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Process for continuously producing polyoxymethylenedimethyl ethers at low temperature

A technology of polyoxymethylene dimethyl ether and paraformaldehyde, applied in the preparation of organic compounds, membranes, physical/chemical process catalysts, etc., to reduce costs and energy consumption, high product selectivity, and achieve long-term continuous operation Effect

Active Publication Date: 2019-08-23
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the invention is: in order to solve the technical problem of continuous production polyoxymethylene dimethyl ether, the present invention provides a kind of technique of low temperature continuous production polyoxymethylene dimethyl ether

Method used

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  • Process for continuously producing polyoxymethylenedimethyl ethers at low temperature
  • Process for continuously producing polyoxymethylenedimethyl ethers at low temperature
  • Process for continuously producing polyoxymethylenedimethyl ethers at low temperature

Examples

Experimental program
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Effect test

Embodiment 1

[0040] 20 g of MCM-22 molecular sieve catalysts with a high silicon-aluminum ratio are loaded into a reactor 10 with an effective volume of 500 ml. will preheat to 40 oC methylal is injected into the first batching tank 3 (or the second batching tank 16) that has been equipped with paraformaldehyde, and mixed evenly, wherein the molar ratio of methylal:paraformaldehyde is 2:1. The mixed raw materials are continuously injected into the reactor 10 by the second feeding pump 14, and the stirring is maintained continuously, so that the catalyst and the reaction raw materials are uniformly mixed and reacted. During the reaction, the reactor temperature was controlled to be 40° C., the flow rate of the second feed pump 14 was 5 mL / min, the timing switching time of the four-way flow path valve 7 was 6 hours, and the opening pressure of the reaction back pressure valve 8 was 0.5 MPa. The opening pressure of material back pressure valve 15 is 1.3MPa. The initial pressure of the gas f...

Embodiment 2

[0044] 20 g of ZSM-5 molecular sieve catalysts with a low silicon-aluminum ratio are loaded into a reactor 10 with an effective volume of 500 ml. Inject the methylal preheated to 35°C into the first batching tank 3 (or the second batching tank 16) filled with paraformaldehyde, and mix well, wherein the molar ratio of methylal:paraformaldehyde is 6:1. The mixed raw materials are continuously injected into the reactor 10 by the second feeding pump 14, and the stirring is maintained continuously, so that the catalyst and the reaction raw materials are uniformly mixed and reacted. During the reaction, the reactor temperature was controlled to be 60° C., the flow rate of the second feed pump 14 was 10 mL / min, the timing switching time of the four-way flow path valve 7 was 6 hours, and the opening pressure of the reaction back pressure valve 8 was 0.6 MPa. The opening pressure of material back pressure valve 15 is 1.5MPa. The initial pressure of the gas flow control meter 13 is 5 s...

Embodiment 3

[0048] 20 g of Hβ molecular sieve catalysts were loaded into a reactor 10 with an effective volume of 500 ml. Inject the methylal preheated to 32°C into the first batching tank 3 (or the second batching tank 16) filled with paraformaldehyde, and mix well, wherein the molar ratio of methylal:paraformaldehyde is 10:1. The mixed raw materials are continuously injected into the reactor 10 by the second feeding pump 14, and the stirring is maintained continuously, so that the catalyst and the reaction raw materials are uniformly mixed and reacted. During the reaction, the reactor temperature was controlled to be 69° C., the flow rate of the second feed pump 14 was 10 mL / min, the timing switching time of the four-way flow path valve 7 was 6 hours, and the opening pressure of the reaction back pressure valve 8 was 0.6 MPa. The opening pressure of material back pressure valve 15 is 1.5MPa. The initial pressure of the gas flow control meter 13 is 5 sccm, and then adjusted according to...

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Abstract

The invention relates to a process for continuously producing polyoxymethylenedimethyl ethers (DMMn) at a low temperature, belongs to the technical field of preparation processes of the polyoxymethylenedimethyl ethers, and solves the technical problem of continuously producing the polyoxymethylenedimethyl ethers. The process provided by the invention uses a membrane separation element for precisely controlling film pores to realize direct separation of a material from a catalyst in a tank and effectively reduce permeability resistance of separation membrane tubes; the process uses a time-sharing back flowing manner to clean and inhibit adhesion of the catalyst on the separation membrane tubes to ensure continuous operation of the reaction process; and the process can realize long-term continuous operation under the condition that the catalyst satisfies good mechanical strength, and fully exerts the advantages of long service life cycle of the molecular sieve catalyst, the process is simple, has mild conditions and high product selectivity, greatly reduces costs and energy consumption of the industrial process of DMMn synthesis, and has broad industrial application prospects.

Description

technical field [0001] The invention belongs to the technical field of polyoxymethylene dimethyl ether preparation technology, and specifically relates to a process for continuously producing polyoxymethylene dimethyl ether at low temperature. Background technique [0002] Polyoxymethylene dimethyl ether (CH 3 -O-(CH 2 -O) n -CH 3 , n > 1, referred to as DMM n ) is a new type of polyether methanol derivative, in which DMM 2-8 Due to its high oxygen content and cetane number, as a diesel additive, it can significantly improve the combustion conditions in diesel engines and effectively reduce CO, NO x and emission of particulate pollutants. DMM 2-8 Can be made of methanol or methylal (DMM) with formaldehyde (FA), paraformaldehyde (TOM) or paraformaldehyde (PF n ) etc. are synthesized by polymerization reaction. Therefore, efficient preparation of DMM from methanol and its derivatives 2-8 It has important research value and wide application prospect in alleviating...

Claims

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Application Information

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IPC IPC(8): C07C41/56C07C41/58C07C43/30
CPCC07C41/56C07C41/58C07C43/30B01D67/0072B01D69/04B01J4/008B01J19/0066B01J19/18B01J29/40B01J29/7007B01J29/7038B01J2219/00033B01J2219/00051B01J2219/00761C07C43/303
Inventor 王国富郭佳琪樊卫斌王建国董梅王鹏飞岑友良肖亚宁王东飞孙守靖王伟林张俊才张敏李运宏
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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