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Catalyst for preparing polyethylene oxide and its preparation method and application

A polyoxyethylene and catalyst technology, which is applied to a catalyst for preparing polyoxyethylene and its preparation method and application field, can solve the problems of inability to synthesize polyoxyethylene and high ash content, achieve finer particle size, larger particle size, and increase active sites. point effect

Active Publication Date: 2022-03-18
SHANGHAI RES INST OF CHEM IND +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst mentioned in patent ZL200810203003.X can only prepare polyethylene oxide with a molecular weight of 800,000 to 3 million, and cannot synthesize polyethylene oxide with a lower molecular weight; patent CN 103539931 A reports alkaline earth metal calcium-ammonia-modified catalyst system, the modifier is composed of propylene oxide and acetonitrile, and the suspension catalyst is subjected to aging treatment, but the catalyst is suitable for preparing PEO with a molecular weight between 600,000 and 1.6 million; in the patent CN 108456300 A The catalyst mentioned is capable of producing polyethylene oxide with a molecular weight between 100,000 and 2 million, but the low molecular weight polyethylene oxide produced has an ash content above 1%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Synthesis of catalyst:

[0029] Keep the device in an anhydrous and oxygen-free state, and collect 60g of liquid ammonia in a 2L flask after cooling down to -60°C. Under slow stirring, 2 g of metallic calcium was added to the flask to obtain a blue-black ammonia-calcium complex solution. The modifying agent that 2.90g propylene oxide, 2.88g acetonitrile is formed is dissolved in the mixed solvent (n-hexane and toluene mass ratio is 4:1) that 300g normal hexane and toluene form, then it is added to above-mentioned ammonia calcium complexation In the object, react for 2h; raise the temperature to 0°C to volatilize excess liquid ammonia, and keep it for 1h; raise the reaction temperature to 60°C for aging treatment for 1.5h, and finally get a white slurry catalyst; The suspension was ultrasonically treated at 33KHz for 10 min; finally, 0.13 g of azobisisovaleronitrile was added to the catalyst suspension, and stirred at room temperature for 1 h. The whole reaction sy...

Embodiment 2

[0033] (1) Synthesis of catalyst:

[0034] The mass ratio of azobisisovaleronitrile to metallic calcium was changed to 0.01:1, and other operating procedures were the same as in Example 1.

[0035] (2) Ethylene oxide polymerization reaction:

[0036] The polymerization operation process is identical with the polymerization operation process of embodiment 1. The ash content of the prepared polyethylene oxide product is 0.44%, the viscosity-average molecular weight is 440,000, and the polymerization yield is 99.8%.

Embodiment 3

[0038] (1) Synthesis of catalyst:

[0039] Azobisisovaleronitrile was changed to azobicyclohexylnitrile, the mass ratio of which to calcium metal was 1:1, and other operating procedures were the same as in Example 1.

[0040] (2) Ethylene oxide polymerization reaction:

[0041] The polymerization operation process is identical with the polymerization operation process of embodiment 1. The ash content of the prepared polyethylene oxide product is 0.48%, the viscosity average molecular weight is 400,000, and the polymerization yield is 81.8%.

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Abstract

The present invention relates to a kind of catalyst for preparing polyoxyethylene and its preparation method and application, and this catalyst comprises ammonia calcium catalyst and azo compound, wherein the mass ratio of azo compound and metal calcium in ammonia calcium catalyst is (0.01-10 ):1. The preparation method is to ultrasonically treat the calcium ammonia catalyst at room temperature to obtain a catalyst suspension, then add an azo compound as a molecular chain transfer agent to regulate the molecular weight of polyethylene oxide, and stir the reaction at room temperature for 0.2h Between ~ 3h, the catalyst slurry for preparing low ash and low molecular weight polyethylene oxide is obtained. Compared with the prior art, the catalyst prepared by the present invention has the characteristics of fine particle size and high activity, and the obtained polymer has low ash content and adjustable molecular weight. among polyethylene oxide products.

Description

technical field [0001] The invention relates to the synthesis and application of a catalyst, in particular to a catalyst for preparing polyoxyethylene and its preparation method and application. Background technique [0002] Polyethylene oxide (abbreviated as PEO) is a kind of water-soluble polymer formed by ring-opening polymerization of ethylene oxide. It belongs to "environmentally friendly materials", and its development has been supported by the state. The molecular weight of PEO can vary from 100,000 to 8 million. When the molecular weight is different, it has water retention, lubrication, slow release, thickening, adhesion and other properties. It is widely used in papermaking, medicine, agriculture, daily chemical products, medicine, industry Engineering and many other fields have a wide range of applications. [0003] At room temperature, PEO can self-polymerize slowly, but the efficiency is low. After adding a catalyst, the polymerization efficiency of ethylene ox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/10
Inventor 孔猛徐玄之罗勇储根初刘婷婷柴延军陆平晔
Owner SHANGHAI RES INST OF CHEM IND