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A kind of synthetic method of epoxy-terminated butanol polyoxyethylene polyoxypropylene ether

A technology of polyoxyethylene polyoxypropylene ether and synthesis method, which is applied in the field of organic compound synthesis, can solve problems such as limited catalyst cycle life, catalyst failure to recycle, catalyst equipment corrosion, etc., and achieve high selectivity and good industrial application value , less side effects

Active Publication Date: 2017-07-21
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The active components of the catalyst used in the reported patent, boron trifluoride and concentrated sulfuric acid, will be lost as the reaction progresses, so the catalyst cannot be recovered. These lost catalysts will cause serious corrosion to the equipment, and the cycle life of the catalyst is limited. Moreover, the reported patents are mainly end-capped single molecules, and there is no epoxy group-terminated polyether with long chain and large molecular weight.

Method used

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  • A kind of synthetic method of epoxy-terminated butanol polyoxyethylene polyoxypropylene ether
  • A kind of synthetic method of epoxy-terminated butanol polyoxyethylene polyoxypropylene ether
  • A kind of synthetic method of epoxy-terminated butanol polyoxyethylene polyoxypropylene ether

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Embodiment 1

[0050] Dissolve 1.6g of ammonium metatungstate in 6.5ml of deionized water, add to 12.6g of Zr(OH) 4 immersion at 80-90°C for 24 hours, then dried at 110°C, and calcined at 700°C for 3 hours in an air atmosphere to obtain a catalyst with a tungsten content of 10wt%.

Embodiment 2

[0052] Dissolve 0.75g of ammonium metatungstate in 6.5ml of deionized water, add to 12.6g of Zr(OH) 4 immersion at 80-90°C for 24 hours, then dried at 110°C, and calcined at 700°C for 3 hours in an air atmosphere to obtain a catalyst with a tungsten content of 5wt%.

Embodiment 3

[0054] Dissolve 2.6g of ammonium metatungstate in 6.5ml of deionized water, add to 12.6g of Zr(OH) 4 immersion at 80-90°C for 24 hours, then dried at 110°C, and calcined at 700°C for 3 hours in an air atmosphere to obtain a catalyst with a tungsten content of 15wt%.

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Abstract

The invention relates to a method for synthesizing epoxy-terminated butanol polyoxyethylene polyoxypropylene ether, and belongs to the technical field of organic compound synthesis. will WO 3 / ZrO 2 The catalyst is added to the butanol polyoxyethylene polyoxypropylene ether, and epichlorohydrin is slowly added dropwise under the protection of nitrogen. After the reaction is completed, the catalyst is recovered by filtration, and the epichlorohydrin is recovered by distillation under reduced pressure to obtain the intermediate of the chlorohydrin ether. The product is added with solid alkali and quaternary ammonium salt catalyst, and under nitrogen protection, after the reaction is filtered and demineralized, neutralized by adding neutralizer, and then adding adsorbent, and then refining. The invention is applied to the synthesis of epoxy-terminated polyoxyethylene polyoxypropylene ether, which not only effectively recovers and recycles the catalyst for more than 15 times, avoids the impact of the strong acid catalyst on equipment and operating environment, but also realizes the end-capping rate. The balance of color and luster not only imparts high reactivity, but also ensures the quality index of the finished product.

Description

technical field [0001] The invention relates to a method for synthesizing epoxy-terminated butanol polyoxyethylene polyoxypropylene ether, which belongs to the technical field of organic compound synthesis. Background technique [0002] The molecule of epoxy-terminated butanol polyoxyethylene polyoxypropylene ether contains epoxy-based active groups, which has good reactivity and is mainly used in epoxy resin diluents, catalysts, cross-linking agents and chain transfer agents , chloride stabilizer, fabric finishing agent and modified silicone oil, etc., are important intermediates for the synthesis of various surfactants and important polymerization intermediates. [0003] At present, there are two main methods of epoxy-terminated polyether: [0004] The first is a one-step method, that is, a phase transfer method: polyether and epichlorohydrin are used as raw materials, and the target product is directly generated by reacting in the presence of a phase transfer catalyst an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/331C08G65/08
CPCY02P20/582Y02P20/584
Inventor 张美军金一丰颜吉校陈荧杰王月芬
Owner ZHEJIANG HUANGMA TECH
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