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Process for producing polyoxymethylene dimethyl ether from methanol and paraformaldehyde

A technology of polyoxymethylene dimethyl ether and process methods, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low yield of process products and achieve good technical effects and good selectivity

Active Publication Date: 2014-12-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The technical problem to be solved by the present invention is the problem that the yield of polyoxymethylene dimethyl ether process products is low in the prior art with methanol and paraformaldehyde as raw materials, and a new process for producing polyoxymethylene dimethyl ether is provided. Has the advantage of high yield

Method used

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  • Process for producing polyoxymethylene dimethyl ether from methanol and paraformaldehyde
  • Process for producing polyoxymethylene dimethyl ether from methanol and paraformaldehyde
  • Process for producing polyoxymethylene dimethyl ether from methanol and paraformaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In the reaction process shown in the accompanying drawings, the volume of the spray tower 9 is 5L, and the volume of the reactor 11 is 2L, equipped with an electric stirring device and heated by an electric heating mantle.

[0030] Fill 300g of HZSM-5 molecular sieve (Si / Al=30) in the liquid phase reaction kettle 11, purge the device with nitrogen, and continuously add 15000g of paraformaldehyde in the mixing tank, the temperature of the mixing tank is 250°C, the formaldehyde generated after heating The gas enters the spray tower 9 after dewatering through the drying tube, and contacts with methanol countercurrently in the spray tower. The feed rate of methanol is 93.75 g / h, the operating pressure of the spray tower is 0.3 MPa, and the operating temperature is 55°C; The formed methanol solution of formaldehyde is fed to the liquid phase reactor 11, and at the same time, a mixed solution of methylal and polyoxymethylene dimethyl ether (n=2, 5, 6) is added to the liquid ph...

Embodiment 2

[0033] Fill 300g of ethylenediaminetetraacetic acid in the liquid-phase reaction kettle 11, purge the device with nitrogen, and continuously add 10,000g of paraformaldehyde into the mixing tank. The temperature of the mixing tank is 250°C. Then enter the spray tower 9, contact with methanol countercurrently in the spray tower, the feed rate of methanol is 62.5 g / h, the operating pressure of the spray tower is 0.3 MPa, and the operating temperature is 55 °C; the methanol solution of formaldehyde formed Feed to the liquid phase reactor 11, and simultaneously add the mixed solution of methylal and polyoxymethylene dimethyl ether (n=2,5,6) into the liquid phase reactor 11, the feed rate is 45.5g / h respectively, 46g / h. The operating conditions of the liquid phase reactor 11 are a reaction temperature of 130° C. and a reaction pressure of 1.50 MPa. The reaction output enters the anion exchange resin bed layer.

[0034] Other operations are the same as in Example 1, continuous reac...

Embodiment 3

[0036] Fill the liquid phase reaction kettle 11 with 300g of strong acidic styrene-based cation exchange resin, purge the device with nitrogen, and continuously add 7500g of paraformaldehyde into the mixing tank, the temperature of the mixing tank is 250°C, and the formaldehyde gas generated after heating is dried After removing water, the tube enters the spray tower 9, and contacts with methanol countercurrently in the spray tower. The feed rate of methanol is 93.75 g / h, the operating pressure of the spray tower is 0.3 MPa, and the operating temperature is 55 ° C; the formed formaldehyde The methanol solution is fed into the liquid phase reactor 11, and the mixed solution of methylal and polyoxymethylene dimethyl ether (n=2,5,6) is added to the liquid phase reactor 11 at the same time, and the feeding rate is 44.8g respectively / h, 69.5g / h. The operating conditions of the liquid phase reactor 11 are a reaction temperature of 100° C. and a reaction pressure of 0.50 MPa. The r...

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Abstract

The invention relates to a process for producing polyoxymethylene dimethyl ether from methanol and paraformaldehyde. The invention mainly solves the problem of low yield of polyoxymethylene dimethyl ether by using the process for producing polyoxymethylene dimethyl ether from methanol and paraformaldehyde. The process is divided into a reaction zone and a separation zone. The reaction zone includes a nitrogen storage tank, a methanol storage tank, a mixing tank with a heater, a drying tube, a spray tower and a liquid phase reaction still. The process steps in the reaction zone are as below: heating paraformaldehyde in the mixing tank into formaldehyde gas; transmitting the formaldehyde gas by nitrogen purging to the drying tube for water removal; introducing the formaldehyde gas into the spray tower from the bottom to the top; conducting countercurrent contact with methanol in the spray tower to form a methanol solution of formaldehyde and sending the solution to a liquid phase reactor; under the effect of a solid acid catalyst, reacting the solution with a mixture recycling to the reactor to generate polyoxymethylene dimethyl ether. The technical scheme well solves the problem, and can be used in industrial production of polyoxymethylene dimethyl ether.

Description

technical field [0001] The invention relates to a process for producing polyoxymethylene dimethyl ether with methanol and paraformaldehyde. 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. According to statistics, in 2011 my country's dependence on foreign oil reached 56.5%, an increase of 1.7 percentage points compared with 2010. Since my country became a net oil importer for the first time in 1993, China's dependence on foreign oil has been rising from 6% in that year, and broke through the warning line of 50% in 2009. 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 fuel substitutes based on coal has...

Claims

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Application Information

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IPC IPC(8): C07C43/30C07C41/56
CPCC07C41/56C07C41/58C07C43/30
Inventor 高晓晨刘奕石竹高焕新
Owner CHINA PETROLEUM & CHEM CORP
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