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A kind of method for preparing dicapped glycol ether

A technology of glycol ether and ethylene glycol monoether, which is applied in the field of preparation of double-terminated glycol ether, can solve the problems of difficult regeneration of resin catalysts, low catalyst yield, selectivity and service life, etc., and achieves selectivity The effect of lifting, long catalyst one-way life, and large investment scale

Inactive Publication Date: 2018-05-18
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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  • A kind of method for preparing dicapped glycol ether
  • A kind of method for preparing dicapped glycol ether
  • A kind of method for preparing dicapped glycol ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] 2.0Kg of hydrogen-type MCM-22 molecular sieve catalyst with a silicon-aluminum ratio (Si:Al)=45:1 was extruded with alumina as a binder. ℃ for 5 hours to obtain a rod-shaped catalyst with a diameter of 3 mm, a length of 3 mm, and a mass content of alumina of 20%. Get 1.0Kg of this catalyst and put it into a stainless steel reaction tube with an internal diameter of 32mm, activate it with nitrogen at normal pressure and 550°C for 4 hours, then drop it to the reaction temperature (abbreviated as T)=50°C, the molar ratio of the fresh raw materials introduced for CH 3 OCH 3 :CH 3 OCH 2 CH 2 OH=1:1, reaction pressure (abbreviated as P)=0.1MPa, mass space velocity of ethylene glycol monoether in fresh raw materials (abbreviated as WHSV)=0.01h -1 , without carrier gas, after the reaction is stable, the product is analyzed by gas chromatography, and the conversion rate of ethylene glycol monoether and the single-pass selectivity of the product are calculated. Then the mon...

Embodiment 2

[0067] Raw material and mol ratio among the embodiment 1 are changed into

[0068] CH 3 CH 2 OCH 3 CH 2 :CH 3 CH 2 OCH 2 CH 2 OH=1:1, the rest of the experimental steps are consistent with Example 1. The reaction conditions and results are shown in Table 1.

Embodiment 3

[0070] The catalyzer among the embodiment 1 is changed into hydrogen type ferrierite molecular sieve, Si:Al=15:1, T=300 ℃, P=15MPa, the mol ratio of feeding raw material is

[0071] CH 3 OCH 3 :CH 3 OCH 2 CH 2 OH=100:1, WHSV=15h -1 , the carrier gas is nitrogen, the carrier gas nitrogen volume space velocity (abbreviated as GHSV) = 10000h -1 , the rest of the experimental steps are consistent with Example 1. The reaction conditions and results are shown in Table 1.

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Abstract

The present application discloses a method for preparing double-capped glycol ethers, comprising steps: a) raw materials containing ethylene glycol monoethers and monohydric alcohol ethers, at a reaction temperature of 50-300°C and a reaction pressure of 0.1-15Mpa , The mass space velocity of ethylene glycol monoether is 0.01~15.0h-1, and the molar ratio of monohydric alcohol ether and ethylene glycol monoether is under the condition of monohydric alcohol ether: ethylene glycol monoether=1~100:1, Lead into the reactor to contact and react with the acidic molecular sieve catalyst, and the product is separated to obtain the double-capped glycol ether product, unreacted glycol monoether and monohydric alcohol ether, by-product components, and the remaining components; b) Unreacted ethylene glycol monoethers and monohydric alcohol ethers and by-product components in step a) are returned to the reactor. The method has the advantages of long single-pass life of the catalyst, high yield and selectivity of target products, low energy consumption for product separation, high economic value of by-products, large or small production scales, and flexible application.

Description

technical field [0001] The application belongs to the field of chemistry and chemical engineering, in particular, it relates to a method for preparing double-capped 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, and good coking resistance. Good, low 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 (Willia...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/11C07C41/09
Inventor 倪友明朱文良刘红超刘勇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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