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Method for preparing triethyl citrate through using nanometer intercalated hydrotalcite catalyst

A technology of triethyl citrate and hydrotalcite, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve the problems of environmental pollution of waste acid, difficulty in post-treatment, carbonization of organic matter, etc. The product has high purity, saves the removal of miscellaneous processes, and is not easy to run off.

Inactive Publication Date: 2016-03-16
JIANGSU RUIJIA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For a long time, the synthesis of triethyl citrate is to use concentrated sulfuric acid as a catalyst. Due to the strong oxidizing property of concentrated sulfuric acid, it is easy to carbonize and oxidize organic matter, and the side reactions increase. The strong corrosiveness has a great impact on the service life of the equipment, and the discharge of a large amount of waste acid also pollutes the environment. Therefore, finding new environmentally friendly catalysts is the research focus of the industry
[0003] At present, some use aluminum chloride or strong solid acid to catalyze triethyl citrate, but these catalysts are not easy to remove impurities during use, and still cause side reactions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: a kind of method that nanoscale intercalation hydrotalcite catalyst prepares triethyl citrate comprises the steps:

[0025] Step a, feeding: Add nano-scale intercalated hydrotalcite catalyst, citric acid, and excess ethanol into the container, and stir evenly; when feeding, the molar ratio of citric acid to ethanol is 1: (5-6); citric acid and nano-scale The mass ratio of the intercalated hydrotalcite catalyst is 1: (0.03~0.05);

[0026] Step b. Esterification reaction: heating in an oil bath to maintain the reaction temperature between 100-110°C; during the heating process, continuously add ethanol dropwise until the ethanol is excessive, and at the same time condense and reflux to collect and evaporate ethanol; the esterification reaction time is 16-20 hours ;

[0027] Step c, purification: After the esterification reaction is completed, filter the nano-scale intercalated hydrotalcite catalyst, extract the residual ethanol in the reaction vessel from th...

Embodiment 2

[0029] Embodiment 2: The difference between this embodiment and Embodiment 1 is that in this embodiment, the nano-scale intercalated hydrotalcite catalyst is a kind of magnesium-aluminum hydrotalcite and zinc-aluminum hydrotalcite intercalated with multiple acids, The chemical formula of the anion of the polyacid used is [XM 11 CoO 39 ] n- , where X=P or Si; M=W or Mo; n is the valence number, n=5-6.

Embodiment 3

[0030] Embodiment 3: a kind of nanoscale intercalation hydrotalcite catalyst prepares the method for triethyl citrate, comprises the steps:

[0031] Step a, feeding: Add nano-scale intercalation hydrotalcite catalyst, citric acid, and excess ethanol into the container, and stir evenly; when feeding, the molar ratio of citric acid to ethanol is 1:5; citric acid and nano-scale intercalation hydrotalcite The mass ratio of the catalyst is 1:0.03;

[0032] Step b. Esterification reaction: heating in an oil bath to maintain the reaction temperature between 100-105°C; during the heating process, continuously add ethanol dropwise until the ethanol is excessive, and at the same time condense and reflux to collect and evaporate ethanol; the esterification reaction time is 15-18 hours ;

[0033]Step c, purification: After the esterification reaction is completed, filter the nano-scale intercalated hydrotalcite catalyst, extract the residual ethanol in the reaction vessel from the filtra...

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PUM

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Abstract

The invention discloses a method for preparing triethyl citrate through using a nanometer intercalated hydrotalcite catalyst. The method comprises the following steps: 1, charging: adding the nanometer intercalated hydrotalcite catalyst, citric acid and excess ethanol to a container, and stirring the added materials until uniformity; 2, carrying out an esterification reaction: carrying out oil bath heating, continuously adding ethanol in the heating process until ethanol is excess, and carrying out condensation refluxing and evaporated ethanol collection, wherein the esterification reaction is carried out for 16-20h; and 3, purifying: filtering out the nanometer intercalated hydrotalcite catalyst after the esterification reaction ends, dealcoholizing, neutralizing the dealcoholized material, washing the neutralized material with water, decolorizing the washed material, and purifying the decolorized material to obtain the finished triethyl citrate. The method for preparing triethyl citrate by using the nanometer intercalated hydrotalcite catalyst allows the citric acid conversion rate to be not lower than 99%, the product prepared in the invention is highly pure, the whole catalysis reaction is easy to operate, the temperature is easy to control, and the catalyst can be repeatedly used after being filtered.

Description

technical field [0001] The invention relates to a chemical catalysis method, in particular to a method for preparing triethyl citrate by using a hydrotalcite catalyst. Background technique [0002] Triethyl citrate (TEC) is a new type of non-toxic plasticizer, which can be used as deodorant, food additive, etc. Soluble in most organic solvents, and many cellulose and resins such as cellulose acetate, ethyl cellulose, polyvinyl chloride, vinyl chloride-vinyl acetate copolymer, polyvinyl butyral, polyvinyl acetate, chlorinated rubber, etc. Have good compatibility. As a plasticizer, due to the toxicity of DOP, the production of citric acid ester has been greatly developed abroad recently, such as Pricey Company and Morflex Company in the United States. Among them, triethyl citrate has been approved by the US Food Administration (FDA) as a non-toxic plasticizer, and is widely used in food packaging, medical appliances, children's toys, personal hygiene products, cigarette fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08B01J31/26
CPCC07C67/08B01J31/26B01J2231/49B01J2531/0216
Inventor 陈祥杨旭忠张勇赵重光
Owner JIANGSU RUIJIA CHEM
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