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Process for preparing methylal

A technology for methylal and formaldehyde is applied in the field of preparation of methylal to achieve the effects of low cost, simple operation and easy sharing

Inactive Publication Date: 2014-12-24
山东滨州新天阳化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] For the synthesis of methylal from methanol and formaldehyde, inorganic salts (such as sulfuric acid, hydrochloric acid), and Lewis acids (such as ferric chloride, trichloride Aluminum, etc.) as catalysts, but these catalysts are difficult to separate and recover, are highly corrosive and have low catalyst activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] After the raw material formaldehyde is mixed with methanol, it is pumped into the heater for preheating, and the preheated mixed solution enters the pre-reactor. At this time, part of the raw material undergoes condensation and dehydration reaction to form methylal. There is a catalyst in the pre-reactor. ;

[0032] The material reacted by the pre-reactor enters the rectification tower, and the hot gas rises and contacts the refluxed cold liquid countercurrently. The methylal gas obtained from the top of the tower enters the cooler and is cooled to 90% methylal solution.

[0033] The above molar ratio of formaldehyde to methanol is 1:1.5.

[0034] The temperature at which the material is preheated in the heater is 70°C.

[0035] The molar ratio of the methylal gas obtained from the top of the tower to the refluxed methylal solution is 2:1.

[0036] The catalyst is a strongly acidic large-pore cation exchange resin, and the consumption of the catalyst is 4% of the weig...

Embodiment 2

[0043] After the raw material formaldehyde is mixed with methanol, it is pumped into the heater for preheating, and the preheated mixed solution enters the pre-reactor. At this time, part of the raw material undergoes condensation and dehydration reaction to form methylal. There is a catalyst in the pre-reactor. ;

[0044] The material reacted by the pre-reactor enters the rectification tower, and the hot gas rises and contacts the refluxed cold liquid countercurrently. The methylal gas obtained from the top of the tower enters the cooler and is cooled to 85% methylal solution.

[0045] The molar ratio of formaldehyde to methanol is 1:2.

[0046] The temperature at which the material is preheated in the heater is 60°C.

[0047] The molar ratio of the methylal gas obtained from the top of the tower to the refluxed methylal solution is 1:1.

[0048] The catalyst is a strongly acidic large-pore cation exchange resin, and the consumption of the catalyst is 2% of the weight of th...

Embodiment 3

[0054] After the raw material formaldehyde is mixed with methanol, it is pumped into the heater for preheating, and the preheated mixed solution enters the pre-reactor. At this time, part of the raw material undergoes condensation and dehydration reaction to form methylal. There is a catalyst in the pre-reactor. ;

[0055] The material reacted by the pre-reactor enters the rectification tower, and the hot gas rises and contacts the refluxed cold liquid countercurrently. The methylal gas obtained from the top of the tower enters the cooler and is cooled to a 92% methylal solution.

[0056] The above molar ratio of formaldehyde to methanol is 1:3.

[0057] The molar ratio of formaldehyde to methanol is 1:3.

[0058] The temperature at which the material is preheated in the heater is 80°C.

[0059] The molar ratio of the methylal gas obtained from the top of the tower to the refluxed methylal solution is 2:3.

[0060] The catalyst is a strongly acidic large-pore cation exchange ...

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PUM

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Abstract

The invention belongs to the technical field of chemical engineering, and in particular relates to a process for preparing methylal. The process comprises the following steps: mixing raw materials, namely, formaldehyde and methanol, feeding the mixed materials into a heater, preheating, further feeding the preheated materials into a prereactor and performing condensation and dehydration reaction to generate methylal; feeding the materials which are reacted in the prereactor into a distillation tower, raising the hot gas to be in countercurrent contact with a cold liquid, feeding a methylal gas obtained from the tower top into a cooler, and cooling into a methylal solution. The purity of the methylal which is prepared by using the method provided by the invention is as high as 98%, the methyal yield is as high as 88%, the process procedures are short, the operation is simple, the catalyst and the product are easy to share, the industrialization production can be expanded, and the cost is low.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of methylal. Background technique [0002] With the continuous development of coal chemical industry, the technology of synthesizing methanol from coal has matured. As one of the most important downstream products of methanol, methylal has a very wide application prospect because of its good physical and chemical properties. Methylal oxidation can produce high-concentration formaldehyde; because methylal has good oil removal ability and volatility, it can be used as a cleaning agent to replace F11, F13 and chlorinated solvents. ) emissions and reduce air pollution (Lin Bin, a new generation of environmentally friendly solvents - methylal, 2008); methylal itself is an oxygenated fuel, when used as a diesel additive, it can significantly reduce the harmful emissions; adding a certain amount of methylal to methanol gasoline can improve it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/56C07C43/30
CPCC07C41/56C07C41/58
Inventor 吴振峰王志村张延明李光军闫光国王志英
Owner 山东滨州新天阳化工有限责任公司
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