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Preparation method for 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 life, difficult regeneration of resin catalyst, etc. The effect of raw material utilization rate, selectivity improvement, and low economic value

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 for double-terminated glycol ether
  • Preparation method for double-terminated glycol ether
  • Preparation method for double-terminated glycol ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] 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 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 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 monohyd...

Embodiment 2

[0069] Raw material and mol ratio among the embodiment 1 are changed into

[0070] CH 3 CH 2 OH: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

[0072] 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 ratio 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, 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 invention discloses a preparation method for double-terminated glycol ether. The preparation method comprises the following steps: a) introducing raw materials containing glycol monoether and monohydric ether alcohol into a reactor for contact and reaction with an acidic molecular sieve catalyst under the conditions that reaction temperature is 50 to 300 DEG C, reaction pressure is 0.1 to 15 MPa, the mass space velocity of the glycol monoether in the raw materials is 0.01 to 15.0 / h, and a mol ratio of monohydric ether alcohol to glycol monoether in the raw materials is 1-100: 1, and separating obtained products so as to obtain a double-terminated glycol ether product, unreacted glycol monoether and monohydric ether alcohol, by-product components and other components; and b) returning the unreacted glycol monoether and monohydric ether alcohol and the by-product components obtained in the step a) to the reactor. The preparation method has the advantages that the catalyst has long single-pass life; the target product, i.e., double-terminated glycol ether has high yield and selectivity; energy consumption in separation of the products is low; by-products have high economic value; production scale can be large or small; and application of the method is flexible.

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 Applications(China)
IPC IPC(8): C07C43/11C07C41/09
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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