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Method for preparing electronic grade dimethoxymethane through lateral-line reactive extraction rectifying

An extractive rectification and extractive rectification tower technology, which is applied in the field of side-line reactive extraction and rectification to prepare electronic grade methylal, can solve the problems of complicated purification process, low purity of reaction products, high utilization cost of by-products, and reduce energy consumption. , the process is simple, the effect of improving the purity and yield

Inactive Publication Date: 2011-08-31
江苏沿江化工资源开发研究院有限公司
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Problems solved by technology

The disadvantages of these methods are the low purity of the reaction product, the complicated purification process, the high utilization cost of the by-products generated by drying, and it is difficult to obtain high purity, especially electronic-grade methylal products with a purity of more than 99.70%.

Method used

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  • Method for preparing electronic grade dimethoxymethane through lateral-line reactive extraction rectifying
  • Method for preparing electronic grade dimethoxymethane through lateral-line reactive extraction rectifying
  • Method for preparing electronic grade dimethoxymethane through lateral-line reactive extraction rectifying

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Embodiment Construction

[0023] The method for preparing electronic-grade methylal by side line reaction extraction rectification of the present invention, with reference to figure 1 The process flow shown and the process condition parameters shown in Table 1 were carried out. The experiment was carried out under normal pressure, and the equipment such as figure 2 and image 3 As shown, the inner diameter of the tower is 22mm, and the φ3*3θ type stainless steel packing is installed inside. The height of the equal plate is 27mm as measured by the standard system.

[0024] Catalyst toluenesulfonic acid is added to the reactor of reactive extraction distillation column B1 at one time, the addition amount is 5.0kg, excess methanol and formaldehyde solution are added continuously by ①, the mass ratio of methanol and formaldehyde solution is 1.2~1.3:1.0, The extractant glycerin is continuously added by ②, with a flow rate of 100kg / h. The two materials ① and ② are simultaneously added to the tower kettle ...

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Abstract

The invention provides a method for preparing electronic grade dimethoxymethane through lateral-line reactive extraction rectifying. The method comprises the following steps: adding acid catalyst in a reactive extraction rectifying tower for the tower bottom at one time, adding mixed liquid of formaldehyde and methanol from the lower middle part of the tower continuously, adding glycerin from theupper middle part of the tower continuously, wherein the temperature of the tower bottom is 81.0-83.0 DEG C, the temperature of the tower top is 39.0-42.0 DEG C; obtaining more than 99.70% of dimethoxymethane from the top of the reactive extraction rectifying tower, rectifying distillate from the tower bottom by a lateral-line rectifying tower, wherein the temperature of the top of the lateral-line rectifying tower is 61.0-64.5 DEG C, the temperature of the tower bottom of the lateral-line rectifying tower is 165.0-169.0 DEG C; obtaining methanol and glycerin separately from the top and bottom of the lateral-line rectifying tower and recycling so that produced water at a lateral line reaches discharge standard. By the method, more than 99.70% of electronic grade dimethoxymethane can be prepared, the purity and yield of dimethoxymethane can be further increased; and the technical process is simple, the energy consumption is obviously reduced and no wastewater is discharged.

Description

technical field [0001] The invention relates to a reaction and separation process of methylal, in particular to a method for preparing electronic-grade methylal by extracting and rectifying a side line reaction. Background technique [0002] Methylal is an important chemical raw material with excellent physical and chemical properties, that is, good solubility, low boiling point, and good compatibility with water. It can be widely used in cosmetics, medicines, household products, industrial automotive supplies, and insecticides. , leather polish, cleaning agent, rubber industry, paint, ink and other products, because methylal has good degreasing ability and volatility, it can replace F11 and F113 and chlorine-containing solvents as a cleaning agent, so it is an alternative Freon, an environmentally friendly product that reduces emissions of volatile organic compounds (VOCs) and air pollution. [0003] For example, pyrethroids such as tetramethrin, permethrin, beta-cypermeth...

Claims

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Application Information

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IPC IPC(8): C07C43/303C07C41/56C07C41/58
Inventor 顾正桂詹其伟
Owner 江苏沿江化工资源开发研究院有限公司
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