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Method for preparing low acid-value fatty acid methyl ester

A technology of fatty acid methyl ester and low acid value, applied in the preparation of carboxylate, sulfonate, preparation of organic compounds, etc., can solve the problems of long reaction time, many by-products, equipment corrosion, etc., and achieve a simple preparation process , the effect of high reactivity and low production cost

Active Publication Date: 2013-08-28
ZANYU TECH GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, sulfuric acid catalyst has disadvantages such as serious corrosion to equipment, large discharge of three wastes, complicated post-treatment, many by-products, poor reaction selectivity, carbonization of organic matter at high temperature, etc., and the reaction time is long, and the general cycle is more than 12 hours.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 35g 732 type cation exchange resin and 100g lauric acid (acid value 278.1mgKOH / g) in a 500mL three-necked bottle, place in a constant temperature oil bath, and install a thermometer, constant pressure dropping funnel, distillation Condenser, the end of the distillation condenser is connected to a vacuum pump; when the system temperature reaches 50°C, anhydrous methanol is slowly added through a constant pressure dropping funnel at a rate of about 10mL / h, and the vacuum pump is turned on to maintain a reaction pressure of 10Kpa. After reacting for 4 hours, the catalyst was filtered off, and excess methanol and generated water were further distilled off under reduced pressure to obtain methyl laurate with an acid value of 0.60 mgKOH / g and an esterification conversion rate of 99.78%.

Embodiment 2

[0027] Weigh 50g D001 type catalytic resin and 100g lauric acid (acid value 278.1mgKOH / g) in a 500mL three-necked bottle, place in a constant temperature oil bath, and install a thermometer, a constant pressure dropping funnel, a distillation condensing The end of the distillation condenser tube is connected to a vacuum pump; when the system temperature reaches 60°C, turn on the vacuum pump to maintain the reaction pressure at 30Kpa. Anhydrous methanol was slowly added through a constant pressure dropping funnel at a rate of about 15 mL / h. After reacting for 5 hours, the catalyst was filtered off, and the catalyst was washed with hot anhydrous ethanol three times, filtered, dried at 70°C, and recovered. The filtrate was further distilled off under reduced pressure to remove excess methanol and generated water to obtain methyl laurate with an acid value of 0.48 mgKOH / g and an esterification conversion rate of 99.82%.

Embodiment 3

[0029] Weigh 5g of p-toluenesulfonic acid and 100g of palmitic acid (acid value 218.3mgKOH / g) in a 500mL three-necked bottle, place it in a constant temperature oil bath, and install a thermometer, a constant pressure dropping funnel, a distillation condensing tube; when the temperature of the system reaches 55°C, keep the reaction pressure at 90Kpa, add anhydrous methanol slowly through the constant pressure dropping funnel, and the dropping rate is about 20mL / h. After reacting for 6 hours, the catalyst was filtered off. The catalyst was washed three times with hot absolute ethanol, filtered, dried at 70°C, and recovered. The filtrate was further distilled off under reduced pressure to remove excess methanol and generated water to obtain methyl laurate with an acid value of 0.52 mgKOH / g and an esterification conversion rate of 99.76%.

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PUM

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Abstract

The invention relates to a method for synthesizing low acid-value fatty acid methyl ester by esterification reaction and aims at providing the method with the characteristics that a process is simple; a catalyst and a product are easy to separate and can be recycled; the reaction conversion rate is high; and the obtained fatty acid methyl ester has low acid value. The method for preparing the lowacid-value fatty acid methyl ester sequentially comprises the following steps of: 1, feeding fatty acid and a resin catalyst together or feeding the fatty acid and a solid acid catalyst together, andthen heating the mixture with stirring; 2, after a temperature of a reaction system is raised to 50 to 80 DEG C, dropwise adding methanol into the reaction system, distilling the methanol and water generated in the reaction process, sampling and monitoring the reaction conversion rate in the reaction process and finishing the reaction until the acid value reaches below 0.5mgKOH / g, wherein the pressure of the reaction system is in the range of 10 to 101Kpa and the reaction time is in the range of 4 to 6 hours; and 3, after finishing the reaction, filtering out the catalyst, carrying out reduced pressure distillation on filtrate to separate out excessive methanol and water to obtain a finished product and directly recycling the resin catalyst or the solid acid catalyst.

Description

technical field [0001] The invention relates to the technical field of green and renewable energy, and specifically refers to a method for synthesizing fatty acid methyl ester with low acid value through esterification reaction of fatty acid and methanol under the catalysis of solid acid by adding methanol while distilling. Background technique [0002] Fatty acid methyl ester is a mild, stable structure, non-corrosive important surfactant raw material. Two types of surfactants can be produced from fatty acid methyl esters, one is the production of fatty acid methyl ester sulfonate (MES) through sulfonation and neutralization, and the other is the production of fatty alcohols through hydrogenation. 57% of fatty alcohols worldwide are produced from fatty acid methyl esters and 43% from fatty acids. [0003] At present, the production process of fatty acid methyl ester generally uses fatty acid and methanol as raw materials, and carries out esterification reaction under the a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/24C07C309/17C07C303/32
CPCY02P20/584
Inventor 冯耀平周大鹏葛赞黄亚茹史立文
Owner ZANYU TECH GRP CO LTD
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