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Method for preparing diethylene glycol dibenzoate

A technology of diethylene glycol dibenzoate and benzoic acid, which is applied in the field of preparing diethylene glycol dibenzoate by catalytic rectification, can solve the problems of long time, slow drainage process, and high catalyst cost, and can achieve equipment Low corrosiveness, small catalyst loss, and no environmental pollution

Inactive Publication Date: 2012-06-13
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN102172533A discloses a method for synthesizing a DEDB solid acid catalyst. The process is simpler than the previous processes, but the cost of the catalyst is relatively high
The process of draining water in ordinary tank reactors is very slow, and the time required for complete conversion of the reaction is very long

Method used

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  • Method for preparing diethylene glycol dibenzoate
  • Method for preparing diethylene glycol dibenzoate
  • Method for preparing diethylene glycol dibenzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] use figure 1 As shown in the flow process, the molar ratio of feed diethylene glycol and benzoic acid is: 1:1.8, the heating temperature of the batching tank is 100 ° C, the addition of catalyst tetrabutyl titanate is 0.9% of the total amount of materials, and the reflux ratio of the catalytic rectification tower is 2 : 1, the vacuum at the top of the tower is 0.09MPa, and the temperature is 140°C. Packing is filled in the catalytic rectification column, and a liquid distributor is installed every 3 meters of packing. The obtained result is as follows: water 90% in the tower top material, benzoic acid 10%, obtain DEDB product at the bottom of the tower and detect as follows through chromatography image 3 shown, and DEDB standard (see figure 2 ) after comparison, the product purity can reach 99%.

Embodiment 2

[0026] use figure 1 As shown in the flow process, the molar ratio of feed diethylene glycol and benzoic acid is: 1: 2.2, the heating temperature of the batching tank is 150 ° C, the addition of catalyst tetrabutyl titanate is 0.6% of the total amount of materials, and the reflux ratio of the catalytic rectification tower is 4 : 1, the vacuum at the top of the tower is 0.1MPa, and the temperature is 120°C. Packing is filled in the catalytic rectification column, and a liquid distributor is installed every 3 meters of packing. Gained result is as follows: water 85% in the tower top material, benzoic acid 15%, obtain DEDB product at the bottom of the tower through chromatographic detection such as Figure 4 shown, and DEDB standard (see figure 2 ) after comparison, the product purity can reach 99%.

Embodiment 3

[0028] use figure 1 As shown in the flow process, the molar ratio of feed diethylene glycol and benzoic acid is: 1:2.0, the heating temperature of the batching tank is 120 ° C, the addition of catalyst tetrabutyl titanate is 1.0% of the total amount of materials, and the reflux ratio of the catalytic rectification tower is 3 : 1, the vacuum at the top of the tower is 0.09MPa, and the temperature is 140°C. Packing is filled in the catalytic rectification column, and a liquid distributor is installed every 3 meters of packing. Gained result is as follows: water 85% in the tower top material, benzoic acid 15%, obtain DEDB product at the bottom of the tower through chromatographic detection such as Figure 5 shown, and DEDB standard (see figure 2 ) after comparison, the product purity can reach 99%.

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Abstract

The invention relates to a method for preparing diethylene glycol dibenzoate, and relates to the diethylene glycol dibenzoate. The invention provides a method which has a simple production process, is low in investment and energy-saving, is suitable for large-scale production and is used for preparing the diethylene glycol dibenzoate. The method comprises the following steps of: mixing benzoic acid and diethylene glycol in a batching kettle, heating, and inputting the mixture to the upper part of a catalytic rectifying tower by a pump; adding a catalyst from a feed inlet of the catalytic rectifying tower, and reacting by a catalytic rectifying section to obtain the diethylene glycol dibenzoate in a tower kettle; discharging water generated in reaction out of a liquid separation tank by a tower top material, and recovering the unreacted benzoic acid. The prepared diethylene glycol dibenzoate is high in purity and does not contain the diethylene glycol, and a subsequent process is avoided. The diethylene glycol dibenzoate is faint yellow liquid, is not needed to be decolorized further, is small in loss of a catalyst and small in corrosivity on equipment, does not have pollution on environment, and has high application value.

Description

Technical field [0001] The present invention relates to a diethylene glycol dibenzoate, and in particular to a method for preparing diethylene glycol dibenzoate by catalytic distillation. Background technique [0002] Diethylene glycol dibenzoate (DEDB) is a slightly light yellow transparent oily liquid and a new plasticizer. Compared with the traditional plasticizer phthalate (DOP), DEDB has good compatibility, good cold resistance, significant antistatic and anti-pollution properties, outstanding thermal stability, low volatility, and good resistance to light discoloration, etc. It has special characteristics and has low toxicity. Relevant foreign food, hospital, cosmetics and other departments consider it a plasticizer that can be used in food packaging materials and has good market prospects. [0003] At present, the industrial method of synthesizing DEDB mainly uses benzoic acid and diethylene glycol as raw materials, and uses concentrated sulfuric acid, heteropoly aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/78C07C67/08C07C67/54
CPCY02P20/10
Inventor 郑艳梅李清彪何宁孙道华王远鹏黄加乐王海涛
Owner XIAMEN UNIV
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