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Method for preparing polyformaldehyde dimethyl ether from paraformaldehyde

A technology of polyoxymethylene dimethyl ether and paraformaldehyde, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as difficult separation of catalysts, low conversion rate of raw materials, poor product selectivity, etc. Excellent performance, high conversion rate of raw materials, good yield

Active Publication Date: 2014-03-26
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0007] The technical problem to be solved by the present invention is that there are problems in the synthesis of polyoxymethylene dimethyl ether with methanol, methylal and paraformaldehyde as reaction raw materials in the prior art, such as difficult catalyst separation, low conversion rate of raw materials, and poor product selectivity. A new method for preparing polyoxymethylene dimethyl ether from paraformaldehyde

Method used

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  • Method for preparing polyformaldehyde dimethyl ether from paraformaldehyde

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 2 g of Catalyst H to a 300 ml tank reactor 5 PMo 10 V 2 o 40 / SiO 2 , where the heteropolyacid H 5 PMo 10 V 2 o 40 with oxide support SiO 2 The mass fraction ratio is 20:80, 100 ml of methanol and 100 g of paraformaldehyde were reacted at 130°C and 0.8 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 material methanol and paraformaldehyde, and its composition distribution is shown in Table 1.

[0015]

Embodiment 2

[0017] Add 2 g of Catalyst H to a 300 ml tank reactor 4 PWM 6 o 40 / TiO 2 , where the heteropolyacid H 4 PWM 6 o 40 with oxide support TiO 2 The mass fraction ratio is 20:80, 100 ml of methanol and 100 g of paraformaldehyde were reacted for 4 hours at 130 ° C and 0.6 MPa autogenous pressure, and the samples were extracted and analyzed by gas chromatography after centrifugation. The product contains polyoxymethylene dimethyl ether and unreacted raw material methanol and paraformaldehyde, and its composition distribution is shown in Table 1.

[0018]

Embodiment 3

[0020] Add 2 grams of catalyst PMo in a 300 ml tank reactor 12 / TiO 2 , where the heteropolyacid PMo 12 with oxide support TiO 2 The mass fraction ratio is 70:30, 100 ml of methylal and 100 g of paraformaldehyde are reacted at 130 ° C and 0.6 MPa autogenous pressure for 4 hours, and the samples are 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.

[0021]

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Abstract

The invention relates to a method for preparing polyformaldehyde dimethyl ether from paraformaldehyde, which is mainly used for solving the problems that the conventional method for synthesizing the polyformaldehyde dimethyl ether by taking trioxymethylene as a material is high in cost and not high in catalyst reaction selectivity. In order to solve the problems betters, a following technical scheme is as follows: methanol, methylal and polyformaldehyde are taken as materials in a mass ratio of (0-10):(0-10):1 to contact with a catalyst for reaction to generate polyformaldehyde dimethyl ether CH3O(CH2O)nCH3 under conditions with a reaction temperature of 70 DEG C-200 DEG C and reaction pressure of 0.2 MPa-0.6 MPa, wherein the dosages of the methanol and the methylal cannot be 0 at the same time, and the used catalyst comprises the following components in parts by weight: 30-80 parts of an oxide carrier and 20-70 parts of heteropoly acid. And therefore, the method can be used for industrial production of polyformaldehyde dimethyl ether.

Description

technical field [0001] The invention relates to a method for preparing polyoxymethylene dimethyl ether from paraformaldehyde, in particular to a method for synthesizing polyoxymethylene dimethyl ether with paraformaldehyde as a 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 10-20 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 performan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/30C07C41/56
CPCC07C41/56C07C43/30
Inventor 高晓晨刘志成高焕新杨为民
Owner CHINA PETROLEUM & CHEM CORP
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