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A continuous ring-opening production process for epoxy-terminated polyether

A capped polyether, production process technology, applied in the field of continuous ring-opening production process of epoxy-capped polyether, can solve the problem of limited capping report, no more than 90%, and achieve stable and controllable product quality High effect with few by-products

Active Publication Date: 2016-12-21
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] At present, the reports in the literature mainly use small molecule alcohols as capping substrates, and the product yield basically does not exceed 90%, while the capping reports of long-chain polymer polyethers are limited.

Method used

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  • A continuous ring-opening production process for epoxy-terminated polyether
  • A continuous ring-opening production process for epoxy-terminated polyether
  • A continuous ring-opening production process for epoxy-terminated polyether

Examples

Experimental program
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Effect test

Embodiment 1

[0050] This embodiment is a continuous ring-opening production process of epoxy-terminated allyl alcohol polyoxyethylene ether, using allyl alcohol polyoxyethylene ether and epichlorohydrin as raw materials, and using solid super acid WO 3 / Al 2 o 3 As a catalyst, its basic synthesis route is as follows:

[0051] (1) Fill the solid superacid catalyst into the bed layer at the upper and lower ends of the continuous flow fixed bed reactor, replace the air with nitrogen, and the allyl alcohol polyoxyethylene ether and epichlorohydrin are metered into the mixer by the metering pump and mixed , and heated to a certain temperature with a heater, the heated material is continuously added from the upper end of the fixed bed reactor, and the reaction liquid is continuously collected in the collection tank at the lower end of the reactor to obtain the intermediate product of chlorohydrin ether;

[0052] (2) metering the reaction solution in the collection tank in step (1) into the rea...

Embodiment 2

[0069] Dissolve 2.1g of ammonium metatungstate in 11g of deionized water and add to 35g of γ-Al 2 o 3 In the 80-90 ℃ oscillating oil bath, shake and impregnate for 24 hours, then add 1.1g pseudoboehmite and 0.7g 10wt% dilute nitric acid while stirring, and add an appropriate amount of deionized water, knead and knead to form a semi-wet It is most suitable that the shape can be smoothly extruded into strips, extruded into strips with a diameter of 3mm in a single-screw extruder, then dried at 110°C, roasted in an air atmosphere of 750°C for 3 hours, and sieved to obtain 18-24 mesh three Catalyst with 5 wt% tungsten oxide content.

Embodiment 3

[0071] Dissolve 7.7g of ammonium metatungstate in 11g of deionized water and add to 35g of γ-Al 2 o 3 In the 80-90 ℃ oscillating oil bath, shake and impregnate for 24 hours, then add 1.1g pseudoboehmite and 0.7g 10wt% dilute nitric acid while stirring, and add an appropriate amount of deionized water, knead and knead to form a semi-wet It is most suitable that the shape can be extruded into strips smoothly, extruded into strips with a diameter of 3mm in a single-screw extruder, then dried at 110°C, roasted in an air atmosphere of 750°C for 3 hours, and sieved to obtain 18-24 mesh tungsten Catalyst at 18% by weight.

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Abstract

The invention relates to a continuous ring-opening production process for epoxy-terminated polyether and belongs to the technical field of organic polymer compounds. Allyl alcohol polyoxyethylene ether and epichlorohydrin are adopted as raw materials. The process includes mixing the allyl alcohol polyoxyethylene ether and the epichlorohydrin, heating, continuously feeding the mixture to a two-stage fixed bed reactor, performing a ring-opening reaction under catalysis of a solid superacid, adding a product collected by a collecting tank at the lower end of the reactor to a reaction kettle through a metering pump every 2-4 h, adding an alkali and a quaternary ammonium salt catalyst, stirring for 1-4 h while maintaining the temperature, filtering to obtain a crude product, performing vacuum distillation to recover the epichlorohydrin, and purifying to obtain a qualified product. The process is applied for producing the epoxy-terminated polyether, and has advantages of a high equipment utilization rate, a high production efficiency, and the like.

Description

technical field [0001] The invention relates to a continuous ring-opening production process of epoxy-terminated polyether, which belongs to the technical field of organic polymer compounds. Background technique [0002] The molecule of epoxy-terminated allyl alcohol polyoxyethylene ether contains two active sites of carbon-carbon double bond and epoxy bond, which makes it have good reactivity and can be widely used, mainly in epoxy resin Diluents, catalysts, crosslinking agents and chain transfer agents, chloride stabilizers, fabric finishing agents and modified silicone oils are important intermediates for the synthesis of various surfactants and important polymerization intermediates. [0003] At present, the method of epoxy-terminated polyether can be mainly divided into the following two types: [0004] 1. One-step method: use polyether and epichlorohydrin as raw materials, and react in the presence of solid alkali such as sodium hydroxide or potassium hydroxide or its...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/337
CPCC08G65/337C08G2650/06C08G2650/10
Inventor 王俊金一丰张美军陈荧杰
Owner ZHEJIANG HUANGMA TECH
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