Ethylene glycol diarylether preparation method

A technology of ethylene glycol diaryl ether and polyethylene glycol, applied in ether preparation, organic chemistry and other directions, can solve problems such as difficult control, complicated operation, influence reaction, etc. simple effect

Inactive Publication Date: 2004-11-10
SHANXI UNIV +1
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  • Application Information

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Problems solved by technology

In this method, the ratio of phenol to dichloroethane is basically 2 to 1. However, the author adopts the operation of gradually adding alkali to gradually increase the concentration of alkali in the system. However, due to the lower concentration of phenolic oxygen anions in the system, the progress of the reaction is partially affected, so the yield is little changed (72.8%), and the concentration of alkali in the system needs to be carefully controlled for a long time , the operation is complex and difficult to control

Method used

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Examples

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example 11

[0026] Example 1.1,2-bis(3-methylphenoxy)ethane

[0027] Add 108 g (1 mole) of m-cresol into a 1000 ml four-neck flask, stir, add 50% potassium hydroxide solution (56 g potassium hydroxide+56 ml water), heat up to 80° C. for half an hour. Add 99 (1 mole) gram dichloroethane and 10 gram PEG1000, reflux 7 hours (76-83 ℃), then add 50% potassium hydroxide solution (56 gram potassium hydroxide+56 milliliter water), then in 87- Stir at 93°C for 13 hours. Raise the temperature and concentrate, so that the temperature gradually reaches 120° C. in about 3 hours, and keep the temperature at 118-120° C. for one hour. Add 350ml of water, stir vigorously at about 100°C for 10 minutes, let stand to separate layers, and discard the water layer. Add 270ml of isopropanol to the oil layer, heat up and return to distillation to dissolve the solid, gradually lower the temperature to 60°C within two hours, keep it at this temperature for one hour, then slowly cool down to 5°C, and keep at this ...

example 21

[0028] Example 2.1,2-bis(3-methylphenoxy)ethane

[0029] The consumption of ethylene dichloride is 49.5 grams (0.5 mol), and other materials consumption and operating process are with example 1. 68 grams of the product were obtained, the yield was 56%, and the purity was greater than 99%.

example 31

[0030] Example 3.1,2-bis(3-methylphenoxy)ethane

[0031] Do not use PEG1000, other material consumption and operation process are the same as example 1. 75 grams of the product were obtained, the yield was 62%, and the purity was greater than 99%.

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Abstract

The invention discloses an easy-to-operate, high yield preparation process for ethylene glycol di-aromatic ether suitable for industrialized production which comprises the steps of, charging substituted phenol and queous alkali into reactor for stirring reaction, filling excess dichloroethane and phase transition catalyst, carrying out inverse flow reaction at 70-100 deg. C, the reacting time being 15-35 hours, concentrating water at 95-130 deg. C, thus completing the reaction, watering so as to dissolve inorganic salt completely, abandoning the water layer, recrystallizing the residue.

Description

1. Technical field [0001] The invention relates to a preparation method of organic ether compounds, in particular to a preparation method of ethylene glycol diaryl ether. 2. Background technology [0002] Ethylene glycol diaryl ether can be used as a sensitizer for thermal recording materials, a raw material for synthetic polymer materials and various flame retardants, and has a large demand in the international market. Ethylene glycol diaryl ether structural formula (I) is as follows, wherein R 1 -R 5 It may be hydrogen, alkyl, alkoxy, halogen, etc. [0003] [0004] The synthesis of this type of compound generally adopts the theoretical process described by reaction formula (II), which is generally considered to be a nucleophilic substitution reaction between phenolic oxyanion and dichloroethane. Due to the weak ability of the chlorine atom as a leaving group, and the side reactions (III) such as elimination and hydroxyl substitution of dichloroethane under alkaline ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/01C07C43/235
Inventor 郭炜李歆王长生夏炽中王金平杨斌
Owner SHANXI UNIV
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