New preparing method of allyl alcohol random polyether glycidyl ether

A technology of glycidyl ether and random polyether, which is applied in the chemical field, can solve the problems of low reactivity, increasing difficulty in preparing allyl alcohol random polyether glycidyl ether, difficulty in popularizing raw material costs, and many by-products, etc. The effect of ensuring uniformity, reducing side reactions and improving reaction efficiency

Inactive Publication Date: 2017-03-08
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

Chinese patents CN104387576A, CN101928389A, CN102050943A and CN102060989A report several preparation methods of glycidyl ether group-terminated allyl alcohol polyether, using allyl alcohol polyether as raw material, through catalyst NaH, or raw material NaH, or solid base as Raw materials, glycidyl ether group-terminated allyl alcohol polyether has been prepared in a stirred tank reactor, but there are disadvantages such as high cost of raw materials and difficulty in popularization, too strong alkalinity of raw materials, deep color of products, and many by-products, etc., especially For random polyethers, since the terminal secondary hydroxyl groups are the main ones, its low reactivity sharply increases the difficulty in the preparation of allyl alcohol random polyether glycidyl ethers.

Method used

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  • New preparing method of allyl alcohol random polyether glycidyl ether

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (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 400kg of allyl alcohol random polyether raw material (molecular weight: 400), deoxygenate and nitrogen replacement protection, open the external circulation pump 3 for high-speed jet mixing.

[0033] (2) Control the temperature at 30°C, slowly feed 93.5 kg of epichlorohydrin raw materials and 135 kg of liquid caustic soda (30% NaOH solution) into the jet loop reactor, jet mix and realize the full reaction of the three, The feed time was 20 hours. After the addition was complete, the reaction was terminated after continuing the reaction in the jet loop reactor for 8 hours.

[0034] (3) After the reaction is finished, the obtained crude product is neutralized with 50% phosphoric acid, and then undergoes a post-tre...

Embodiment 2

[0036] (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 allyl alcohol random polyether raw material (molecular weight: 6000), deoxygenation and nitrogen replacement protection, open the external circulation pump 3 for high-speed jet mixing.

[0037] (2) Control the temperature at 120°C, slowly feed 14.8 kg of epichlorohydrin raw materials and 9.0 kg of solid potassium hydroxide particles into the injection loop reactor, spray and mix to achieve a full reaction of the three, and the feeding time for 5 hours. After the addition was complete, the reaction was terminated after continuing the reaction in the jet loop reactor for 1 hour.

[0038] (3) After the reaction is finished, the obtained crude product is neutralized with 50% phosphoric acid, and then underg...

Embodiment 3

[0040] (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 512.5 kg 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.

[0041] (2) Control the temperature at 60°C, slowly feed 60.1 kg of epichlorohydrin raw materials and 15.60 kg 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 hours. After the addition was complete, the reaction was terminated after continuing the reaction in the jet loop reactor for 4 hours.

[0042] (3) After the reaction is finished, the obtained crude product is neutralized with 50% phosphoric acid, and then undergoes a post-...

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Abstract

The invention discloses a new preparing method of allyl alcohol random polyether glycidyl ether. The preparing method comprises the steps of adding an allyl alcohol random polyether raw material in a jet loop reactor based on a venturi effect through a feed inlet of materials, conducting deoxygenization and pumping into inert gases to be subjected to replacement protection, and opening an external circulating pump to be subjected to high speed spraying mixture; controlling the temperature at 30-120 DEG C, slowly adding an epoxy chloropropane raw material and an alkali raw material into the jet loop reactor through the feed inlet of epoxy chloropropane and the feed inlet of the material respectively, and the like. Due to the fact that the system belongs to a system of kinetic control, and a side reaction is inhibited sufficiently, thus the selectivity of a reaction system is higher. The new preparing method is especially applicable to allyl alcohol random polyether of which molecular tail end is secondary hydroxyl, the color luster of the finally obtained product, namely, the allyl alcohol random polyether glycidyl ether product, is less than 40, and the stop end rate of the product is more than 96%.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a new preparation method of allyl alcohol random polyether glycidyl ether. Background technique [0002] Polymerizable surfactant is a kind of surfactant containing polymerizable groups. As a functional surfactant, it not only has significant surface activity, but also can undergo homogeneous (co)polymerization reaction under certain triggering conditions. Polymerizable surfactants can be divided into allyl type, styrene type, (meth)acrylic acid type, acrylamide type and maleic acid type according to the polymerization active group, and can be divided into anion, Nonionic and cationic. Among them, allyl polyether has good hydrophilicity, emulsifying ability and chemical stability, and is a polymerizable nonionic surfactant with excellent performance, so it plays an important role in polymer synthesis. However, the traditional allyl polyether is not resistant to acid, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/337
CPCC08G65/337C08G2650/06
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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