Refining process of polyoxymethylene dimethyl ether condensation product

A technology of polyoxymethylene dimethyl ether and condensation products, which is applied in the preparation of hydroxyl compounds, organic compounds, metal/metal oxide/metal hydroxide catalysts, etc., and can solve unsolved separation problems and difficulties in hydrogen recovery Large scale, high refining costs, etc., to achieve the effect of facilitating large-scale continuous production, reducing decomposition problems, and high activity

Active Publication Date: 2020-09-22
DONGFANG HONGSHENG NEW ENERGY APPL TECH RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this refining method only changes formaldehyde into methanol, and does not solve the separation problem of other components such as formic acid, water and methyl formate
At the same time, the hydrogen-oil ratio in the refining process is 100:1 to 600:1. It is difficult to separate a large amount of hydrogen from the gas-liquid of low-boiling substances such as methylal, methanol, and methyl formate. The recovery of hydrogen is difficult, energy consumption is high, and the cost of refining is high.

Method used

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  • Refining process of polyoxymethylene dimethyl ether condensation product
  • Refining process of polyoxymethylene dimethyl ether condensation product
  • Refining process of polyoxymethylene dimethyl ether condensation product

Examples

Experimental program
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Effect test

Embodiment 1

[0065] Paraformaldehyde (water content 8%) and methylal according to the molar ratio CH 2 O:DMM=1.2:1 mixed to obtain the condensation raw material, then added to the reaction kettle, and then added the condensation catalyst, the addition amount was 5% of the mass of the condensation raw material. Replace the excess air in the reactor with nitrogen, press it to 1.0MPa, then raise the temperature to 120°C, and react at a stirring speed of 600r / min for 2 hours. After the reaction, filter the catalyst to obtain the condensation product.

[0066] Put the refined catalyst into a fixed-bed refining reactor, and perform reduction pretreatment on the catalyst. The reduction conditions are: 230°C, 0.5MPa, and hydrogen air velocity of 120h -1 , Nitrogen air velocity 480h -1 .

[0067] Then refine the condensation equilibrium product, the process conditions are: reaction pressure 2.0MPa, reaction temperature 120°C, liquid space velocity 1.0h -1 , hydrogen air velocity 50h -1 . The c...

Embodiment 2

[0076] Paraldehyde and methylal according to the molar ratio CH 2O:DMM=1.2:1 mixed to obtain the condensation raw material, then added to the reaction kettle, and then added the condensation catalyst, the addition amount was 2.5% of the mass of the condensation raw material. Replace the excess air in the reactor with nitrogen, then press to 0.6MPa, then raise the temperature to 60°C, and react at a stirring speed of 600r / min for 1h. After the reaction, filter the catalyst to obtain the condensation product.

[0077] Put the refined catalyst into a fixed-bed refining reactor, and perform reduction pretreatment on the catalyst. The reduction conditions are: 230°C, 0.5MPa, and hydrogen air velocity of 120h -1 , Nitrogen air velocity 480h -1 .

[0078] The condensation equilibrium product is mixed with water according to the mass ratio of 100:0.04, and then refined. The process conditions are: reaction pressure 2.0MPa, reaction temperature 120°C, liquid space velocity 1.0h -1 ,...

Embodiment 3

[0082] Concentrate 37% formaldehyde solution to obtain 85% formaldehyde solution, then mix 85% formaldehyde solution and methylal according to the molar ratio CH 2 O:DMM=1.2:1 mixed to obtain the condensation raw material, then added to the reaction kettle, and then added the condensation catalyst, the addition amount was 7.0% of the mass of the condensation raw material. Replace the excess air in the reactor with nitrogen, then press to 1.5MPa, then raise the temperature to 130°C, and react at a stirring speed of 600r / min for a reaction time of 2h. After the reaction, filter the catalyst to obtain a condensation product.

[0083] Put the refined catalyst into a fixed-bed refining reactor, and perform reduction pretreatment on the catalyst. The reduction conditions are: 230°C, 0.5MPa, and hydrogen air velocity of 120h -1 , Nitrogen air velocity 480h -1 .

[0084] Then refine the condensation equilibrium product, the process conditions are: reaction pressure 2.0MPa, reaction ...

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Abstract

The invention discloses a refining process of a polyoxymethylene dimethyl ether condensation product. The process includes: carrying out hydrolysis reaction on water, formaldehyde and formic acid in acondensation equilibrium product under the action of a catalyst, enabling the produced active hydrogen to reduce unhydrolyzed formaldehyde and methyl formate into methanol under the action of the catalyst, thus reaching the multi-effect refining purpose of aldehyde removal, deacidification, degreasing and dehydration of a condensation equilibrium product, and sending the refined product to a subsequent separation unit. According to the invention, the chemical characteristics of a small amount of water, formaldehyde, formic acid and methyl formate in the condensation equilibrium product are skillfully utilized, a hydrolysis reduction reaction network is formed under the action of a catalyst, formaldehyde, formic acid, methyl formate and water in the condensation equilibrium product react with one another to generate methanol which is easy to separate, and the catalytic refining process achieves multi-effect refining of aldehyde removal, deacidification and dehydration on a polyoxymethylene dimethyl ether condensation product.

Description

technical field [0001] The invention provides a process for refining polyoxymethylene dimethyl ether condensation products, which belongs to the field of chemical production processes. Background technique [0002] Polyoxymethylene dimethyl ethers (Polyoxymethylene dimethyl ethers, referred to as PODE n or DMM n ) is a low molecular weight acetal polymer with methyleneoxy as the main chain, and its structural formula is CH 3 (OCH 2 ) n OCH 3 . When n=3~6, the average cetane number reaches over 76, the oxygen content reaches 47~50%, the flash point is 65.6°C, and the boiling point is 160~280°C. The physical properties are very similar to diesel oil. Add 10~15% to diesel oil PODE 3-6 , No need to modify the fuel supply system of the diesel vehicle engine, it can significantly improve the combustion characteristics of diesel, and reduce the emission of particulate pollutants in the combustion exhaust such as nitrogen oxides and PM2.5 in the exhaust of diesel vehicles by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/58C07C43/30C07C29/149C07C29/00C07C31/04B01J35/10B01J37/00B01J37/03B01J37/08
CPCC07C41/58B01J23/002B01J23/80C07C29/149C07C29/00B01J37/0018B01J37/031B01J37/086B01J35/1004B01J2523/00B01J2523/17B01J2523/27B01J2523/41C07C43/30C07C31/04Y02P20/52
Inventor 雷骞邓聪迩张小明陈洪林洪正鹏冯孝庭
Owner DONGFANG HONGSHENG NEW ENERGY APPL TECH RES INST
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