Preparation method of polyoxymethylene dimethyl ether

A technology of polyoxymethylene dimethyl ether and paraformaldehyde, which is applied in the preparation of organic compounds, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problems of low product selectivity and achieve good yield and good technical effect. Effect

Active Publication Date: 2019-04-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is that there is a problem of low product selectivity of n=2-10 in the process of synthesizing polyoxymethylene dimethyl ether with methanol, methylal and paraformaldehyde as reaction raw materials in the prior art, and a new method is provided The preparation method of polyoxymethylene dimethyl ether

Method used

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  • Preparation method of polyoxymethylene dimethyl ether

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1. Preparation of catalyst

[0039] Sodium sulfonate type polystyrene cation exchange resin 7320 is washed with deionized water until clear water flows out, then soaked four times with 4w% hydrochloric acid, each use is equivalent to 10 times the dry weight of sodium sulfonate type polystyrene cation exchange resin 7320 4w% hydrochloric acid, soaked for 4 hours each time, then washed with deionized water until the eluate was free of chloride ions, and dried at 60°C to obtain a sulfonic acid polystyrene cation exchange resin with a total exchange capacity of 4.10 mmol / g. Get the Ga(OH) that is equivalent to the sulfonic acid type polystyrene cation-exchange resin of 98 grams of dry base resin and 300ml containing Ga is 2 grams 3 Mix the aqueous suspensions, add 1 drop of glacial acetic acid, mix, let stand at room temperature for 24 hours, and dry to constant weight in a vacuum oven to prepare a catalyst with a Ga content of 2w%.

[0040] 2. Synthesis of polyoxymethyle...

Embodiment 2

[0043] 1. Preparation of catalyst

[0044]Sodium sulfonate type polystyrene cation exchange resin 7320 is washed with deionized water until clear water flows out, then soaked four times with 4w% hydrochloric acid, each use is equivalent to 10 times the dry weight of sodium sulfonate type polystyrene cation exchange resin 7320 4w% hydrochloric acid, soaked for 4 hours each time, then washed with deionized water until the eluate was free of chloride ions, and dried at 60°C to obtain a sulfonic acid polystyrene cation exchange resin with a total exchange capacity of 4.10 mmol / g. Get the sulfonic acid type polystyrene cation exchange resin equivalent to 98 grams of dry base resin, under nitrogen protection, be 2 grams of Ra(OH) with 300ml containing Ra 2 Mix the aqueous suspensions, add 1 drop of glacial acetic acid, mix, let stand at room temperature for 24 hours, and dry to constant weight in a vacuum oven to prepare a catalyst with an Ra content of 2w%.

[0045] 2. Synthesis ...

Embodiment 3

[0048] 1. Preparation of catalyst

[0049] Sodium sulfonate type polystyrene cation exchange resin 7320 is washed with deionized water until clear water flows out, then soaked four times with 4w% hydrochloric acid, each use is equivalent to 10 times the dry weight of sodium sulfonate type polystyrene cation exchange resin 7320 4w% hydrochloric acid, soaked for 4 hours each time, then washed with deionized water until the eluate was free of chloride ions, and dried at 60°C to obtain a sulfonic acid polystyrene cation exchange resin with a total exchange capacity of 4.10 mmol / g. Get the sulfonic acid type polystyrene cation exchange resin equivalent to 98 grams of dry base resin, under nitrogen protection, be 2 grams of Be(OH) with 300ml containing Be 2 Mix the aqueous suspensions, add 1 drop of glacial acetic acid, mix, let stand at room temperature for 24 hours, and dry to constant weight in a vacuum oven to prepare a catalyst with a Be content of 2w%.

[0050] 2. Synthesis ...

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Abstract

The invention relates to a preparation method of polyoxymethylene dimethyl ether and mainly solves problems of low catalyst activity and low selectivity in the process of synthesizing polyoxymethylenedimethyl ether by using methanol, methylal and paraformaldehyde as reaction materials in the prior art. The preparation method of polyoxymethylene dimethyl ether comprises the following step: raw materials including methanol, methylal and paraformaldehyde is contacted with a catalyst to react so as to generate polyoxymethylene dimethyl ether, wherein the mass ratio of methanol to methylal to paraformaldehyde is (0-10): (0-10):1; use amount of methanol and use amount of methylal cannot be 0 at the same time; the catalyst is metal ion-modified cation exchange resin; and the modified metal is IIA metal. The method in the technical scheme can be used in the industrial production of polyoxymethylene dimethyl ether.

Description

technical field [0001] The invention relates to a preparation method of polyoxymethylene dimethyl ether. Background technique [0002] In recent years, with the deepening influence of the industrial revolution and my country's unique resource pattern of "more coal, less oil, and gas", my country's oil resources have become increasingly tense, and the pressure on oil supply has increased unprecedentedly. It is estimated that in the next 10 to 20 years, my country's oil supply rate will only be ~50%. How to use our country's rich coal resources to solve our country's energy crisis has become an urgent problem for scientific researchers. Therefore, the development of new oil substitutes from coal-based methanol has attracted increasing attention. [0003] DME was first proposed as a diesel additive. However, due to its poor cold start performance, high vapor pressure at room temperature, and easy air resistance, the cost of DME as an alternative fuel for vehicles has increase...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/56C07C43/30B01J31/10B01J37/02
CPCC07C41/56B01J31/10B01J37/0201C07C43/30
Inventor 高晓晨石竹柏诗哲
Owner CHINA PETROLEUM & CHEM CORP
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