CN107459455B - Method for extracting methyl stearate from benzoyl methane stearate residual liquid - Google Patents
Method for extracting methyl stearate from benzoyl methane stearate residual liquid Download PDFInfo
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- CN107459455B CN107459455B CN201610383201.3A CN201610383201A CN107459455B CN 107459455 B CN107459455 B CN 107459455B CN 201610383201 A CN201610383201 A CN 201610383201A CN 107459455 B CN107459455 B CN 107459455B
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Abstract
The invention discloses a method for extracting methyl stearate from benzoyl methane stearate residual liquid, and belongs to the field of chemical engineering. The specific scheme is that SBM residual liquid is introduced into a vacuum rectification tower, after vacuum rectification, components with a boiling point lower than that of methyl stearate flow out from the tower top, and methyl stearate and heavy components flow out from the tower bottom. The bottom effluent is extracted with liquid-liquid to separate methyl stearate with purity over 85%. The method separates methyl stearate with the purity of more than 85 percent from the benzoyl stearate residual liquid, and meanwhile, the yield can reach more than 85 percent. Compared with the prior art, the method has the advantages of simple process, easy operation and higher purity and yield of the obtained methyl stearate.
Description
Technical Field
The invention belongs to the field of chemical engineering, and particularly relates to a method for extracting methyl stearate from benzoyl methane stearate residual liquid.
Background
The production method of Stearoylbenzoylmethane (SBM) is characterized by that after the condensation, acidification and concentration steps of acetophenone, methyl stearate and sodium methoxide are implemented, the obtained solid crude product is dissolved in crystallization solvent to make crystallization, and the filtered crystallized product is dried so as to obtain the stearoylbenzoylmethane product. The Stearoylbenzoylmethane (SBM) raffinate is the raffinate left after crystallization separation of a product in the SBM production process and recovery of a solvent from a mother liquor through distillation, and the content of methyl stearate in the raffinate is about 60 percent, but the SBM raffinate has complex components and high boiling points of most of the components, so that the methyl stearate in the raffinate is difficult to separate. Patent CN201210332441 discloses a method for extracting methyl stearate from SBM raffinate, which adopts a methanol extraction crystallization method to extract methyl stearate from SBM raffinate, but the content of methyl stearate obtained by extraction is low, and the yield of methyl stearate is low due to the complex process.
Disclosure of Invention
The invention provides a method combining reduced pressure distillation and extraction aiming at the current situation that the purity and yield of methyl stearate extracted from SBM raffinate are low, and methyl stearate is separated from SBM raffinate. The SBM residual liquid has complex composition and similar boiling point, and can be coked at higher temperature, the invention focuses on keeping lower temperature in the process of separating the methyl stearate, so the methyl stearate in the SBM residual liquid is enriched by adopting a reduced pressure distillation method, and the methyl stearate with higher purity is obtained by adopting an extraction process subsequently. The method has simple process and easy operation, can extract the methyl stearate with the purity of more than 85 percent from the SBM residual liquid, and simultaneously, the yield can reach more than 85 percent.
The technical scheme provided by the invention is as follows:
(1) and (3) reduced pressure distillation: introducing the stearoylbenzoylmethane residual liquid into a vacuum rectification tower, wherein the pressure of the vacuum rectification tower is 0.6 KPa-10 KPa, the temperature of a tower kettle is 160-200 ℃, the number of theoretical plates of the vacuum rectification tower is 20-40, the reflux ratio is 2-5, after vacuum rectification, components with the boiling point lower than that of methyl stearate flow out of the tower top, and the methyl stearate and heavy components flow out of the tower bottom;
(2) liquid-liquid extraction: introducing the methyl stearate enrichment liquid into an extraction tower, wherein the operating temperature of the extraction tower is 20-60 ℃, the mass ratio of an extracting agent to the methyl stearate enrichment liquid is 1-3: 1, the methyl stearate enrichment liquid enters from the upper part of the extraction tower, the extracting agent enters from the lower part of the extraction tower, and after countercurrent extraction, methyl stearate flows out from the bottom of the extraction tower.
In the technical scheme, the pressure of the reduced pressure distillation tower is 0.6KPa to 10KPa, the number of theoretical plates of the reduced pressure distillation tower is 20 to 40, the reflux ratio is 2 to 5, and the temperature of a tower kettle is 160 ℃ to 200 ℃.
In the technical scheme, the extracting agent is organic solvent such as sulfolane, N-methyl pyrrolidone and the like. The operating temperature of the extraction tower is 20-60 ℃, the number of theoretical plates of the extraction tower is 8-12, and the mass ratio of the extracting agent to the solution to be extracted is 1-3: 1.
Introducing the SBM residual liquid into a vacuum rectification tower, and after vacuum rectification, enabling components with a boiling point lower than that of methyl stearate to flow out of the tower top, and enabling methyl stearate and heavy components to flow out of the tower bottom. The bottom effluent is extracted with liquid-liquid to separate methyl stearate with purity over 85%.
Specifically, the steps of separating the SBM residual liquid by a method combining reduced pressure distillation and liquid-liquid extraction are as follows: introducing the SBM residual liquid into a vacuum rectification tower, wherein the number of theoretical plates of the vacuum rectification tower is more than 20, the tower pressure of the rectification tower is kept at 0.6 KPa-10 KPa, the temperature of a tower kettle is 160-200 ℃, the reflux ratio is 2-5, and through vacuum distillation, light components in the SBM residual liquid flow out of the tower top and methyl stearate enriched liquid flow out of the tower kettle. Introducing the methyl stearate concentrated solution into an extraction tower, wherein the operating temperature of the extraction tower is 20-60 ℃, the number of theoretical plates of the extraction tower is 8-12, the mass ratio of an extracting agent to the methyl stearate concentrated solution is 1-3: 1, the methyl stearate concentrated solution enters from the upper part of the tower, the extracting agent enters from the lower part of the tower, and methyl stearate with the purity of 85% flows out from the bottom of the tower after countercurrent extraction.
Advantageous effects
The SBM residual liquid has complex composition and similar boiling points, most of components have higher boiling points and can be coked at higher temperature, the relative volatility between separated substances can be improved by adopting the vacuum rectification for enriching the methyl stearate on one hand, the enrichment of the methyl stearate is facilitated, and meanwhile, the operation temperature of a tower kettle is lower in the vacuum rectification process, so that the coking of high-boiling-point substances can be prevented. The methyl stearate enrichment liquid can reduce the coking of high boiling point substances by a normal temperature extraction method. Compared with the prior art, the method has the advantages that the process combining reduced pressure distillation and liquid-liquid extraction is adopted, the process is simple, the operation is easy, and methyl stearate with higher purity can be obtained from the stearoylbenzoylmethane residual liquid.
Detailed Description
The following detailed description of the embodiments of the present invention is provided, but it should be noted that the scope of the present invention is not limited by the embodiments, but is defined by the appended claims.
Example 1
Introducing the SBM residual liquid into a vacuum rectification tower, wherein the number of theoretical plates of the vacuum rectification tower is 20, the tower pressure of the rectification tower is kept at 0.6KPa, the temperature of a tower kettle is 160 ℃, the reflux ratio is 5, light components in the SBM residual liquid flow out of the tower top through vacuum distillation, methyl stearate enriched liquid flows out of the tower kettle, and the purity of the methyl stearate is 75%. Introducing methyl stearate enrichment liquid into an extraction tower, wherein the methyl stearate enrichment liquid enters from the upper part of the extraction tower, sulfolane enters from the lower part of the extraction tower, the mass ratio of the sulfolane to the methyl stearate is 3: 1, the number of theoretical plates of the extraction tower is 10, the extraction temperature is 40 ℃, after countercurrent extraction, methyl stearate with the purity of 88% flows out from the bottom of the extraction tower, and the yield of the methyl stearate is 90%.
Example 2
Introducing the SBM residual liquid into a vacuum distillation tower, wherein the number of theoretical plates of the vacuum distillation tower is 20, the tower pressure of the distillation tower is kept at 10KPa, the temperature of a tower kettle is 200 ℃, the reflux ratio is 5, and through vacuum distillation, light components in the SBM residual liquid flow out of the tower top, methyl stearate enriched liquid flows out of the tower kettle, and the purity of the methyl stearate is 75%. Introducing methyl stearate enrichment liquid into an extraction tower, wherein the methyl stearate enrichment liquid enters from the upper part of the extraction tower, sulfolane enters from the lower part of the extraction tower, the mass ratio of the sulfolane to the methyl stearate is 3: 1, the number of theoretical plates of the extraction tower is 10, the extraction temperature is 40 ℃, after countercurrent extraction, methyl stearate with the purity of 88% flows out from the bottom of the extraction tower, and the yield of the methyl stearate is 90%.
Example 3
Introducing the SBM residual liquid into a vacuum distillation tower, wherein the number of theoretical plates of the vacuum distillation tower is 40, the tower pressure of the distillation tower is kept at 10KPa, the temperature of a tower kettle is 200 ℃, the reflux ratio is 3, through vacuum distillation, light components in the SBM residual liquid flow out of the tower top, methyl stearate enriched liquid flows out of the tower kettle, and the purity of the methyl stearate is 75%. Introducing methyl stearate enrichment liquid into an extraction tower, wherein the methyl stearate enrichment liquid enters from the upper part of the extraction tower, sulfolane enters from the lower part of the extraction tower, the mass ratio of the sulfolane to the methyl stearate is 3: 1, the number of theoretical plates of the extraction tower is 10, the extraction temperature is 40 ℃, after countercurrent extraction, methyl stearate with the purity of 88% flows out from the bottom of the extraction tower, and the yield of the methyl stearate is 90%.
Example 4
Introducing the SBM residual liquid into a vacuum distillation tower, wherein the number of theoretical plates of the vacuum distillation tower is 20, the tower pressure of the distillation tower is kept at 0.6KPa, the temperature of a tower kettle is 160 ℃, the reflux ratio is 2, light components in the SBM residual liquid flow out of the tower top through vacuum distillation, methyl stearate enriched liquid flows out of the tower kettle, and the purity of the methyl stearate is 73%. Introducing methyl stearate enrichment liquid into an extraction tower, wherein the methyl stearate enrichment liquid enters from the upper part of the extraction tower, sulfolane enters from the lower part of the extraction tower, the mass ratio of the sulfolane to the methyl stearate is 3: 1, the number of theoretical plates of the extraction tower is 10, the extraction temperature is 40 ℃, after countercurrent extraction, methyl stearate with the purity of 85% flows out from the bottom of the extraction tower, and the yield of the methyl stearate is 92%.
Example 5
Introducing the SBM residual liquid into a vacuum rectification tower, wherein the number of theoretical plates of the vacuum rectification tower is 20, the tower pressure of the rectification tower is kept at 0.6KPa, the temperature of a tower kettle is 160 ℃, the reflux ratio is 5, light components in the SBM residual liquid flow out of the tower top through vacuum distillation, methyl stearate enriched liquid flows out of the tower kettle, and the purity of the methyl stearate is 75%. Introducing methyl stearate enrichment liquid into an extraction tower, wherein the methyl stearate enrichment liquid enters from the upper part of the extraction tower, sulfolane enters from the lower part of the extraction tower, the mass ratio of the sulfolane to the methyl stearate is 1: 1, the number of theoretical plates of the extraction tower is 10, the extraction temperature is 40 ℃, after countercurrent extraction, methyl stearate with the purity of 85% flows out from the bottom of the extraction tower, and the yield of the methyl stearate is 90%.
Example 6
Introducing the SBM residual liquid into a vacuum rectification tower, wherein the number of theoretical plates of the vacuum rectification tower is 20, the tower pressure of the rectification tower is kept at 0.6KPa, the temperature of a tower kettle is 160 ℃, the reflux ratio is 5, light components in the SBM residual liquid flow out of the tower top through vacuum distillation, methyl stearate enriched liquid flows out of the tower kettle, and the purity of the methyl stearate is 75%. Introducing methyl stearate enrichment liquid into an extraction tower, wherein the methyl stearate enrichment liquid enters from the upper part of the extraction tower, N-methyl pyrrolidone enters from the lower part of the extraction tower, the mass ratio of the N-methyl pyrrolidone to the methyl stearate is 3: 1, the theoretical plate number of the extraction tower is 10, the extraction temperature is 40 ℃, methyl stearate with the purity of 87% flows out from the bottom of the extraction tower after countercurrent extraction, and the yield of the methyl stearate is 90%.
Example 7
Introducing the SBM residual liquid into a vacuum rectification tower, wherein the number of theoretical plates of the vacuum rectification tower is 20, the tower pressure of the rectification tower is kept at 0.6KPa, the temperature of a tower kettle is 160 ℃, the reflux ratio is 5, light components in the SBM residual liquid flow out of the tower top through vacuum distillation, methyl stearate enriched liquid flows out of the tower kettle, and the purity of the methyl stearate is 75%. Introducing methyl stearate enrichment liquid into an extraction tower, wherein the methyl stearate enrichment liquid enters from the upper part of the extraction tower, sulfolane enters from the lower part of the extraction tower, the mass ratio of the sulfolane to the methyl stearate is 3: 1, the number of theoretical plates of the extraction tower is 10, the extraction temperature is 20 ℃, after countercurrent extraction, methyl stearate with the purity of 85% flows out from the bottom of the extraction tower, and the yield of the methyl stearate is 90%.
Example 8
Introducing the SBM residual liquid into a vacuum rectification tower, wherein the number of theoretical plates of the vacuum rectification tower is 20, the tower pressure of the rectification tower is kept at 0.6KPa, the temperature of a tower kettle is 160 ℃, the reflux ratio is 5, light components in the SBM residual liquid flow out of the tower top through vacuum distillation, methyl stearate enriched liquid flows out of the tower kettle, and the purity of the methyl stearate is 75%. Introducing methyl stearate enrichment liquid into an extraction tower, wherein the methyl stearate enrichment liquid enters from the upper part of the extraction tower, sulfolane enters from the lower part of the extraction tower, the mass ratio of the sulfolane to the methyl stearate is 3: 1, the number of theoretical plates of the extraction tower is 10, the extraction temperature is 60 ℃, after countercurrent extraction, methyl stearate with the purity of 86% flows out from the bottom of the extraction tower, and the yield of the methyl stearate is 90%.
Example 9
Introducing the SBM residual liquid into a vacuum rectification tower, wherein the number of theoretical plates of the vacuum rectification tower is 20, the tower pressure of the rectification tower is kept at 0.6KPa, the temperature of a tower kettle is 160 ℃, the reflux ratio is 5, light components in the SBM residual liquid flow out of the tower top through vacuum distillation, methyl stearate enriched liquid flows out of the tower kettle, and the purity of the methyl stearate is 75%. Introducing methyl stearate enrichment liquid into an extraction tower, wherein the methyl stearate enrichment liquid enters from the upper part of the extraction tower, N-methyl pyrrolidone enters from the lower part of the extraction tower, the mass ratio of the N-methyl pyrrolidone to the methyl stearate is 3: 1, the theoretical plate number of the extraction tower is 10, the extraction temperature is 40 ℃, methyl stearate with the purity of 88% flows out from the bottom of the extraction tower after countercurrent extraction, and the yield of the methyl stearate is 90%.
Although the embodiments of the present invention have been described in detail with reference to the examples, it should be noted that the scope of the present invention is not limited by the embodiments, but is defined by the claims. Those skilled in the art can appropriately modify the embodiments without departing from the technical spirit and scope of the present invention, and the modified embodiments are also clearly included in the scope of the present invention.
Claims (2)
1. A method for extracting methyl stearate from benzoyl methane residual liquid of stearic acid is characterized in that:
(1) and (3) reduced pressure distillation: introducing the stearoylbenzoylmethane residual liquid into a vacuum rectification tower, wherein the pressure of the vacuum rectification tower is 0.6 KPa-10 KPa, the temperature of a tower kettle is 160-200 ℃, the number of theoretical plates of the vacuum rectification tower is 20-40, the reflux ratio is 2-5, after vacuum rectification, components with the boiling point lower than that of methyl stearate flow out of the tower top, and the methyl stearate and heavy components flow out of the tower bottom;
(2) liquid-liquid extraction: introducing the methyl stearate concentrated solution into an extraction tower, wherein the operating temperature of the extraction tower is 20-60 ℃, and the mass ratio of an extracting agent to the methyl stearate concentrated solution is 1-3: 1, methyl stearate enrichment liquid enters from the upper part of the tower, an extracting agent enters from the lower part of the tower, and after countercurrent extraction, methyl stearate flows out from the bottom of the tower;
the extractant is sulfolane or N-methyl pyrrolidone.
2. The method of claim 1, wherein: the number of the theoretical plates of the extraction tower is 8-12.
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| AU676689B2 (en) * | 1992-11-06 | 1997-03-20 | Rhone-Poulenc Chimie | Beta-diketones, processes for making beta-diketones and use of beta-diketones as stabilizers for PVC |
| BRPI0803361A2 (en) * | 2008-06-30 | 2010-03-09 | Petroleo Brasileiro Sa | liquid-liquid extraction process for purifying solids for use as lubricants |
| CN101531580A (en) * | 2009-03-17 | 2009-09-16 | 蚌埠佳先化工有限公司 | Crystallization method of stearoylbenzoylmethane |
| CN102503793B (en) * | 2011-11-23 | 2014-03-19 | 山东瑞丰高分子材料股份有限公司 | Preparation method of stearoylbenzoylmethane and application thereof in molding processing of thermoplastic resin |
| CN102898303A (en) * | 2012-09-11 | 2013-01-30 | 安徽佳先功能助剂股份有限公司 | Method for extracting methyl stearate from stearoylbenzoylmethane raffinate |
| CN103396310B (en) * | 2013-07-25 | 2015-02-25 | 浙江大学 | Method for separating and purifying eicosapentaenoic acid ester and docosahexenoic acid ester from micro-algal oil or fish oil |
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