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Method for synthesizing polyformaldehyde dimethyl ether by taking methanol and methanal as raw materials

A polyoxymethylene dimethyl ether and methanol technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as difficult separation, high equipment requirements, and large environmental pollution, and achieve high reaction conversion rate, The effect of good technical effect and high product yield

Inactive Publication Date: 2012-01-18
HENAN COAL CHEM IND GROUP INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Dimethyl ether was first proposed as a diesel additive. However, due to its poor cold start performance, high vapor pressure at room temperature, and easy air resistance, the cost of DME as an alternative fuel for vehicles has increased significantly.
US5,746,785 and WO2006 / 045506A1 describe the synthesis process of polyoxymethylene dimethyl ether with methylal and paraformaldehyde as raw materials using protonic acid (such as formic acid, sulfuric acid and trifluoromethanesulfonic acid) as a catalyst. Although protonic acid catalysts are cheap and easy to obtain, they are highly corrosive, difficult to separate, cause great environmental pollution, and require high equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 2 g of catalyst SO to a 300 ml tank reactor 4 2- / Fe 2 o 3 , 100 ml methanol and 300 ml formaldehyde, at 130 oC React with 0.8MPa autogenous pressure for 4h, extract the sample and analyze it by gas chromatography after centrifugation. The product contains polyoxymethylene dimethyl ether (CH 3 O(CH 2 O) n CH 3 ) and unreacted raw material methanol and formaldehyde, the composition of which is distributed as follows (in % by weight): methanol 3.1%; methylal 22.5%; formaldehyde 4.7%; n=2, 25.8%; n=3, 24.2%; n =4, 11.3%; n=5~10, 8.2%; n>10, margin.

[0017] The solid superacid SO used 4 2- / Fe 2 o 3 Catalyst preparation method:

[0018] In 200ml of 0.5mol / L FeCl 3 Add 12.5 mass% NH to the solution 3 ·H 2 O, adjust pH=9, let stand for 24h, filter and wash until free of Cl - Check out. 100 o C drying, grinding. The powder is added to 1mol / L (NH 4 ) 2 SO 4 In solution, immerse for 14h, dry, 600 o C roasting.

Embodiment 2

[0020] 2 g of catalyst Cl was added to a 300 ml tank reactor - / TiO 2 , 100 milliliters of methanol and 150 milliliters of formaldehyde were reacted at 130oC and 0.6 MPa autogenous pressure for 4 hours, and the samples were extracted and analyzed by gas chromatography after centrifugation. The product contains polyoxymethylene dimethyl ether (CH 3 O(CH 2 O) n CH 3 ) and unreacted raw material methanol and formaldehyde, the composition of which is distributed as follows (in % by weight): methanol 38.5%; methylal 32.1%; formaldehyde 0%; n=2, 17.1%; n=3, 10.2%; n =4, 0%; n=5~10, 0%; n>10, margin.

[0021] The solid superacid Cl used - / TiO 2 Catalyst preparation method:

[0022] Measure 100ml of TiCl 4 The solution was quickly added 12.5% ​​by mass of NH in a 200 ml beaker 3 ·H 2 O until there is no white smoke, filter and wash for 100 o C drying. The powder is added into the hydrochloric acid solution of 2mol / L, soaked for 2h, dried, 600 o C roasting.

Embodiment 3

[0024]Add 2 g of catalyst SO to a 300 ml tank reactor 4 2- / ZrO 2 , 100 ml methanol and 300 ml formaldehyde, at 80 o C was reacted for 4 hours, and the sample was extracted and analyzed by gas chromatography after centrifugation. The product contains polyoxymethylene dimethyl ether (CH 3 O(CH 2 O) n CH 3 ) and unreacted raw material methanol and formaldehyde, the composition of which is distributed as follows (in % by weight): methanol 14.3%; methylal 42.2%; formaldehyde 3.2%; n=2, 11.2%; n=3, 8.7%; n =4, 5.5%; n=5~10, 14.4%; n>10, margin.

[0025] The solid superacid SO used 4 2- / ZrO 2 Catalyst preparation method:

[0026] Weigh 100 g of ZrOCl 2 Place in a 400ml beaker to make a 15% by mass aqueous solution, add 12.5% ​​by mass of NH dropwise 3 ·H 2 O, adjust pH=9, age for 3h, filter with suction, wash until free of Cl - Check out. The above filter cake 100 o C drying, grinding. Add 10 g of the above powder to 150 ml of 0.5 mol / L H 2 SO 4 In solution, soa...

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Abstract

The invention relates to a method for synthesizing polyformaldehyde dimethyl ether by taking methanol and methanal as raw materials. Dimethoxymethane or methanol or the mixture of the dimethoxymethane and the methanol and methanal are used as raw materials, the mass ratio of the dimethoxymethane or the methanol or the mixture of the dimethoxymethane and the methanol to the methanal is 0.2-10:1, the reaction temperature is 70-200 DEG C, the reaction pressure is 0.2-6MPa, solid super strong acid is used as a catalyst for catalytic reaction to prepare polyformaldehyde dimethyl ether, the dosage of the catalyst accounts for 0.05-10% of the total weight of the raw materials, wherein the solid super acid catalyst comprises the following components in percentage by weight: 20-70% of at least one of sulphuric acid, hydrochloric acid or peroxosulfuric acid or salt thereof, and the balance of carrier selected from at least one of ZrO2, TiO2, SiO2, Fe2O3, SnO2, WO3 and Al2O3. The method disclosed by the invention solves the existing technical problem of high cost in producing the polyformaldehyde dimethyl ether.

Description

technical field [0001] The invention relates to a method for synthesizing polyoxymethylene dimethyl ether with methanol and formaldehyde as raw materials. 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 to 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 performance, high vapor pressure at room temperature, and easy air resistance, the cost of DM...

Claims

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Application Information

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IPC IPC(8): C07C43/30C07C41/56B01J27/053B01J27/135
Inventor 李丰蒋元力李伍成魏灵朝闫捷尚如静丁建础贾金才张秀全徐才华徐柳王占修
Owner HENAN COAL CHEM IND GROUP INST
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