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A kind of allyl alcohol polyoxypropylene polyoxyethylene random polyether and preparation method thereof

A technology of allyl alcohol polyoxypropylene polyoxyethylene and atactic polyether, which is applied in the field of organic polymer compound preparation, can solve the problems of uneven foam opening, difficult molecular weight, and high content, and achieve chain growth speed, Increase the effect of mass transfer and ensure the effect of mass transfer efficiency

Active Publication Date: 2020-04-14
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the synthesis method of patent CN101914200 A and patent CN 102134313 A, allyl alcohol polyoxypropylene polyoxyethylene random is synthesized by using sodium allyl alcohol / sodium methallylate or potassium allyl alcohol / potassium methallylate as a catalyst. After the polyether product is directly neutralized with acid, potassium and sodium metal ions are not removed, so it cannot be directly used for polyether modification of silicone oil. The presence of metal ions will deactivate the chloroplatinic acid catalyst in the reaction of polyether modified silicone oil, and The synthesized allyl alcohol random polyether has a high content of by-products of propylene-based polyether, which affects the foaming quality of the product
[0008] To sum up, in the synthesis of random polyether, a class of bimetallic or multimetallic cyanides such as DMC and MMC are used as catalysts to synthesize high molecular weight allyl alcohol polyethers. However, due to the residual catalyst, it is not suitable for silicone oil. There are defects in the polyether modification industry, which will poison and deactivate the catalyst for the reaction between hydrogen-containing silicone oil and allyl alcohol. It is necessary to increase the amount of catalyst, and the synthesized polyether modified silicone oil is used as a foam stabilizer for polyurethane soft foam foaming When the foam opening is uneven, it will affect the product quality
The other is to use alkali metal catalysts such as sodium allylate, potassium allylate, and KOH to synthesize allyl alcohol polyethers. Under alkaline and high temperature conditions, allyl groups will be isomerized into propenyl groups. Alcohol polyether is partially isomerized into acryl polyether, and propylene oxide will also be isomerized into propylene alcohol or allyl alcohol, especially when the allyl alcohol polyether reaches a certain molecular weight, the growth rate of the allyl alcohol polyether chain decreases. Slow, but the isomerization speed of propylene oxide to propenyl alcohol is relatively fast, and propenyl alcohol can react with ethylene oxide and propylene oxide, making it difficult to achieve a molecular weight of allyl alcohol polyether above 2000; and propenyl alcohol polyether cannot Reaction with hydrogen-containing silicone oil, residual acryl polyether in polyether-modified silicone oil affects the foam-leveling effect of polyether-modified silicone oil, making polyurethane flexible foam open cells unevenly, affecting product quality, and seriously affecting product performance

Method used

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  • A kind of allyl alcohol polyoxypropylene polyoxyethylene random polyether and preparation method thereof
  • A kind of allyl alcohol polyoxypropylene polyoxyethylene random polyether and preparation method thereof
  • A kind of allyl alcohol polyoxypropylene polyoxyethylene random polyether and preparation method thereof

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Effect test

Embodiment 1

[0035] Embodiment 1: Preparation of allyl alcohol random polyether oligomer

[0036] Add 400g of allyl alcohol and 0.6g of boron trifluoride ether into a 2.5L high-pressure stirred reactor, and vacuumize with a vacuum pump, using N 2 Replace the air in the reactor. After three replacements, turn off the vacuum and start to heat up the material to 30°C under a vacuum degree ≥ -0.096MPa. After that, continue to add 980g of a mixture of ethylene oxide and propylene oxide, ethylene oxide and The weight ratio of propylene oxide is 1:1. Control the reaction temperature at 20-40°C, and the pressure in the reactor at -0.05-0.2Mpa. After the addition, keep warm and continue the reaction until the pressure no longer drops. The entire reaction addition time is about 6h. After the reaction is completed, vacuum degassing, keep the vacuum ≥ -0.098MPa for 10 minutes, and then discharge to obtain the finished product for later use. The product is analyzed by a nuclear magnetic resonance ana...

Embodiment 2

[0043] Embodiment 2: experiment with theoretical molecular weight 2000 feed intake

[0044] Add 150g of allyl alcohol polyether oligomer and 3.0g of sodium methoxide into a 2.5L stirring and 2-way external circulation reactor, and use N 2 After replacing the air in the reaction kettle three times, under the vacuum degree ≥ -0.096MPa, start to vacuumize and raise the temperature to 90°C to remove the methanol generated by the reaction, and keep it for 1 hour. After dealcoholization is completed, the temperature is lowered to 65°C, and 1350 g of a mixture of ethylene oxide and propylene oxide is continuously added, and the weight ratio of ethylene oxide to propylene oxide is 1:1. Control the reaction temperature at 60-70°C, and the pressure in the reactor at -0.02-0.4Mpa. After the addition is complete, keep warm and continue the reaction until the pressure no longer drops. The entire reaction addition time is about 8 hours. After the reaction is completed, use vacuum degassing...

Embodiment 3

[0053] Embodiment 3: experiment with theoretical molecular weight 4000 feed intake

[0054] Add 100 g of allyl alcohol polyether oligomer obtained in Example 1, 2.5 g of sodium methylate in a 2.5 L stirring and stirring and adding 2 external circulation reactors, and use N 2 After replacing the air in the reaction kettle three times, under the vacuum degree ≥ -0.096MPa, start to vacuumize and raise the temperature to 90°C to remove the methanol generated by the reaction, and keep it for 1 hour. After dealcoholization is completed, the temperature is lowered to 65°C, and 1900 g of a mixture of ethylene oxide and propylene oxide is continuously added, and the weight ratio of ethylene oxide to propylene oxide is 3:1. Control the reaction temperature at 65-75°C, and the pressure in the reactor at -0.02-0.4Mpa. After the addition, keep warm and continue the reaction until the pressure no longer drops. The entire reaction addition time is about 10h. After the reaction is completed,...

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Abstract

The invention relates to allyl alcohol polyoxypropylene polyoxyethylene random polyether and a preparation method thereof, belonging to the technical field of preparation of organic high-molecular compounds. The preparation method comprises the following steps: with allyl alcohol, epoxy ethane and epoxy propane as raw materials, adding allyl alcohol and an initial polymerization catalyst into a reaction kettle, replacing air in the reaction kettle with N2, heating to a certain temperature, and adding a mixture of epoxy ethane and epoxy propane to react, so as to synthesize an oligomer; and putting the oligomer and a final polymerization catalyst into a stirring and external circulating reactor, so as to synthesize a product with a molecular weight of 1000-6000. When being used for synthesizing and preparing polyether, the preparation method has the advantages that the byproduct content is low, residual metal ions are few, the molecular weight distribution is narrow, and the like.

Description

technical field [0001] The invention relates to an allyl alcohol polyoxypropylene polyoxyethylene atactic polyether and a preparation method thereof, belonging to the technical field of organic polymer compound preparation. Background technique [0002] Allyl alcohol polyoxypropylene polyoxyethylene random polyether is an unsaturated polyether with an allyl group at one end and a hydroxyl group at the other end. It mainly uses the reaction between the double bond of the polyether in its structure and various active groups. The special properties such as lubricating effect, softening effect, good spreadability and emulsification stability provided by the polyether chain segment are introduced into various new multifunctional fine chemical products. [0003] Allyl alcohol polyoxypropylene polyoxyethylene atactic polyether can carry out hydrosilylation reaction with polysiloxane containing active silicon-hydrogen bonds under the action of a catalyst, and according to the differ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28C08G65/30
CPCC08G65/2609C08G65/2648C08G65/2654C08G65/2696C08G65/30C08G2650/58C08G65/2663
Inventor 金一丰马定连尹红王新荣余江张雨
Owner ZHEJIANG HUANGMA TECH
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