Method for continuously catalytically synthesizing triethyl citrate plasticizer

A technology of triethyl citrate and catalyst, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve the problems of long reaction time, high price, complicated post-treatment process, etc., and achieve high yield And the effect of high purity, low comprehensive cost, and no three wastes

Inactive Publication Date: 2012-09-12
KAIRUI ENVIRONMENTAL PROTECTION TECH
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  • Description
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AI Technical Summary

Problems solved by technology

[0005] The above patents have disadvantages such as easy loss of catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0018] Example 1:

[0019] The inner diameter of the reactor is Stainless steel tube, one in the center of the reactor The thermocouple temperature measuring tube is used to measure the temperature at any position between the inlet and the outlet of the reactor; the reactor is jacketed outside, and the reactor temperature is controlled by the high-speed flowing constant temperature water in the reactor jacket.

[0020] The citric acid and ethanol enter the reactor from the upper part of the isothermal fixed-bed integrating reactor for esterification reaction. The catalyst in the catalyst bed is 100ml. The reaction conditions are: alkyd ratio n (ethanol) / n (citric acid) = 2, empty Speed ​​1h -1 , The reaction pressure is 1MPa, the temperature is 60°C, and the reacted materials are discharged from the bottom of the reactor and enter the gas-liquid separator for separation. The unreacted ethanol is discharged from the upper part of the gas-liquid separator, and the triethyl citrate ...

Example Embodiment

[0021] Example 2

[0022] The reaction temperature was 40°C, and the others were the same as in Example 1. The resulting product number is KRB-2.

Example Embodiment

[0023] Example 3

[0024] The reaction temperature was 50°C, and the others were the same as in Example 1. The product number obtained is KRB-3.

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PUM

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Abstract

The invention relates to a method for continuously catalytically synthesizing triethyl citrate. The method comprises the following steps: taking citric acid and alcohol as raw materials; performing continuous catalytic esterification reaction on a fixed bed; taking a styrene cation exchange resin catalyst loaded with lewis acid as catalyst; filling the catalyst in the serially connected fixed bed; discharging materials after reacting from the bottom of a reactor and pouring into a gas-liquid separator for separating; discharging the unreacted alcohol from the upper part of the gas-liquid separator; discharging a triethyl citrate crude product from the bottom of the gas-liquid separator; and refining the triethyl citrate crude product, thereby obtaining the qualified product. According to the method provided by the invention, the esterification reaction yield is high, the reaction is free from corrosiveness and three wastes, the yield and the purity are high, and the comprehensive cost is low. The method is the most ideal and energy-saving production method for synthesizing the triethyl citrate at present and is worthy of quick popularization and application in industry.

Description

technical field [0001] The invention relates to a production method of triethyl citrate, in particular to a method for continuously catalytically synthesizing triethyl citrate. technical background [0002] Triethyl citrate has attracted wide attention because of its good compatibility, high plasticizing efficiency, non-toxicity, non-volatile, strong weather resistance, etc., and has become the first choice to replace phthalates as a green and environmentally friendly product. Triethyl citrate is synthesized by esterification of citric acid and ethanol under the action of a catalyst. The traditional esterification reaction has always used concentrated sulfuric acid as a catalyst. Although they all have good catalytic effects, due to the corrosion of equipment by sulfuric acid It is highly reactive and prone to side reactions. In recent years, many new catalysts have been developed to replace sulfuric acid. [0003] CN102079704A A method for preparing triethyl citrate. Throu...

Claims

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Application Information

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IPC IPC(8): C07C69/704C07C67/08
Inventor 王金明刘文飞
Owner KAIRUI ENVIRONMENTAL PROTECTION TECH
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