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Method for preparing methyl-ended butanol random polyether

A random polyether and butanol-terminated technology, which is applied in the chemical industry, can solve problems such as difficult mass transfer, dark product color, and complicated post-treatment process, so as to promote the mass transfer process, improve the uniformity of concentration distribution, and ensure uniformity Effect

Inactive Publication Date: 2017-03-29
ZHEJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This synthesis method adopts solid base as reaction raw material, mass transfer is difficult in the reaction, the product color is dark, and the post-treatment process of the product is too complicated

Method used

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  • Method for preparing methyl-ended butanol random polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) In the jet loop reactor based on the Venturi effect, (its operation principle is based on the Venturi effect, the loop operation is downward flow, and the end of the jet mixer 1 of the reactor is immersed in the liquid phase of the loop reactor Middle), add 300 kg of butanol random polyether raw material (molecular weight: 300), deoxygenate and nitrogen replacement protection, open the external circulation pump 3 for high-speed jet mixing.

[0036] (2) Control the temperature at 20°C, slowly feed 51kg of monochloromethane raw material and 135kg of liquid caustic soda (30% NaOH solution) into the injection loop reactor, spray and mix and realize the full reaction of the three, and the feeding time for 24 hours. After the addition was complete, the reaction was terminated after continuing the reaction in the jet loop reactor for 8 hours.

[0037] (3) After the reaction is finished, the obtained crude product is neutralized with 50% phosphoric acid, and then undergoes...

Embodiment 2

[0039] (1) In the jet loop reactor based on the Venturi effect, (its operation principle is based on the Venturi effect, the loop operation is downward flow, and the end of the jet mixer 1 of the reactor is immersed in the liquid phase of the loop reactor Middle), add 600kg of butanol random polyether raw material (molecular weight: 6000), deoxygenate and nitrogen replacement protection, open the external circulation pump 3 for high-speed jet mixing.

[0040] (2) Control the temperature at 80°C, slowly feed 10.1 kg of monochloromethane raw material and 11.3 kg of solid potassium hydroxide particles into the jet loop reactor, jet mix and realize the full reaction of the three, and the feeding time is 3 Hour. After the addition was complete, the reaction was terminated after continuing the reaction in the jet loop reactor for 1 hour.

[0041] (3) After the reaction is finished, the obtained crude product is neutralized with 50% phosphoric acid, and then undergoes a post-treatme...

Embodiment 3

[0043] (1) In the jet loop reactor based on the Venturi effect, (its operation principle is based on the Venturi effect, the loop operation is downward flow, and the end of the jet mixer 1 of the reactor is immersed in the liquid phase of the loop reactor Middle), add butanol random polyether raw material (molecular weight: 1025) 512.5kg, deoxygenation and nitrogen replacement protection, open the external circulation pump 3 for high-speed jet mixing.

[0044] (2) Control the temperature at 30°C, slowly feed 32.8kg of monochloromethane raw materials and 15.6kg of solid sodium hydride particles into the jet loop reactor, jet mix and realize the full reaction of the three, and the feeding time is 12 Hour. After the addition was complete, the reaction was terminated after continuing the reaction in the jet loop reactor for 4 hours.

[0045] (3) After the reaction is finished, the obtained crude product is neutralized with 50% phosphoric acid, and then undergoes a post-treatment ...

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Abstract

The invention discloses a method for preparing methyl-ended butanol random polyether. The method comprises the following steps: adding a butanol random polyether raw material into a Venturi effect-based jet loop reactor through a material inlet; removing oxygen and introducing inert gases for replacement and protection; starting an outer circulating pump for high-speed jet mixing; and controlling the temperature to be 20-80 DEG C, slowly adding a methane chloride raw material and a bas raw material respectively through a methane chloride inlet and the material inlet, and the like. The system belongs to a kinetic control system, and the side effect is sufficiently inhibited. Furthermore, according to the characteristic of high side reaction activation energy, a low-temperature method is adopted for kinetic reaction control, the hydrolysis reaction of methane chloride is inhibited, and thus the reaction system has higher selectivity. Finally, the methyl-ended butanol random polyether product has the color of less than 30 and the ending rate of more than 98 percent.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a method for preparing methyl-terminated butanol random polyether. Background technique [0002] Butanol random polyether is a macromolecular product obtained by ring-opening copolymerization of butanol, ethylene oxide and propylene oxide. It has excellent defoaming, wetting and emulsifying properties. It can be used as a defoamer in coatings and as a leveling agent after modified silicone oil. Butanol random polyether has good water solubility and viscosity-temperature characteristics, reversible solubility, good lubrication, heat resistance, antistatic and surface properties, no coking, low foam and other characteristics. It is used in textiles, metal processing, equipment lubrication and other fields. The Ucon series of United Carbide and the Synalox series of Dow Chemical Company have such products, which are mainly used for water-based quenching fluid, lubrican...

Claims

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Application Information

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IPC IPC(8): C08G65/337C08G65/28
CPCC08G65/337C08G65/2609C08G65/2696
Inventor 张治国朱建华索艳格杨振施旭亮
Owner ZHEJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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