Method for synthesizing polyoxymethylene dimethyl ether by methylal and trioxane

A technology of polyoxymethylene dimethyl ether and paraformaldehyde, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of poor selectivity and high content of by-product methylal, and achieve improved distribution, High specific surface area, effect of reducing selectivity

Active Publication Date: 2016-02-10
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is that in the process of synthesizing polyoxymethylene dimethyl ether with methanol and paraformaldehyde as raw materials in the prior art, the by-product methylal content is relatively high and the selectivity is poor, and a new polyoxymethylene dimethyl ether is provided. The synthetic method of formaldehyde dimethyl ether

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 2 g of catalyst SO to a 300 ml tank reactor 4 2- / ZrO 2 / SBA-15 (wherein the solid superacid SO 4 2- / ZrO 2 The mass fraction ratio of molecular sieve carrier SBA-15 is 20:80, SO 4 2- accounted for ZrO 2 The load of the carrier is 1wt.%), 97.2 milliliters of methylal and 100 grams of paraformaldehyde, reacted at 130 ° C and 0.5 MPa autogenous pressure for 4 hours, and the samples were extracted and analyzed by gas chromatography after centrifugation. The product contains polyoxymethylene dimethyl ether and unreacted raw materials methylal and paraformaldehyde, and its composition distribution is shown in Table 1.

Embodiment 2

[0017] 2 g of catalyst Cl was added to a 300 ml tank reactor - / Fe 2 o 3 / MCM-22 (wherein the solid superacid Cl - / Fe 2 o 3 The mass fraction ratio with molecular sieve carrier MCM-22 is 20:80, Cl - accounted for Fe 2 o 3 The load of the carrier is 2wt.%), 120 ml of methylal and 30 g of paraformaldehyde, reacted at 130 ° C and 0.7 MPa autogenous pressure for 4 hours, and the samples were extracted and analyzed by gas chromatography after centrifugation. The product contains polyoxymethylene dimethyl ether and unreacted raw materials methylal and paraformaldehyde, and its composition distribution is shown in Table 1.

Embodiment 3

[0019] Add 0.5 g catalyst SO to a 300 ml tank reactor 4 2- / ZrO 2 / SBA-15 (wherein the solid superacid SO 4 2- / ZrO 2 The mass fraction ratio of molecular sieve carrier SBA-15 is 40:60, SO 4 2- accounted for ZrO 2 The load of the carrier is 1wt.%), 120 ml of methylal and 30 g of paraformaldehyde, and react for 4 hours at 130 °C with nitrogen flushing to a pressure of 4 MPa. The sample is extracted and analyzed by gas chromatography after centrifugation. The product contains polyoxymethylene dimethyl ether and unreacted raw materials methylal and paraformaldehyde, and its composition distribution is shown in Table 1.

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Abstract

The present invention relates to a polyformaldehyde dimethyl ether synthesis method, wherein problems of more by-product methylal generation and poor product selectivity during a polyformaldehyde dimethyl ether synthesis process adopting methanol and trioxymethylene as raw materials in the prior art are mainly solved with the present invention. The technical scheme comprises that methylal and trioxymethylene are adopted as raw materials, and the raw materials and a solid super acid catalyst are subjected to a contact reaction at a reaction temperature of 70-200 DEG C under a reaction pressure of 0.5-6 MPa to produce the polyformaldehyde dimethyl ether (CH3O(CH2O)nCH3), wherein the amount of the catalyst is 0.1-5.0% of the weight of the raw materials, and the catalyst comprises, by weight, a) 30-80 parts of a molecular sieve carrier, and b) 20-70 parts of a solid super acid. With the technical scheme, the problems in the prior art are well solved, and the method can be used for industrial production of polyformaldehyde dimethyl ether.

Description

technical field [0001] The invention relates to a method for synthesizing polyoxymethylene dimethyl ether. Background technique [0002] In recent years, with the deepening influence of the industrial revolution, 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 10-20 years, my country's oil supply rate will only be ~50%. Therefore, 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 increased significantly. Polyoxymethylene dimethyl ether, or Polyoxymeth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/30C07C41/56
Inventor 高晓晨刘志成许云风高焕新杨为民
Owner CHINA PETROLEUM & CHEM CORP
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