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Ethylene glycol monobutyl ether benzoate and preparation method thereof

A technology of ethylene glycol monobutyl ether and benzoic acid is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as low boiling point, high cost, peculiar smell, etc. Low cost and high work efficiency

Inactive Publication Date: 2019-09-27
上海中溶科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the defects of existing products such as high cost, low boiling point, and peculiar smell, the present invention provides a low-cost, high boiling point, and clean-taste coalescent, namely ethylene glycol monobutyl ether benzoate, and a preparation method thereof

Method used

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  • Ethylene glycol monobutyl ether benzoate and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 1 mol of benzoic acid, 2 mol of ethylene glycol monobutyl ether, and 0.02 mol of concentrated sulfuric acid in a 1000 mL round bottom flask. The temperature was raised to 170°C for condensing and reflux reaction for 6 hours, and after the reaction was completed, it was cooled to room temperature, and the conversion rate of benzoic acid was 85.5% as tested by gas chromatography.

[0034] The reacted material is rectified in the rectification tower, and the pressure in the tower is about -0.095MPa. The top temperatures of the four towers are 42°C, 91°C, 125°C, and 180°C in sequence. The final product has a purity of 99.72% and no peculiar smell.

Embodiment 2

[0036] Add 1 mol of benzoic acid, 5 mol of ethylene glycol monobutyl ether, and 0.05 mol of p-toluenesulfonic acid in a 1000 mL round bottom flask. Raise the temperature to 170°C to condense and reflux for 12 hours. After the reaction, cool to room temperature. The conversion rate of benzoic acid is 96.5% as tested by gas chromatography.

[0037] The reacted material is rectified in the rectification tower, and the pressure in the tower is about -0.095MPa. The top temperatures of the four towers are 42°C, 90°C, 128°C, and 178°C in sequence. The final product has a purity of 99.85% and no peculiar smell.

Embodiment 3

[0039] 1 mol of benzoic acid, 3 mol of ethylene glycol monobutyl ether, and 0.001 mol of tetrabutyl titanate were successively added into a 1000 mL round bottom flask. The temperature was raised to 150°C for condensing and reflux reaction for 4 hours, and after the reaction was completed, it was cooled to room temperature, and the conversion rate of ethylene glycol monobutyl ether was 92.3% as tested by gas chromatography.

[0040] The reacted material is rectified in the rectification tower, and the pressure in the tower is about -0.090MPa. The top temperatures of the four towers are 45°C, 100°C, 130°C, and 180°C in sequence. The final product has a purity of 99.65% and no peculiar smell.

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Abstract

The invention relates to a preparation method of ethylene glycol monobutyl ether benzoate. The ethylene glycol monobutyl ether benzoate is prepared from the raw materials of benzoic acid and ethylene glycol monobutyl ether at a molar ratio of 1:(1-5); the adding molar weight of a catalyst is 0.1-5% of the molar weight of the benzoic acid; quantitative benzoic acid, ethylene glycol monobutyl ether and catalyst are sequentially added into a tank reactor; the total volume of the materials accounts for 30-70% of the total volume of the tank reactor; the reactor is heated to 120-200 DEG C, and then a heat preservation reaction is carried out for 4-12 h; after the reaction is finished, the reactor is cooled to room temperature; the materials which complete the reaction and are cooled are subjected to vacuum rectification by passing through a plurality of rectifying towers in sequence, wherein the pressure in each rectifying tower is between minus 0.090 and minus 0.098 Mpa (G); an ethylene glycol monobutyl ether benzoate finished product is collected by the last rectifying tower in the entire rectification process. According to the ethylene glycol monobutyl ether benzoate and the preparation method thereof, the boiling point is high, no foreign smell exists, and the cost is low; the raw materials of the ethylene glycol monobutyl ether benzoate are simple, the preparation process is simple, the control is easy, the work efficiency is high, and the product quality is good.

Description

technical field [0001] The invention belongs to the fine chemical industry field, specifically a kind of ethylene glycol monobutyl ether benzoate and preparation method thereof. Background technique [0002] At present, the PM2.5 content in the air in our country exceeds the standard, and the smog pollution is serious. The country attaches great importance to the prevention and control of air pollution, and the emission of volatile organic compounds (VOCs) accounts for about 21% of the main sources of air pollution. The most common consensus is that VOCs are those chemicals whose boiling point is equal to or lower than 250°C. The VOCs emissions of solvent-based coatings generally exceed the standard. In view of environmental protection factors, the use conditions will become more stringent. In order to reduce the impact of coatings on the environment and human health in the process of production and use, the National Environmental Protection Agency has continuously introduc...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/54C07C69/78
CPCC07C67/08C07C67/54C07C69/78
Inventor 吴超勇代淑梅李秋园
Owner 上海中溶科技有限公司
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