Method for preparing ethylene glycol phenyl ether, propylene glycol phenyl ether and butylene glycol phenyl ether

A technology of butanediol phenyl ether and propylene glycol phenyl ether, which is applied in the preparation of ether from alkylene oxide, ether preparation, organic chemistry, etc., can solve the problems of increased comprehensive cost, complicated operation control, and reduced economic benefits, and achieves easy maintenance, Simple operation and control, significant economic benefits

Inactive Publication Date: 2010-05-26
JIAHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the rectification process requires equipment such as distillation towers, it is prone to problems such as large equipment investment, high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: In a 2-liter autoclave, 940 g of phenol and 2.63 g of potassium hydroxide were added. After sealing the kettle, replace the air with nitrogen to ensure that the oxygen content in the kettle is less than 150ppm. Stir to raise the temperature, control the reaction temperature to 95-105°C, the reaction pressure is not higher than 0.04MPa, and add 374g of ethylene oxide. Close the ethylene oxide feed valve and age for 1 hour to obtain the crude product of ethylene glycol phenyl ether. Pour the crude product into a 2-liter distillation pot, raise the temperature to 83-93°C for vacuum distillation, and remove excess phenol. Keep the vacuum at 0.09MPa-0.10MPa, and distill for 3 hours to obtain a product of ethylene glycol phenyl ether with a purity of 99.12%.

Embodiment 2

[0016] Example 2: In a 2-liter autoclave, 1034 g of phenol and 2.21 g of monoethanolamine were added. After sealing the kettle, replace the air with nitrogen to ensure that the oxygen content in the kettle is less than 150ppm. Stir to raise the temperature, control the reaction temperature to 100-110°C, the reaction pressure is not higher than 0.06MPa, and add 436g of ethylene oxide. Close the ethylene oxide feed valve and age for 2 hours to obtain the crude product of ethylene glycol phenyl ether. Pour the crude product into a 2-liter still, heat up to 85-90°C for vacuum distillation, and remove excess phenol. Keep the vacuum at 0.08MPa-0.09MPa, and distill for 3 hours to obtain a product of ethylene glycol phenyl ether with a purity of 99.23%.

Embodiment 3

[0017] Embodiment 3: In a 2-liter autoclave, 940 g of phenol and 2.52 g of sodium hydroxide were added. After sealing the kettle, replace the air with nitrogen to ensure that the oxygen content in the kettle is less than 150ppm. Stir to raise the temperature, control the reaction temperature to 125-130°C, the reaction pressure is not higher than 0.04MPa, and add 464g of propylene oxide. Close the propylene oxide feed valve and age for 1.5 hours to obtain the crude product of propylene glycol phenyl ether. Pour the crude product into a 2-liter distillation pot, raise the temperature to 80-85°C for vacuum distillation, and remove excess phenol. Keep the vacuum at 0.1MPa-0.11MPa, and distill for 2.5 hours to obtain a propylene glycol phenyl ether product with a purity of 99.07%.

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Abstract

The invention discloses a method for preparing ethylene glycol phenyl ether, propylene glycol phenyl ether and butylene glycol phenyl ether, comprising the following steps: 1) firstly, adding phenyl into a reaction kettle, introducing inert gas and adding catalyst, then adding ethylene oxide or propylene oxide or butylene oxide, reacting under the conditions that the temperature is at 70-140 DEG C and the pressure is less than 1 MPa, thereby generating the crude product of ethylene glycol phenyl ether or propylene glycol phenyl ether or butylene glycol phenyl ether, wherein the mol ratio of the added phenyl to the added ethylene oxide or propylene oxide or butylene oxide is 1:0.6-1; and 2) reducing pressure and distilling the prepared crude benzene under the conditions that the vacuum degree is not less than 0.07MPa and the temperature is at 80-110 DEG C, thereby obtaining the product of ethylene glycol phenyl ether or propylene glycol phenyl ether or butylene glycol phenyl ether. The product of ethylene glycol phenyl ether or propylene glycol phenyl ether or butylene glycol phenyl ether prepared by the invention has a purity more than 99%, and does not need to be rectified and purified; and the method has the advantages of low equipment investment, convenient maintenance, simple operation control, low comprehensive cost and the like, and has considerable economic benefit.

Description

1. Technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for preparing ethylene, propylene and butanediol phenyl ethers. 2. Background technology [0002] Ethylene glycol phenyl ether, propylene glycol phenyl ether, and butanediol phenyl ether are three important chemical organic solvents, which are widely used in many industries and fields such as coatings, plastics, textiles, printing and dyeing, medicine, and washing. At present, the production techniques for preparing the above three phenyl ethers mainly include kettle-type batch method and tubular continuous method. , Butylene oxide reacts to produce the above three phenyl ethers. Due to the certain toxicity of phenol, in order to make the product after the reaction free of phenol, the molar ratio of the added alkylene oxide to phenol is usually adjusted to be greater than 1, that is, the amount of added alkylene oxide is more than that of phenol...

Claims

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Application Information

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IPC IPC(8): C07C43/205C07C43/23C07C41/03
Inventor 李金彪梁国强徐仕睿包雷
Owner JIAHUA CHEM
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