Novel method for terminating allyl alcohol irregular polyether methyl

A random polyether, methyl-terminated technology, applied in ether preparation, ester reaction to ether, organic chemistry, etc., can solve the problems of complex post-treatment process, difficult mass transfer, deep color of the product, etc., and achieve uniform concentration distribution Improve and promote the mass transfer process and ensure the effect of uniformity

Inactive Publication Date: 2017-04-19
ZHEJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis method adopts solid alkali as the reaction raw material, the mass transfer is difficult during the reaction, the product color is deep, and the post-treatment process of the product is complicated.

Method used

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  • Novel method for terminating allyl alcohol irregular polyether methyl

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) In the jet loop reactor based on the Venturi effect, (the operating 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 400kg of allyl alcohol random polyether raw material (molecular weight: 400), deoxygenate and nitrogen replacement protection, turn on 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, the obtained crude product is neutralized with 50% phosphoric acid, and then undergoes a po...

Embodiment 2

[0039] (1) In the jet loop reactor based on the Venturi effect, (the operating 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 allyl alcohol random polyether raw material (molecular weight: 6000), deoxygenate and nitrogen replacement protection, turn on the external circulation pump 3 for high-speed jet mixing.

[0040] (2) Control the temperature at 70°C, slowly feed 10.1kg of monochloromethane raw material and 11.3kg of solid potassium hydroxide particles into the injection loop reactor, spray and mix to realize the full reaction of the three, and the feeding time is 4 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, the obtained crude product is neutralized with 50% phosphoric acid, and then undergoes a post-t...

Embodiment 3

[0043] (1) In the jet loop reactor based on the Venturi effect, (the operating 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 512.5kg of allyl alcohol random polyether raw material (molecular weight: 1025), deoxygenate 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 32.8 kg of monochloromethane raw materials and 15.6 kg of solid sodium hydride particles into the injection loop reactor, spray and mix to achieve a 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, the obtained crude product is neutralized with 50% phosphoric acid, and then undergoes a post-trea...

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Abstract

The invention discloses a novel method for terminating allyl alcohol irregular polyether methyl. The novel method comprises the following steps of: adding allyl alcohol irregular polyether raw materials through a material inlet in a jetting loop reactor based on Venturi effect, deoxidizing and introducing inert gases for replacement and protection, and starting an external circulating pump to carry out high-speed jetting mixing; and at a control temperature ranging from 20 DEG C to 70 DEG C, slowly adding a methane chloride raw material and an alkali raw material into the jetting loop reactor through a methane chloride raw material feeding hole and a material feeding hole separately, and the like. According to the novel method disclosed by the invention, this system belongs to a dynamic control system, side reactions are restrained sufficiently, a low-temperature method is further adopted to carry out dynamic reaction control according to the characteristic that activation energy of side reactions is high, hydrolysis reaction of methane chloride is restrained, and isomerization reaction of allyl is further restrained, and therefore, selectivity of a reaction system is higher. Finally obtained allyl alcohol irregular polyether methyl terminated product has color and luster smaller than 30, and has a terminating rate greater than 98%.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a new method for capping allyl alcohol random polyether methyl groups. Background technique [0002] As a polyether with special structure and performance, alkyl-terminated polyether has been widely used in the fields of synthetic lubricating oil, daily chemical industry and chemical fiber oil. [0003] Due to the existence of double bonds and the adjustable polyether chain segment, allyl alcohol polyether and its end-capped products can be added with active hydrogen or copolymerized with unsaturated compounds to endow the product with good lubricating effect, soft effect and good spreading It is widely used in polyurethane soft or hard foam stabilizer, agricultural silicone synergist, construction water reducer, low foam detergent, lubricating oil, base oil, textile defoamer, etc. field. Allyl alcohol polyether-capped products, because the active hydrogen of the t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/332C08G65/324C07C41/16C07C43/14
CPCC08G65/3322C07C41/16C08G65/324
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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