embodiments, in step (1), the basic catalyst is at least one of anhydrous sodium acetate, anhydrous trisodium citrate, and anhydrous potassium carbonate. Preferably, the basic catalyst is anhydrous sodium acetate.
In some embodiments, the mass concentration of the inorganic salt in the aqueous solution of the inorganic salt is 1% to 10%; the mass concentration of the weak alkaline metal organic non-carbonate in the weak alkaline metal organic non-carbonate aqueous solution is 1-10%.
Specifically, the mass concentration of the inorganic salt in the aqueous solution of the inorganic salt is 3-5%; the mass concentration of the weak alkaline metal organic non-carbonate in the weak alkaline metal organic non-carbonate aqueous solution is 3-5%
In some of these embodiments, in step (1), the molar ratio of the fatty alcohol and the maleic anhydride is: 1:1-1.5. Preferably, the molar ratio of the fatty alcohol to the maleic anhydride is: 1: 1-1.1. Specifically, the molar ratio of the fatty alcohol to the maleic anhydride is: 1: 1.05.
in some of these embodiments, the mass of the basic catalyst is 0.8-1.2% of the mass of the fatty alcohol. Preferably, the mass of the alkaline catalyst is 1% of the mass of the fatty alcohol.
In some embodiments, in step (3), the mass concentration of the aqueous solution of sodium sulfite is 15-30%;
in some of the examples, in step (3), the aqueous solution of sodium sulfite has a mass concentration of 15 to 25%.
In some of these embodiments, in step (3), the molar ratio of the fatty alcohol to the sodium sulfite is: 1 (1-1.5); preferably, the molar ratio of the fatty alcohol to the sodium sulfite is: 1:(1-1.2). Specifically, the molar ratio of the fatty alcohol to the sodium sulfite is: 1:1.1.
In some embodiments, in step (3), the time for mixing and reacting the upper layer liquid with the sodium sulfite is (1-4) h.
In some of these embodiments, the fatty alcohol is a C8-C18 fatty alcohol.
In some of these embodiments, the fatty alcohol is n-decanol, lauryl alcohol, or tetradecanol.
The present invention will be described in further detail with reference to specific examples.
Example 1
(1) Esterification reaction: after the moisture content of lauryl alcohol is detected to be less than or equal to 0.5 percent by a card type moisture content analyzer, 1000g of lauryl alcohol and 10g of catalyst anhydrous sodium acetate are respectively added into a double-layer glass reaction kettle of 5 kg, nitrogen is introduced for protection, then the temperature is raised to 60 ℃, 553g of maleic anhydride is slowly added, the temperature in the system is maintained at 80 ℃, the reaction is carried out for 3 hours, the acid value of the system is detected to be basically constant, and the reaction is stopped.
(2) Washing and purifying: adding a washing solvent of disodium hydrogen phosphate aqueous solution with the mass concentration of 3% into the reaction liquid obtained in the step (1), wherein the mass is 1563 g. Heating to maintain the temperature in the system at 50 deg.C, maintaining the esterified intermediate in molten state, stirring for 20 min, standing, separating the two phases in the reaction kettle, and discharging the lower layer water solution. The intermediate esterified product of the upper layer was used for the next reaction.
(3) And (3) sulfonation reaction: slowly adding 3023g of sodium sulfite deionized solution with the mass concentration of 24.67% into the upper intermediate ester obtained in the step (2), maintaining the reaction system at 80 ℃, reacting for 3 hours, and stopping the reaction after the sodium sulfite content is measured to be less than or equal to 0.5%. Cooling to 65 ℃, discharging, detecting that 0.98% of fatty alcohol and 4.14% of trisodium sulfosuccinate content are contained, and obtaining the product disodium lauryl sulfosuccinate paste with the mass of 4514g, the solid content of 50.17% and the purity of: 94.87 percent.
Example 2
(1) Esterification reaction: after the moisture content of the n-decanol is detected to be less than or equal to 0.5 percent by a card type moisture content analyzer, 1000g of the n-decanol and 10g of anhydrous sodium acetate serving as a catalyst are respectively added into a double-layer glass reaction kettle of 5 kg, nitrogen is introduced for protection, then the temperature is raised to 60 ℃, 650.5g of maleic anhydride is slowly added, the temperature in the system is maintained at 80 ℃, the reaction is carried out for 3 hours, the acid value of the detection system is basically constant, and the reaction is stopped.
(2) Washing and purifying: and (2) adding a washing solvent of 3% disodium hydrogen phosphate aqueous solution by mass into the reaction solution obtained in the step (1), wherein the mass is 1660 g. Heating to maintain the temperature in the system at 50 deg.C, maintaining the esterified intermediate in molten state, stirring for 20 min, standing, separating the two phases in the reaction kettle, and discharging the lower layer water solution. The intermediate esterified product of the upper layer was used for the next reaction.
(3) And (3) sulfonation reaction: slowly adding 3023g of sodium sulfite supersaturated deionized solution with the mass concentration of 25.97% into the upper intermediate esterified substance obtained in the step (2), maintaining the reaction system at 80 ℃, reacting for 3 hours, and stopping the reaction after the sodium sulfite content is measured to be less than or equal to 0.5%. Cooling to 65 ℃, discharging, detecting that 1.0% of fatty alcohol and 3.41% of trisodium sulfosuccinate content are contained, and obtaining the product of the disodium n-decanol sulfosuccinate paste with the mass of 4713g, the solid content of 50.53%, and the purity: 95.41 percent.
Example 3
(1) Esterification reaction: after the moisture content of the tetradecanol is detected to be less than or equal to 0.5 percent by a card type moisture content analyzer, 1000g of tetradecanol and 10g of anhydrous sodium acetate serving as a catalyst are respectively added into a double-layer glass reaction kettle of 5 kg, nitrogen is introduced for protection, then the temperature is raised to 60 ℃, 480g of maleic anhydride is slowly added, the temperature in the system is maintained at 80 ℃, the reaction is carried out for 3 hours, the acid value of the detection system is basically constant, and the reaction is stopped.
(2) Washing and purifying: and (2) adding a washing solvent of 3% disodium hydrogen phosphate aqueous solution with the mass concentration into the reaction solution obtained in the step (1), wherein the mass is 1490 g. Heating to maintain the temperature in the system at 50 deg.C, maintaining the esterified intermediate in molten state, stirring for 20 min, standing, separating the two phases in the reaction kettle, and discharging the lower layer water solution. The intermediate esterified product of the upper layer was used for the next reaction.
(3) And (3) sulfonation reaction: slowly adding 2760g of sodium sulfite deionized solution with the mass concentration of 23.50% into the upper-layer intermediate ester obtained in the step (2), maintaining the reaction system at 80 ℃, reacting for 3 hours, and stopping the reaction after the sodium sulfite content is less than or equal to 0.5%. Cooling to 70 ℃, discharging, detecting that the tetradecanol is 1.23 percent, the content of the trisodium sulfosuccinate is 5.36 percent, and obtaining the product disodium tetradecanol sulfosuccinate paste with the mass of 4206g, the solid content of 49.90 percent and the purity: 93.75 percent.
Example 4
(1) Esterification reaction: after the moisture content of lauryl alcohol is detected to be less than or equal to 0.5 percent by a card type moisture content analyzer, 1000g of lauryl alcohol and 10g of catalyst anhydrous sodium acetate are respectively added into a double-layer glass reaction kettle of 5 kg, nitrogen is introduced for protection, then the temperature is raised to 60 ℃, 553g of maleic anhydride is slowly added, the temperature in the system is maintained at 80 ℃, the reaction is carried out for 3 hours, the acid value of the system is detected to be basically constant, and the reaction is stopped.
(2) Washing and purifying: adding a washing solvent of a disodium citrate aqueous solution with the mass concentration of 3% into the reaction solution obtained in the step (1), wherein the mass is 1564 g. Heating to maintain the temperature in the system at 50 deg.C, maintaining the esterified intermediate in molten state, stirring for 20 min, standing, separating the two phases in the reaction kettle, and discharging the lower layer water solution. The intermediate esterified product of the upper layer was used for the next reaction.
(3) And (3) sulfonation reaction: slowly adding 3023g of sodium sulfite deionized solution with the mass concentration of 24.67% into the upper intermediate ester obtained in the step (2), maintaining the reaction system at 80 ℃, reacting for 3 hours, and stopping the reaction after the sodium sulfite content is measured to be less than or equal to 0.5%. Cooling to 65 ℃, discharging, detecting that 1.66% of fatty alcohol and 6.18% of trisodium sulfosuccinate content are contained, and obtaining the product disodium lauryl sulfosuccinate paste with 4493g of mass, 50.02% of solid content and purity: 92.08 percent.
Example 5
(1) Esterification reaction: after the moisture content of lauryl alcohol is detected to be less than or equal to 0.5 percent by a card type moisture content analyzer, 1000g of lauryl alcohol and 10g of catalyst anhydrous sodium acetate are respectively added into a double-layer glass reaction kettle of 5 kg, nitrogen is introduced for protection, then the temperature is raised to 60 ℃, 553g of maleic anhydride is slowly added, the temperature in the system is maintained at 80 ℃, the reaction is carried out for 3 hours, the acid value of the system is detected to be basically constant, and the reaction is stopped.
(2) Washing and purifying: the reaction solution obtained in step (1) was added with a washing solvent of a 5% sodium chloride aqueous solution by mass, and the mass was 1564 g. Heating to maintain the temperature in the system at 50 deg.C, maintaining the esterified intermediate in molten state, stirring for 20 min, standing, separating the two phases in the reaction kettle, and discharging the lower layer water solution. The intermediate esterified product of the upper layer was used for the next reaction.
(3) And (3) sulfonation reaction: slowly adding 3023g of sodium sulfite deionized solution with the mass concentration of 24.67% into the upper intermediate ester obtained in the step (2), maintaining the reaction system at 80 ℃, reacting for 3 hours, and stopping the reaction after the sodium sulfite content is measured to be less than or equal to 0.5%. Cooling to 65 ℃, discharging, detecting that 1.53 percent of fatty alcohol and 6.63 percent of trisodium sulfosuccinate content, and obtaining the product disodium lauryl sulfosuccinate paste with 4490g of mass, 50.17 percent of solid content and purity: 91.81 percent.
Example 6
(1) Esterification reaction: after the moisture content of lauryl alcohol is detected to be less than or equal to 0.5 percent by a card type moisture content analyzer, 1000g of lauryl alcohol and 10g of catalyst anhydrous sodium acetate are respectively added into a double-layer glass reaction kettle of 5 kg, nitrogen is introduced for protection, then the temperature is raised to 60 ℃, 553g of maleic anhydride is slowly added, the temperature in the system is maintained at 80 ℃, the reaction is carried out for 3 hours, the acid value of the system is detected to be basically constant, and the reaction is stopped.
(2) Washing and purifying: tap water with the mass of 1564g was added to the reaction solution obtained in step (1). Heating to maintain the temperature in the system at 50 deg.C, maintaining the esterified intermediate in molten state, stirring for 20 min, standing, separating the two phases in the reaction kettle, and discharging the lower layer water solution. The intermediate esterified product of the upper layer was used for the next reaction.
(3) And (3) sulfonation reaction: slowly adding the upper layer intermediate ester obtained in the step (2) into 3023g of sodium sulfite deionized solution with the mass concentration of 24.67%, maintaining the reaction system at 80 ℃, reacting for 3 hours, and stopping the reaction after the sodium sulfite content is measured to be less than or equal to 0.5%. Cooling to 65 ℃, discharging, detecting that the fatty alcohol is 1.82 percent, the content of the trisodium sulfosuccinate is 6.55 percent, and obtaining the product disodium lauryl sulfosuccinate paste with the mass of 4504g, the solid content of 50.22 percent and the purity of: 91.57 percent.
Comparative example 1
(1) Esterification reaction: after the moisture content of lauryl alcohol is detected to be less than or equal to 0.5 percent by a card type moisture content analyzer, 1000g of lauryl alcohol and 10g of catalyst anhydrous sodium acetate are respectively added into a double-layer glass reaction kettle of 5 kg, nitrogen is introduced for protection, then the temperature is raised to 60 ℃, 553g of maleic anhydride is slowly added, the temperature in the system is maintained at 80 ℃, the reaction is carried out for 3 hours, the acid value of the system is detected to be basically constant, and the reaction is stopped.
(2) And (3) sulfonation reaction: slowly adding the intermediate ester obtained in the step (1) into 3023g of sodium sulfite deionized solution with the mass concentration of 24.67%, maintaining the reaction system at 80 ℃, reacting for 3 hours, and stopping the reaction after the sodium sulfite content is measured to be less than or equal to 0.5%. Cooling to 65 ℃, discharging, detecting that the fatty alcohol is 2.54 percent, the content of the trisodium sulfosuccinate is 12.01 percent, and obtaining the product disodium lauryl sulfosuccinate paste with the mass of 4500g, the solid content of 50.00 percent and the purity of: 85.29 percent.
Comparative example 2
(1) Esterification reaction: after the moisture content of lauryl alcohol is detected to be less than or equal to 0.5 percent by a card type moisture content analyzer, 1000g of lauryl alcohol and 10g of catalyst anhydrous sodium acetate are respectively added into a double-layer glass reaction kettle of 5 kg, nitrogen is introduced for protection, then the temperature is raised to 60 ℃, 553g of maleic anhydride is slowly added, the temperature in the system is maintained at 80 ℃, the reaction is carried out for 3 hours, the acid value of the system is detected to be basically constant, and the reaction is stopped.
(2) Washing and purifying: adding a washing solvent of disodium hydrogen phosphate aqueous solution with the mass concentration of 3% into the reaction liquid obtained in the step (1), wherein the mass is 1563 g. Heating to maintain the temperature in the system at 95 deg.C, maintaining the esterified intermediate in molten state, stirring for 20 min, standing, separating the two phases in the reaction kettle, and discharging the lower aqueous solution. The intermediate esterified product of the upper layer was used for the next reaction.
(3) And (3) sulfonation reaction: slowly adding the upper layer intermediate ester obtained in the step (2) into 3023g of sodium sulfite deionized solution with the mass concentration of 24.67%, maintaining the reaction system at 80 ℃, reacting for 3 hours, and stopping the reaction after the sodium sulfite content is measured to be less than or equal to 0.5%. After cooling to 65 ℃, discharging, detecting that the fatty alcohol is 4.61 percent, the content of the trisodium sulfosuccinate is 9.14 percent, and obtaining the product disodium lauryl sulfosuccinate paste with the mass of 4503g, the solid content of 49.96 percent and the purity of 86.13 percent.
Comparative example 3
1) Esterification reaction: after the moisture content of lauryl alcohol is detected to be less than or equal to 0.5 percent by a card type moisture content analyzer, 1000g of lauryl alcohol and 10g of catalyst anhydrous sodium acetate are respectively added into a double-layer glass reaction kettle of 5 kg, nitrogen is introduced for protection, then the temperature is raised to 60 ℃, 553g of maleic anhydride is slowly added, the temperature in the system is maintained at 80 ℃, the reaction is carried out for 3 hours, the acid value of the system is detected to be basically constant, and the reaction is stopped.
(2) Washing and purifying: adding a hydrochloric acid solution with the mass concentration of about 3% into the reaction liquid obtained in the step (1) to wash a solvent, wherein the mass of the hydrochloric acid solution is 1563 g. Heating to maintain the temperature in the system at 50 deg.C, maintaining the esterified intermediate in molten state, stirring for 20 min, standing, separating the two phases in the reaction kettle, and discharging the lower layer water solution. The intermediate esterified product of the upper layer was used for the next reaction.
(3) And (3) sulfonation reaction: slowly adding the upper layer intermediate ester obtained in the step (2) into 3023g of sodium sulfite deionized solution with the mass concentration of 24.67%, maintaining the reaction system at 80 ℃, reacting for 3 hours, and stopping the reaction after the sodium sulfite content is measured to be less than or equal to 0.5%. Cooling to 65 ℃, discharging, detecting 6.68% of fatty alcohol and 11.93% of trisodium sulfosuccinate, and obtaining the product disodium lauryl sulfosuccinate with the mass of 4506g, the solid content of 50.05%, and the purity of: 81.34 percent.
In the method, a washing and purifying step is added to the preparation process of the disodium lauryl alcohol sulfosuccinate, and other preferable test conditions are matched, so that the disodium lauryl alcohol sulfosuccinate with high purity and high quality is finally obtained. Wherein, the kind of the washing solvent and the different purification temperature in the step (2) have a great influence on the quality of the obtained disodium lauryl sulfosuccinate product. In the absence of the washing purification step of the present invention in comparative example 1, the selection of a higher purification temperature in step (2) in comparative example 2, and the selection of other washing solvents in comparative example 3, the impurity content in the objective fatty alcohol sulfosuccinic acid monoester disodium salt was significantly increased. In addition, the inventor finds that when the washing solvent is weakly alkaline metal carbonate, the carbonate in the heating and washing process can be decomposed to generate carbon dioxide gas, so that the upper layer liquid is inconvenient to separate, impurities cannot be effectively removed, and finally the purity of the final product can be greatly reduced.
From examples 1 to 5, it can be seen that the present invention, through a large number of experimental studies, selects water, an aqueous solution of an inorganic salt or an aqueous solution of a weakly basic metal organic non-carbonate as a washing solvent, which can selectively dissolve impurities such as a catalyst and byproducts remaining at 40 to 80 ℃. Furthermore, the maleic acid fatty alcohol monoester is in a molten state at 40-80 ℃, and is hardly soluble in a washing solvent. Therefore, impurities dissolved in the washing solvent can be separated from the intermediate maleic acid fatty alcohol monoester to form incompatible two phases, so that the impurity content in the intermediate maleic acid fatty alcohol monoester is greatly reduced, the high-purity maleic acid fatty alcohol monoester is obtained, and finally the purity of the target product fatty alcohol sulfo succinic acid monoester disodium salt is obviously improved.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of fatty alcohol sulfosuccinic acid monoester disodium salt is characterized by comprising the following steps:
(1) mixing fatty alcohol, an alkaline catalyst and maleic anhydride, and reacting at 70-90 ℃;
(2) mixing the reaction product obtained in the step (1) with a washing solvent, heating to 40-80 ℃, and separating to obtain upper-layer liquid;
(3) mixing the upper layer liquid with an aqueous solution of sodium sulfite, and reacting at 70-90 ℃;
the washing solvent is water, an aqueous solution of an inorganic salt or an aqueous solution of a weakly basic metal organic non-carbonate.
2. The method according to claim 1, wherein the inorganic salt is at least one selected from the group consisting of sodium chloride, potassium chloride, sodium sulfate, disodium hydrogen phosphate, and potassium sulfate; the alkalescent metal organic non-carbonate is disodium citrate.
3. The method according to claim 1, wherein in the step (2), the reaction product is mixed with a washing solvent and then heated to 45 to 55 ℃.
4. The preparation method according to claim 1, wherein in the step (1), the basic catalyst is at least one of anhydrous sodium acetate, anhydrous trisodium citrate and anhydrous potassium carbonate; the mass concentration of the inorganic salt in the aqueous solution of the inorganic salt is 1-10%; the mass concentration of the weak alkaline metal organic non-carbonate in the weak alkaline metal organic non-carbonate aqueous solution is 1-10%.
5. The method according to claim 1, wherein in the step (1), the molar ratio of the fatty alcohol to the maleic anhydride is: 1:1-1.5.
6. The method according to claim 1, wherein in the step (3), the mass concentration of sodium sulfite in the aqueous solution of sodium sulfite is 15 to 25%.
7. The method according to claim 6, wherein in the step (3), the molar ratio of the fatty alcohol to the sodium sulfite is: 1:1-1.5.
8. The process according to any one of claims 1 to 7, wherein in the step (3), the time for mixing and reacting the supernatant liquid with the sodium sulfite is 1 to 4 hours.
9. The method according to any one of claims 1 to 7, wherein the fatty alcohol is a C8-C18 fatty alcohol.
10. The method of claim 9, wherein the fatty alcohol is n-decyl alcohol, lauryl alcohol, or tetradecyl alcohol.
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