High-production-efficiency polytetramethylene ether glycol preparation method

A polytetramethylene ether glycol and production efficiency technology, which is applied in the field of high production efficiency polytetramethylene ether glycol preparation, can solve the problem that the polymerization efficiency of polytetramethylene ether glycol has not been studied in depth Improvements and other issues to achieve fast and efficient recycling

Active Publication Date: 2020-08-25
杭州三隆新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Although the prior art including the above-mentioned patent application has disclosed a variety of different preparation methods of polytetramethylene ether glycol, there is no in-depth study on how to

Method used

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  • High-production-efficiency polytetramethylene ether glycol preparation method
  • High-production-efficiency polytetramethylene ether glycol preparation method
  • High-production-efficiency polytetramethylene ether glycol preparation method

Examples

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Example Embodiment

[0071] A method for preparing polytetramethylene ether glycol with high production efficiency, comprising the following steps:

[0072] 1) The tetrahydrofuran and the heteropolyacid catalyst added with diethyl ether are fully mixed through the intensified disperser, and the temperature is maintained at 50~52 ℃ and then enters the main reactor for polymerization reaction; the intensified disperser is followed by static mixing from bottom to top. It consists of a section, a distribution plate and a circulating heat exchange section.

[0073] 2) The catalyst settled in the main reaction kettle is sent out and recycled from the bottom of the kettle, and the obtained reaction solution is discharged from the top of the kettle and then enters the first-level centrifuge, and most of the catalysts are separated and recycled by centrifugal action.

[0074] 3) The remaining reaction solution enters the first distillation column to remove most of the tetrahydrofuran and all ether, and the...

Example Embodiment

[0091] Example 1

[0092] A method for preparing polytetramethylene ether glycol with high production efficiency, comprising the following steps:

[0093] 1) The tetrahydrofuran and the heteropolyacid catalyst added with diethyl ether are fully mixed through the intensified disperser, and the temperature is maintained at 50~52 ℃ and then enters the main reactor for polymerization reaction; the intensified disperser is followed by static mixing from bottom to top. It consists of a section, a distribution plate and a circulating heat exchange section. The heteropolyacid catalyst is micron phosphotungstic heteropolyacid, and the volume content of the catalyst in the reaction solution is 38%. The content of ether in the tetrahydrofuran is 1.5 wt%, the moisture of the organic phase in the system is 0.3%, and the charging coefficient of the main reaction kettle is 100%.

[0094] 2) The catalyst settled in the main reaction kettle is sent out and recycled from the bottom of the ket...

Example Embodiment

[0100] Example 2

[0101] A method for preparing polytetramethylene ether glycol with high production efficiency, comprising the following steps:

[0102] 1) The tetrahydrofuran and the heteropolyacid catalyst added with diethyl ether are fully mixed through the intensified disperser, and the temperature is maintained at 50~52 ℃ and then enters the main reactor for polymerization reaction; the intensified disperser is followed by static mixing from bottom to top. It consists of a section, a distribution plate and a circulating heat exchange section. The heteropolyacid catalyst is a phosphotungstic heteropolyacid, and the volume content of the catalyst in the reaction solution is 35%. The content of ether in the tetrahydrofuran is 1wt%, and the charging coefficient of the main reactor is 100%.

[0103] 2) The catalyst settled in the main reaction kettle is sent out and recycled from the bottom of the kettle, and the obtained reaction solution is discharged from the top of the...

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Abstract

The invention relates to the field of chemical engineering, and discloses a high-production-efficiency polytetramethylene ether glycol preparation method which comprises the steps: 1) mixing tetrahydrofuran added with diethyl ether and a catalyst through an enhanced disperser, and carrying out a polymerization reaction at a temperature of 50-52 DEG C; 2) separating the catalyst from the reaction liquid through centrifugation; 3) distilling the residual reaction liquid to remove most tetrahydrofuran and all diethyl ether; mixing the concentrated solution with an extracting agent and then centrifuging; 4) adsorbing the residual mixed solution through an adsorption column, thoroughly removing the catalyst, and removing tetrahydrofuran through distillation; and 5) carrying out settling separation on the residual mixed solution at 38 DEG C, and treating by a refiner to obtain the polytetramethylene ether glycol. On one hand, a proper amount of diethyl ether is added into tetrahydrofuran, onthe other hand, the dispersity of the catalyst is improved through the reinforced disperser to increase the reaction speed, the reaction temperature is properly reduced through circulating heat exchange, the equilibrium conversion rate is increased, and thus the upper limit of the yield of polytetramethylene ether glycol is increased.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing polytetramethylene ether glycol with high production efficiency. Background technique [0002] Polytetramethylene ether glycol was first prepared by cationic ring-opening polymerization of tetrahydrofuran (THF) in the 1930s. Its synthetic reaction formula is as follows: [0003] c 4 h 8 O+H 2 O====(initiator)====HO-[-C 4 h 8 O-] n -H [0004] Common synthesis methods of polytetramethylene ether glycol include acetic anhydride-perchloric acid method, concentrated sulfuric acid method, fluorosulfonic acid method, clay method, heteropolyacid method, etc. Among them, with the continuous strengthening of environmental protection awareness, and due to the consideration of process and product quality, the heteropoly acid method has received more and more attention and application. [0005] The Chinese invention whose patent number is CN00811571.0 disclose...

Claims

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Application Information

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IPC IPC(8): C08G65/20C08G65/30B01F5/06B01J31/28B01J35/02
CPCC08G65/20C08G65/30B01J31/28B01J35/0066B01J35/023B01F25/431Y02P20/584
Inventor 施可彬易杰
Owner 杭州三隆新材料有限公司
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