Method for preparing polymethoxy dimethyl ether by virtue of slurry bed in combination with fixed bed

A technology for the joint preparation of polyoxymethylene dimethyl ether, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of low content of effective products, achieve the goal of reducing production cost and improving utilization rate Effect

Active Publication Date: 2014-10-29
DONGFANG HONGSHENG NEW ENERGY APPL TECH RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the method for synthesizing polyoxymethylene dimethyl ether in the prior art is limited by the influence of material reaction balance, resulting in the problem that the content of effective products is low, thereby providing a method that can effectively increase the yield Method for preparing polyoxymethylene dimethyl ether by using slurry bed and fixed bed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] This embodiment provides a method for jointly preparing polyoxymethylene dimethyl ether in a slurry bed and a fixed bed, which includes the following steps:

[0022] (1) Add methanol and paraformaldehyde with a molar ratio of 1:1 to the reaction kettle of the slurry bed reactor, and add ZSM-5 molecular sieve as a catalyst, and the ZSM-5 catalyst accounts for 2.5% of the total mass of the reaction materials. wt%; Replace the air in the reactor with nitrogen, continue to fill in nitrogen until the pressure in the reactor reaches 1.0Mpa, control the reaction temperature at 160°C to react for 5 hours, and reach equilibrium; detect the polymethoxyl in each degree of polymerization in the equilibrium product The content of dimethyl ether, the results are shown in Table 1;

[0023] (2) The equilibrium material product obtained in step (1) is transferred to a fixed-bed reactor filled with Hβ catalyst, and the controlled reaction temperature is 90°C, the pressure is 2.0Mpa, and ...

Embodiment 2

[0025] This embodiment provides a method for jointly preparing polyoxymethylene dimethyl ether in a slurry bed and a fixed bed, which includes the following steps:

[0026] (1) In the reactor of the slurry bed reactor, add methanol and low polymerization degree paraformaldehyde in a molar ratio of 1.5:1, and add a strongly acidic styrene-based cation exchange resin as a catalyst, and the strongly acidic styrene-based The cation exchange resin catalyst accounts for 2.5wt% of the total mass of the reaction material; replace the air in the reactor with nitrogen, continue to charge nitrogen until the pressure in the reactor reaches 1.5Mpa, control the reaction temperature at 150°C for 6 hours, and reach equilibrium; The content of each degree of polymerization polyoxymethylene dimethyl ether in the equilibrium product, the results are shown in Table 1;

[0027] (2) The equilibrium material product system obtained in step (1) is transferred to a fixed bed reactor filled with a soli...

Embodiment 3

[0029] This embodiment provides a method for jointly preparing polyoxymethylene dimethyl ether in a slurry bed and a fixed bed, which includes the following steps:

[0030] (1) in the reaction still of slurry bed reactor, adding mol ratio is methyl alcohol and paraformaldehyde of 2:1, and adds Hβ catalyzer, and Hβ catalyzer accounts for 3wt% of reaction mass; Air, continue to fill in nitrogen until the pressure in the reactor reaches 1.0Mpa, control the reaction temperature to 130°C and react for 7h to reach equilibrium; detect the content of polyoxymethylene dimethyl ether with each degree of polymerization in the equilibrium product, and the results are shown in Table 1 ;

[0031] (2) The equilibrium material product system obtained in step (1) is transferred to a fixed-bed reactor filled with a strongly acidic styrene-based cation exchange resin catalyst, and the controlled reaction temperature is 140°C, the pressure is 0.8Mpa, and the volume space velocity for 2h -1 Unde...

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Abstract

The invention provides a method for preparing polymethoxy dimethyl ether by virtue of a slurry bed in combination with a fixed bed. According to the method, conventional methanol and / or methyl acetal, formaldehyde and / or trioxymethylene in the prior art are taken as synthetic raw materials, by the steps of firstly reacting reaction raw materials in the slurry bed to balance and then moving the obtained product to the fixed-bed reactor and reacting, the original balance of the balanced material system obtained by reacting in the slurry reactor is broken in the fixed bed, and the reaction is further carried out towards the direction capable of forming polymethoxy dimethyl ether so that the distribution of effective polymethoxy dimethyl ether with a low degree of polymerization in a product system containing polymethoxy dimethyl ether is preferable, the content of DMM2-8 component reaches 60%, the utilization rate of raw materials is effectively improved and the production cost is decreased.

Description

technical field [0001] The invention belongs to the technical field of energy and chemical engineering, and in particular relates to a method for jointly preparing polyoxymethylene dimethyl ether by using a slurry bed and a fixed bed. Background technique [0002] The contradiction between the supply and demand of diesel oil in my country has always been very sharp. First, the supply quantity cannot meet the rapid and continuous growth of my country's market demand; second, the quality of diesel oil is poor, and its cetane number (ie CN value) is usually difficult to reach the national standard value of 45 requirements. Diesel engine exhaust in addition to CO, CO 2 and NO x In addition, it also contains a large amount of unburned HC compounds and particulate matter PM and other harmful substances, which is one of the main sources of PM2.5 pollution in urban air. In June 2012, the International Cancer Research Center (IARC) under the World Health Organization (WHO) announce...

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 商红岩洪正鹏薛真真左飞崔春涛
Owner DONGFANG HONGSHENG NEW ENERGY APPL TECH RES INST
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