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Synthetic method of dichloropropanol aliphatic ester

A technology of dichloropropanol and fatty acid ester is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., which can solve the problems of complex products and high energy consumption, achieve good catalytic effect, stable performance, Stable quality effect

Active Publication Date: 2015-04-08
浙江嘉澳环保科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention provides a clean production method of fatty acid esters of dichloropropanol, which solves the shortcomings of complex products and high energy consumption caused by the current high-temperature production process, and solves the problem that commonly used solid acids cannot catalyze the reaction between fatty acids and dichloropropanol , simple operation process, green catalysis, catalyst recycling

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In the self-made fixed-bed reactor, fill the self-made modified ion resin catalyst (the filling amount of the catalyst is 5% of the total weight of fatty acid and dichloropropanol), set the temperature of the heating circulation liquid to be 60 ℃, weigh 6 grams of acetic acid, 15.8 grams of a mixture of 1,3-dichloropropanol and 2,3-dichloropropanol (the molar ratio of 1,3-dichloropropanol to 2,3-dichloropropanol is about 1:1) and Put 5 grams of cyclohexane in a glass container with a stopper, start the plunger metering pump after mixing, adjust the feed rate to 0.5ml / min, pass the feed liquid from bottom to top through the modified ion resin, and circulate the reaction for 2.5 After one hour, take a sample to test that the acid value is 1.05 mgKOH / g, and then take a sample after half an hour of reaction. The acid value is 1.03 mgKOH / g. After the reaction is over, the reaction mixture is collected and cooled to room temperature, and the mass fraction is 10% sodium hydroxi...

Embodiment 2

[0035]In the self-made fixed-bed reactor, fill the self-made modified ion resin catalyst (the filling amount of the catalyst is 8% of the total weight of fatty acid and dichloropropanol), set the temperature of the heating circulation liquid to be 80 ℃, weigh 14.2 grams of oleic acid, 8.4 grams of a mixture of 1,3-dichloropropanol and 2,3-dichloropropanol (the molar ratio of 1,3-dichloropropanol to 2,3-dichloropropanol is about 2:1 ) and 5 grams of hexanaphthene are placed in a glass container with a stopper, after mixing evenly, start the plunger metering pump, adjust the feed rate to be 0.8ml / min, pass the feed liquid from bottom to top through the modified ion resin, and circulate After reacting for 5 hours, take a sample to test that the acid value is 1.08mgKOH / g. After reacting for another hour, take a sample. The acid value is 1.06mgKOH / g. After reacting for another half an hour, take a sample. Collect and cool to room temperature, wash the reaction mixture with 12% aque...

Embodiment 3

[0037] In the self-made fixed-bed reactor, fill the self-made modified ion resin catalyst (the filling amount of the catalyst is 7% of the total weight of fatty acid and dichloropropanol), set the temperature of the heating circulation liquid to be 85 ℃, weigh 14 grams of stearic acid, 8.2 grams of mixture of 1,3-dichloropropanol and 2,3-dichloropropanol (the molar ratio of 1,3-dichloropropanol and 2,3-dichloropropanol is about 1: 5) Place 6 grams of cyclohexane in a glass container with a stopper, start the plunger metering pump after mixing, adjust the feed rate to 1.0ml / min, pass the feed liquid through the modified ion resin from bottom to top, After cyclic reaction for 5 hours, take a sample to test that the acid value is 1.07mgKOH / g. After another hour of reaction, take a sample and the acid value is 1.05mgKOH / g. After another half an hour of reaction, take a sample and the acid value is 1.05mgKOH / g. The mixture was collected and cooled to room temperature, the reaction ...

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Abstract

The invention discloses a synthetic method of dichloropropanol aliphatic ester. The synthetic method comprises the following steps: allowing fatty acid and dichloropropanol to have a esterification reaction under the catalysis of a modified ion resin catalyst; treating after the reaction is ended to obtain the dichloropropanol aliphatic ester, wherein the temperature of the esterification reaction is larger than or equal to 100 DEG C, and the modified ion resin catalyst is a SnCl4 modified and sulfonated polystyrene-divinylbenzene copolymer. The synthetic method of the dichloropropanol aliphatic ester, disclosed by the invention, has the remarkable technical effects and advantages that the transformation rate of the fatty acid is above 96.5%; the catalyst is good in catalytic effect, stable in performance, capable of being continuously used for 60 hours and not reduced obviously in catalytic effect; a solid bed reactor is adopted so that subsequent separation of the catalyst is avoided and reaction products are stable in quality.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, in particular to a method for synthesizing dichloropropanol fatty acid esters. Background technique [0002] Chloropropanol esters, including monochloro-substituted 3-chloro-1,2-propanediol (3-MCPD) esters and 2-chloro-1,3-propanediol (2-MCPD) esters and dichloro-substituted 1,3- Dichloro-2-propanol (1,3-DCP) and 2,3-chloro-1-propanol (2,3-DCP). It is mainly derived from acid hydrolyzed vegetable protein (HVP) and by-products in the refining of edible oils. [0003] At present, the synthesis of dichloropropanol esters is mostly obtained by the esterification of chloropropanol and fatty acid under the action of a catalyst at a high temperature of 200 °C. with There are two chlorine atoms on the carbon atom next to the alcoholic hydroxyl group, the structure is unstable, and the reaction product is complicated at high temperature. [0004] The reaction of fatty acid and dichloropropano...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/003C07C69/63C07C69/65
CPCB01J31/10B01J2231/49C07C67/08C07C69/003C07C69/63C07C69/65
Inventor 沈键傅俊红
Owner 浙江嘉澳环保科技股份有限公司