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The preparation method of polyoxymethylene dimethyl ether

A technology of dimethyl ether and polyoxymethylene, which is used in the preparation of organic compounds, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of low catalyst reaction efficiency and high cost of trioxymethylene problem, to achieve the effect of low production cost, high product yield and high reaction conversion rate

Active Publication Date: 2017-12-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] One of the technical problems to be solved by the present invention is that in the prior art, methanol, methylal and paraformaldehyde are used as reaction raw materials to synthesize polyoxymethylene dimethyl ether, which has the problems of low catalyst reaction efficiency and high cost of paraformaldehyde as raw materials , providing a new method for synthesizing polyoxymethylene dimethyl ether with paraformaldehyde

Method used

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  • The preparation method of polyoxymethylene dimethyl ether
  • The preparation method of polyoxymethylene dimethyl ether
  • The preparation method of polyoxymethylene dimethyl ether

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 1. Preparation of catalyst

[0028] (1) Polymerization and hybridization: at room temperature, add 144 grams of styrene, 16 grams of divinylbenzene, 1 gram of BPO and 40 grams of toluene to a 1000 ml three-necked flask and stir evenly, then add 40 grams of 500-mesh copper oxide, and stir Evenly, add 300 grams of 1.0w% PVA aqueous solution, then react at 70°C for 3 hours, 80°C for 1 hour, and 95°C for 45 minutes under stirring to obtain a pellet-shaped product. Stop stirring and keep boiling the pellets at 95°C for 30 minutes. All the products in the three-necked flask were poured into water for cleaning. The product was washed with ethanol and then washed with H 2 O was washed, placed in an oven and dried at 80° C. for 4 h to obtain 200 g of catalyst precursor I.

[0029] (2) Sulfonation: Add 200 grams of catalyst precursor I to 400 grams of 1,2-dichloroethane to swell at room temperature for 4 hours, then add 100 grams of H with a purity of 98w%. 2 SO 4 , stirring ...

Embodiment 2

[0036] 1. Preparation of catalyst

[0037] (1) Polymerization and hybridization: at room temperature, add 144 grams of styrene, 16 grams of divinylbenzene, 1 gram of BPO and 40 grams of toluene to a 1000 ml three-necked flask and stir evenly, then add 40 grams of 500-mesh silicon oxide, and stir Evenly, add 300 grams of 1.0w% PVA aqueous solution, then react at 70°C for 3 hours, 80°C for 1 hour, and 95°C for 45 minutes under stirring to obtain a pellet-shaped product. Stop stirring and keep boiling the pellets at 95°C for 30 minutes. All the products in the three-necked flask were poured into water for cleaning. The product was washed with ethanol and then washed with H 2 O was washed, placed in an oven and dried at 80° C. for 4 h to obtain 200 g of catalyst precursor I.

[0038] (2) Sulfonation: Add 200 grams of catalyst precursor I to 400 grams of 1,2-dichloroethane to swell at room temperature for 4 hours, then add 100 grams of H with a purity of 98w%. 2 SO 4 , stirring...

Embodiment 3

[0042] 1. Preparation of catalyst

[0043] (1) Polymerization and hybridization: at room temperature, add 144 grams of styrene, 16 grams of divinylbenzene, 1 gram of BPO and 40 grams of toluene to a 1000 ml three-necked flask and stir evenly, then add 40 grams of 500-mesh phosphorus oxide, and stir Evenly, add 300 grams of 1.0w% PVA aqueous solution, then react at 70°C for 3 hours, 80°C for 1 hour, and 95°C for 45 minutes under stirring to obtain a pellet-shaped product. Stop stirring and keep boiling the pellets at 95°C for 30 minutes. All the products in the three-necked flask were poured into water for cleaning. The product was washed with ethanol and then washed with H 2 O was washed, placed in an oven and dried at 80° C. for 4 h to obtain 200 g of catalyst precursor I.

[0044] (2) Sulfonation: Add 200 grams of catalyst precursor I to 400 grams of 1,2-dichloroethane to swell at room temperature for 4 hours, then add 100 grams of H with a purity of 98w%. 2 SO 4 , stirr...

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Abstract

The invention relates to a preparation method of polyoxymethylene dimethyl ether, and mainly solves the problems of low catalyst activity and low selectivity in a process of synthesizing polyoxymethylene dimethyl ether by taking methanol, methylal and paraformaldehyde as reaction raw materials in the prior art. With the adoption of the preparation method of polyoxymethylene dimethyl ether, methanol, methylal and paraformaldehyde are taken as the raw materials, wherein the mass ratio of methanol to methylal to paraformaldehyde is (0 to 10): (0 to 10): 1, the use amounts of methanol and methylal cannot be 0 simultaneously, the raw materials are in contact with a catalyst for reaction to generate polyoxymethylene dimethyl ether, the catalyst is oxide modified sulfonic acid type polystyrene cation exchange resin, and oxide is selected from at least one of copper oxide, silicon oxide and phosphorus oxide. The preparation method disclosed by the invention better solves the problems, and can be used in the industrial production of polyoxymethylene dimethyl ether.

Description

technical field [0001] The invention relates to a method for synthesizing polyoxymethylene dimethyl ether with paraformaldehyde as raw material. 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 al...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/30C07C41/56B01J31/28B01J31/10B01J35/10
Inventor 杨为民高晓晨高焕新
Owner CHINA PETROLEUM & CHEM CORP
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