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Preparation method of double terminated glycol ether

A technology of glycol ether and ethylene glycol monoether, applied in the field of preparation of double-terminated glycol ether, can solve the problems of low catalyst yield, selectivity and service life, difficult regeneration of resin catalyst, etc. Large and small scale, selective improvement, high economical effect

Inactive Publication Date: 2016-07-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield, selectivity and life-span of the catalyzer that these methods adopt are all not high, and resin catalyst is difficult to regenerate, also easily forms a large amount of 1,4-dioxane and high-boiling polyethylene glycol double-capped ether etc. simultaneously by-product

Method used

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  • Preparation method of double terminated glycol ether
  • Preparation method of double terminated glycol ether
  • Preparation method of double terminated glycol ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 50g of hydrogen-type MCM-22 molecular sieve catalyst with a silicon-aluminum ratio (Si:Al)=45:1 was calcined at 550°C for 5 hours in the air atmosphere of a muffle furnace, and a part of the powder sample was taken, pressed into tablets, and crushed into 20-40 mesh , for activity testing. Weigh 10 g of the hydrogen-type MCM-22 molecular sieve catalyst sample, put it into a stainless steel reaction tube with an inner diameter of 8.5 mm, activate it with nitrogen at normal pressure and 550 ° C for 4 hours, and then drop it to the reaction temperature (abbreviated as T) = 50 ° C , the molar composition of the feed material is CH 3 OH:CH 3 OCH 2 CH 2 OH=1:1, reaction pressure (abbreviated as P)=0.1MPa, mass space velocity of ethylene glycol monoether in the raw material (abbreviated as WHSV)=0.01h -1 , without carrier gas, the product was analyzed by gas chromatography. After the reaction was stable, the conversion rate of ethylene glycol monoether and the selectivity o...

Embodiment 2

[0051] The reaction conditions in Example 1 are changed to T=90°C, P=0.9MPa, and the molar composition of the feed material is CH 3 CH 2 OH:CH 3 CH 2 OCH 2 CH 2 OH=2:1, WHSV=0.5h -1 , Carrier gas nitrogen volume space velocity (abbreviated as GHSV) = 100h -1 , all the other experimental procedures are consistent with Example 1, and the reaction conditions and results are shown in Table 1.

Embodiment 3

[0053] The catalyst in Example 1 is replaced by a hydrogen-type ferrierite molecular sieve, Si:Al=15:1, T=300°C, P=15MPa, and the molar composition of the feed material is CH 3 OH:CH 3 OCH 2 CH 2 OH=100:1, WHSV=15h -1 , the carrier gas is nitrogen, GHSV=10000h -1 , all the other experimental procedures are consistent with Example 1, and the reaction conditions and results are shown in Table 1.

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Abstract

The invention relates to a preparation method of double terminated glycol ether. According to the preparation method, raw materials, which contain glycol mono-ether and monohydric alcohol, are introduced into a reactor and then contacted with an acidic molecular sieve catalyst to carry out reactions so as to produce double terminated glycol ether; the reaction temperature is 50 to 300 DEG C, the reaction pressure is 0.1 to 15 MPa; the mass space velocity of glycol mono-ether is 0.01 to 15.0 h<1>; and the mole ratio of monohydric alcohol to glycol mono-ether is 1-100:1. The provided method has the advantages that the single pass service life of catalyst is long, the catalyst can be repeatedly regenerated, the yield and selectivity of target product are high, the energy consumption for separating products is low, the economic value of byproducts is high, the production scale can be large or small, and the application is flexible.

Description

technical field [0001] The application belongs to the field of chemistry and chemical engineering, and in particular relates to a preparation method of double-blocked glycol ethers. Background technique [0002] Double-capped glycol ether refers to the glycol ether obtained by replacing the hydrogen on the two terminal hydroxyl groups of ethylene glycol with hydrocarbon groups. Double-capped glycol ether has no active hydrogen, strong chemical stability, low pour point, small viscosity-temperature change, good heat resistance, enhanced acid-base stability, good emulsifying ability, low foam, strong lipophilicity, anti-coking Better, lower viscosity and density, etc. Therefore, double-capped polyethylene glycol ethers are widely used in the fields of high-speed spinning oils, low-foaming detergents, food processing, and biological fermentation. [0003] The preparation of double-capped glycol ether mainly contains halogenated hydrocarbon and sodium alkoxide (Williamson synt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/10C07C41/09
CPCY02P20/584
Inventor 倪友明朱文良刘勇刘红超刘中民李利娜刘世平周慧
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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