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A kind of narrow distribution random polyether and preparation method thereof

A random polyether, narrow-distribution technology, applied in the field of narrow-distribution random polyether and its preparation, can solve the problems of complex process, unsuitable, high cost, etc., and achieve the effect of strong process feasibility, simple process and low cost

Active Publication Date: 2022-02-08
SHANGHAI DONGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the complex manufacturing process of phosphazene, high production cost and large usage, the cost of polyether prepared by using phosphazene as a catalyst is high, which can only be applied to special polyether, not suitable for the preparation of traditional polyether
[0006] All in all, there are following deficiencies in the prior art (1) the molecular weight distribution of polyether is wide in the base-catalyzed one-step method (2) bimetallic catalysts cannot directly use small molecule alcohols as initiators, and are easily poisoned, and the requirements for initiators are high. Polyethers with high EO content cannot obtain a narrow distribution and cannot directly use EO-capped polyethers, etc. (3) The content of phosphazene catalysts is high, the cost is high, and the process is complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] The present embodiment relates to a kind of preparation method of narrow distribution ethylene oxide, propylene oxide random polyether, and its experimental process is as follows:

[0055] A. In the first step, mix 170g of diethylene glycol and 2g of potassium methoxide into the reactor, replace with nitrogen three times and then raise the temperature to 110°C. When the vacuum is EO / M PO =4 / 6), the temperature is controlled at 110-120°C, the pressure is controlled at 0.05-0.2MPa, after PO and EO are fed, the temperature is maintained at 110-120°C, the pressure is controlled at 0.25-0.3 for 60 minutes, and the aging is completed. Around 110°C, vacuum degassing for 30 minutes;

[0056] B. In the second step, first mix 170 g of the low molecular weight polyether obtained in the first step with 3 g of potassium methylate. After nitrogen replacement three times, the temperature was raised to 110° C., and nitrogen was bubbled for vacuum dehydration until the moisture conten...

Embodiment 2

[0058] The present embodiment relates to a kind of preparation method of narrow distribution ethylene oxide, propylene oxide random polyether, and its experimental process is as follows:

[0059] A. In the first step, mix 170g of propylene glycol and 2g of potassium methoxide into the reaction kettle, set the temperature under nitrogen three times and then raise the temperature to 110°C. When the vacuum is EO / M PO =6 / 4), the temperature is controlled at 110-120°C, and the pressure is controlled at 0.05-0.2MPa. After PO and EO are fed, the temperature is maintained at 110-120°C, and the pressure is controlled at 0.25-0.3 for 60 minutes. Around 110°C, vacuum degassing for 30 minutes;

[0060] B. In the second step, first mix 170 g of the low molecular weight polyether obtained in the first step with 3 g of potassium methylate. After nitrogen replacement three times, the temperature was raised to 110° C., and nitrogen was bubbled for vacuum dehydration until the moisture conten...

Embodiment 3

[0062] The present embodiment relates to a kind of preparation method of narrow distribution ethylene oxide, propylene oxide random polyether, and its experimental process is as follows:

[0063] A. In the first step, mix 170g of glycerol and 2g of potassium methoxide into the reaction kettle, replace with nitrogen three times and then raise the temperature to 110°C. When the vacuum is EO / M PO =5 / 5), the temperature is controlled at 110-120°C, and the pressure is controlled at 0.05-0.2MPa. After PO and EO are fed, the temperature is maintained at 110-120°C, and the pressure is controlled at 0.25-0.3 for 60min. Around 110°C, vacuum degassing for 30 minutes;

[0064] B. In the second step, first mix 170 g of the low molecular weight polyether obtained in the first step with 3 g of potassium methylate. After nitrogen replacement three times, the temperature was raised to 110° C., and nitrogen was bubbled for vacuum dehydration until the moisture content was ≤0.05%. Cool down t...

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Abstract

The present application relates to a method for preparing a narrow distribution random polyether, characterized in that the method comprises the following steps: S1: mixing an initiator containing active hydrogen and a first catalyst to obtain a first reaction mixture, and then in an inert Under the atmosphere, at least two kinds of epoxides are simultaneously added to the heated first reaction mixture to obtain a second reaction mixture, and after aging and vacuum degassing, a narrow distribution random polyether intermediate is obtained; S2: mixing the narrow distribution A random polyether intermediate and a second catalyst to obtain a third reaction mixture, and then simultaneously add at least two epoxides to the heated third reaction mixture under an inert atmosphere to obtain a fourth reaction mixture, ripen and vacuum-desorb The narrow distribution random polyether is obtained after gas. The preparation method described in this paper has low cost and simple process, especially the random copolyether with a large proportion of ethylene oxide, and its molecular weight distribution coefficient can be as low as 1.06 or less.

Description

technical field [0001] This application relates to the technical field of polymer synthesis. Specifically, the present application relates to a narrow distribution random polyether and its preparation method. Background technique [0002] Polyether is prepared by polyaddition reaction between an initiator containing active hydrogen and epoxides such as ethylene oxide (EO), propylene oxide (PO), and butylene oxide in the presence of a catalyst. Polyether mostly uses small molecule alcohol as the initiator, and alkali as the catalyst to react with epoxide (usually propylene oxide and ethylene oxide together), by changing the feeding method and amount of propylene oxide and ethylene oxide Ratio, feeding sequence and other conditions, to produce a variety of general-purpose polyether polyols. It can be used as functional additives such as emulsifier, rubber additive, ink additive, wetting agent, defoamer, demulsifier, dispersant and textile additive. [0003] For polyether, m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28
CPCC08G65/2609C08G65/2648
Inventor 方洇岳瑞丽黄斌刘耀强
Owner SHANGHAI DONGDA CHEM