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A kind of purification method of o-phenylenediethyl ether

A technology of phthalic diethyl ether and purification method, which is applied in ether separation/purification, chemical instruments and methods, ether preparation, etc., can solve problems such as high cost and environmental pollution, and achieve low impurity content, high yield and high purity Effect

Active Publication Date: 2016-08-17
XINYI AGRI CHEM PLANT JIANGSU PROV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the problems of high cost and environmental pollution in the purification of crude phthalic diethyl ether, the present invention provides a method for purifying phthalic diethyl ether using water as a solvent. The method not only saves costs, is environmentally friendly, but also has high purification efficiency. High purity of the purified product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The specific purification steps of the crude product of o-phenylenediethyl ether in the present embodiment are:

[0019] a. Add 2000Kg of water into a 5000L enamel reaction kettle, put 2000Kg of crude phthalic diethyl ether (wet product: content 92%; appearance: khaki, granular) into the reaction kettle under stirring conditions, and heat up to 60°C , after the phthalic diethyl ether is completely melted, add 30% hydrochloric acid dropwise to the reaction kettle under the condition of sufficient stirring, and adjust the pH of the mixed solution to 3.5, and some impurities in the crude product are dissolved in water, forming an aqueous solution layer from bottom to top , non-water-soluble flocculent impurity layer and o-phenylenediyl ether layer;

[0020] b. Pour the mixed solution of phthalic diethyl ether that has adjusted the pH value in step a into the microporous filter through a high-pressure pump, filter out most of the non-water-soluble flocculent impurities in t...

Embodiment 2

[0027] The specific purification steps of the crude product of o-phenylenediethyl ether in the present embodiment are:

[0028] a. Add 3000Kg of water into a 5000L enamel reaction kettle, and put 2000Kg of crude phthalic diethyl ether (wet product: content 90%; appearance: khaki, granular) into the reaction kettle under stirring conditions, and heat up to 60°C , after the phthalic diethyl ether is completely melted, add 30% hydrochloric acid dropwise to the reaction kettle under the condition of sufficient stirring, adjust the pH of the mixed solution to 3.6, and some impurities in the crude product are dissolved in water, forming an aqueous solution layer from bottom to top , non-water-soluble flocculent impurity layer and o-phenylenediyl ether layer;

[0029] b. Pour the mixed solution of phthalic diethyl ether that has adjusted the pH value in step a into the microporous filter through a high-pressure pump, filter out most of the non-water-soluble flocculent impurities in t...

Embodiment 3

[0036] The specific purification steps of the crude product of o-phenylenediethyl ether in the present embodiment are:

[0037] a. Add 3000Kg of water into a 5000L enamel reaction kettle, put 1500Kg of crude phthalic diethyl ether (wet product: content 90%; appearance: khaki, granular) into the reaction kettle under stirring conditions, and heat up to 60°C , after the phthalic diethyl ether is completely melted, add 30% hydrochloric acid dropwise to the reaction kettle under the condition of sufficient stirring, adjust the pH of the mixed solution to 3.8, and some impurities in the crude product are dissolved in water, forming an aqueous solution layer from bottom to top , non-water-soluble flocculent impurity layer and o-phenylenediyl ether layer;

[0038]b. Pour the mixed solution of phthalic diethyl ether that has adjusted the pH value in step a into the microporous filter through a high-pressure pump, filter out most of the non-water-soluble flocculent impurities in the sy...

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PUM

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Abstract

The invention discloses a purification method of o-diethoxybenzene. The purification method comprises the following steps: taking catechol and a sodium hydroxide solution as reactants, chloroethane or bromoethane as an etherifying agent and ethanol as a solvent, and reacting all the materials in a high-pressure kettle to obtain the coarse product o-diethoxybenzene; adding water to the reaction kettle and adding the coarse product o-diethoxybenzene under the condition of stirring, heating until the o-diethoxybenzene is completely molten and then dropwise adding hydrochloric acid to the reaction kettle under the condition of full stirring so that partial impurities in the coarse product can be dissolved into water and a water solution layer, a non-water-soluble flocculent impurity layer and an o-diethoxybenzene layer can be formed from bottom to top; and finally, separating out the o-diethoxybenzene, thereby obtaining the pure product having the purity of greater than or equal to 99% and the moisture content of greater than or equal to 0.5%. According to the purification method of the o-diethoxybenzene, the clean, environment-friendly and cheap water is utilized instead of a traditional organic solvent, and therefore, the cost is saved and the purification method is environment-friendly; besides, the purification method is simple, the yield of the purification process is high, and the purified o-diethoxybenzene is high in purity, low in moisture content and capable of better meeting the export requirements.

Description

technical field [0001] The invention belongs to the technical field of phthalic diethyl ether production, in particular to a method for purifying crude phthalic diethyl ether prepared from catechol and sodium hydroxide solution as reactants. Background technique [0002] O-phenylenediethyl ether, English name: 1,2-Diethoxybenzene, CAS number: 2050-46-6, EINECS number: 218-089-1, is an important drug, spice and fungicide Dimethocarb intermediate. The traditional method of synthesizing o-phenylenediethyl ether is to react catechol and sodium hydroxide solution in an autoclave at 90-120°C as the reactant, ethyl chloride as the etherifying agent, and ethanol as the solvent. . Ethyl bromide is also used as an etherification agent, but ethyl chloride is usually used because ethyl bromide is highly toxic, has strict requirements on the operating environment, and pollutes the environment. [0003] Traditionally, organic solvents such as toluene, dichloroethane, acetone, and chlor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/38C07C41/34C07C43/205
CPCC07C37/66C07C41/16C07C41/34C07C41/38C07C41/44C07C39/08C07C43/205
Inventor 刘宇纪传武高畅行魏星蒋磊周全义蔡小飞
Owner XINYI AGRI CHEM PLANT JIANGSU PROV