A continuous ring-opening production process of 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 problems of no more than 90%, limited capping reports, etc., and achieve stable and controllable product quality High and mild reaction conditions

Active Publication Date: 2019-01-11
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 of epoxy-terminated polyether
  • A continuous ring-opening production process of epoxy-terminated polyether
  • A continuous ring-opening production process of epoxy-terminated polyether

Examples

Experimental program
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Effect test

Embodiment 1

[0050] In this embodiment, an epoxy-terminated allyl alcohol polyoxyethylene ether continuous ring-opening production process uses allyl alcohol polyoxyethylene ether and epichlorohydrin as raw materials, and uses solid super acid WO 3 / Al 2 O 3 As a catalyst, the basic synthesis route is as follows:

[0051] (1) Fill the solid super acid catalyst into the bed at the upper and lower ends of the continuous flow fixed bed reactor, replace the air with nitrogen, and pass the allyl alcohol polyoxyethylene ether and epichlorohydrin into the mixer by a metering pump for mixing. , And use a heater to heat to a certain temperature, the heated materials are 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 chlorohydrin ether intermediate product;

[0052] (2) The reaction liquid in the collecting tank in step (1) is metered into the air-displaced reaction kettl...

Embodiment 2

[0069] Dissolve 2.1g ammonium metatungstate in 11g deionized water and add to 35g γ-Al 2 O 3 Immerse in a shaking oil bath at 80-90℃ for 24 hours, then add 1.1g pseudo-boehmite and 0.7g 10wt% dilute nitric acid while stirring, and add an appropriate amount of deionized water, squeeze, mix and bond into a semi-wet It is most suitable that the shape can be smoothly extruded into strips. It is extruded into a strip with a diameter of 3mm in a single-screw extruder, then dried at 110°C, baked in an air atmosphere at 750°C for 3h, and sieved to obtain 18-24 meshes. A catalyst with a tungsten oxide content of 5 wt%.

Embodiment 3

[0071] Dissolve 7.7g ammonium metatungstate in 11g deionized water and add to 35g γ-Al 2 O 3 Immerse in a shaking oil bath at 80-90℃ for 24 hours, then add 1.1g pseudo-boehmite and 0.7g 10wt% dilute nitric acid while stirring, and add an appropriate amount of deionized water, squeeze, mix and bond into a semi-wet It is most suitable that the shape can be smoothly extruded into a strip. It is extruded into a long strip with a diameter of 3mm in a single screw extruder, then dried at 110°C, baked in an air atmosphere at 750°C for 3h, and sieved to obtain 18-24 mesh tungsten The catalyst content is 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 an epoxy-terminated polyether continuous ring opening production process, 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 for epoxy resin Diluents, catalysts, crosslinking agents and chain transfer agents, chloride stabilizers, fabric finishing agents and modified silicone oils are important intermediates required for the synthesis of various surfactants and important polymerization intermediates. [0003] At present, the methods of epoxy-terminated polyether can be divided into the following two types: [0004] 1. One-step method: take polyether and epichlorohydrin as raw materials, react in the presence of alkali solids such as sodium hydroxide or potassium hydroxide or its solution...

Claims

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Application Information

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Patent Type & Authority Patents(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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