Catalyst capable of regulating and controlling molecular weight of ethylene oxide and preparation method thereof

A polyethylene oxide and catalyst technology, applied in the field of medium and low molecular weight polyethylene oxide, can solve the problems of poor catalytic stability, complex process, high equipment requirements, etc., and achieve the effect of stable polymerization yield

Inactive Publication Date: 2018-08-28
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 U.S. patent (US2006036066) mentions the blending of organoaluminum compounds and alkali metal oxides or hydroxides, and the obtained catalyst can prepare polyethylene oxide with a molecular weight of 20,000 to 200,000. However, the process is complicated and involves high-pressure operation. high equipment requirements
Chinese patent (CN 1306023A) is a catalyst synthesized by dissolving metal calcium in liquid ammonia, adding modifiers and aluminum oxide and other carriers. The catalyst has the characteristics of low temperature, high activity and high yield. The prepared polyoxygen The molecular weight of ethylene reaches 8 million, which is not suitable for the preparation of low molecular weight PEO products
But the catalytic stability of the catalyst mentio

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Synthesis of catalyst:

[0022] Under the protection of high-purity argon, collect 150ml-200ml of liquid ammonia in a 2000ml four-necked flask at -60°C. Under magnetic stirring, add 2g Ca in the flask, obtain ammoniacal calcium complex after reacting 1h; 2.90g propylene oxide and 1.220g azobicyclohexyl nitrile composition modifying agent are dissolved in 300ml n-hexane, then It is added to the above-mentioned ammonia-calcium complex and reacted for 1 hour; heated to raise the reaction temperature to 0°C to volatilize excess liquid ammonia; finally, raise the reaction temperature to 60°C for aging treatment for 1 hour to obtain a white slurry Catalyst. The whole reaction system was carried out under the protection state of high-purity argon.

[0023] (2) Ethylene oxide polymerization reaction:

[0024] The above-mentioned slurry catalyst was added to a well-sealed 2L reaction kettle filled with argon with mechanical stirring, and then 300ml of n-hexane and 200g of...

Embodiment 2

[0026] (1) Synthesis of catalyst:

[0027] The amount of azobicyclohexanenitrile was changed to 0.630g, and other operating procedures were the same as in Example 1.

[0028] (2) Ethylene oxide polymerization reaction:

[0029] The polymerization operation process is identical with the polymerization operation process of embodiment 1. The viscosity-average molecular weight of the prepared polyethylene oxide is 250,000, and the polymerization yield is 99.8%.

Embodiment 3

[0031] (1) Synthesis of catalyst:

[0032] The modifying agent is a mixed solution of azobisisobutyronitrile and propylene oxide, and the amount of azobisisobutyronitrile is 0.835 g. Other operating procedures are the same as in Example 1.

[0033] (2) Ethylene oxide polymerization reaction:

[0034] The polymerization operation process is identical with the polymerization operation process of embodiment 1. The viscosity-average molecular weight of the prepared polyethylene oxide is 440,000, and the polymerization yield is 99.9%.

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PUM

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Abstract

The invention relates to a catalyst capable of regulating and controlling the molecular weight of ethylene oxide and a preparation method thereof. The preparation method of the catalyst includes the steps that liquid ammonia reacts with calcium metal for 0.5-4 h at low temperatures of minus 80 DEG C to minus 10 DEG C to generate an ammonia-calcium complex solution, after a modifying agent composedof propylene oxide and azo compounds is added into solvent, reaction continues for 0.5-4 h, and through heating deamination and aging, the catalyst is obtained. Compared with the prior art, the prepared catalyst has the advantages of being high in activity and stability and capable of adjusting the molecular weight of polymers, and during the ring opening polymerization reaction of ethylene oxide(EO), polyoxyethylene series products of which the molecular weights are 100 thousand to 200 million can be prepared.

Description

technical field [0001] The invention relates to a catalyst, in particular to a method for preparing a catalyst for catalyzing the ring-opening polymerization of ethylene oxide to generate polyethylene oxide, which can synthesize a series of polyethylene oxide with a molecular weight of 100,000 to 2 million. Background technique [0002] Polyethylene oxide (PEO) is a linear polymer formed by heterogeneously catalyzed ring-opening polymerization of ethylene oxide. It is a crystalline, thermoplastic, and water-soluble polymer with low chemical toxicity. Depending on the degree of polymerization, the molecular weight of polyethylene oxide can vary from 100,000 to 8 million. In addition to the above properties, PEO also has a series of other excellent properties at different molecular weights, and can act as a dispersant, flocculant, thickener, hydraulic drag reducer, etc. It is widely used in many fields such as medicine and industrial engineering. In recent years, with the in...

Claims

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Application Information

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IPC IPC(8): C08G65/10C08G65/12
CPCC08G65/10C08G65/12
Inventor 李从严孔猛罗勇刘婷婷储根初陆平晔徐玄之
Owner SHANGHAI RES INST OF CHEM IND
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