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Method for preparing composite catalyst applied to alkylene oxide ring-expansion polymerization and use

A technology for polymerization catalysts and alkylene oxides, which is applied in the field of preparation of alkylene oxide ring-opening polymerization catalysts, can solve the problems of unimproved catalysts, increased production processes, increased production costs, etc., and achieve excellent product properties, broaden the scope of application, The effect of inhibiting caking

Active Publication Date: 2009-03-25
SHANGHAI RES INST OF CHEM IND +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN1611523A introduces that during the polymer synthesis process, a compound with active hydrogen is added as a molecular weight regulator to prepare medium and low molecular weight polyethylene oxide, but this method is completed in the polymerization process and has not been improved on the catalyst
U.S. Patent U.S.4200704 describes the purpose of preparing medium and low molecular weight polyethylene oxide by decomposing high molecular weight polyethylene oxide with peroxide in the presence of oxygen, but the process is complicated and the production cost increases
The preparation methods of medium and low molecular weight alkylene oxide polymers involved in the above patents all use secondary processing to achieve the purpose, which increases the production process, poor product quality, and low economic efficiency.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation of Ammonium Calcium Strontium Solution

[0025] Under the protection of nitrogen, use dry ice / ethanol as a cold trap, and collect 250ml of liquid ammonia in a 500ml four-neck glass flask at -70°C to -33.5°C. Under stirring conditions, add 7g of calcium and 3g of strontium into the flask, and the reaction will immediately generate a blue organic ammonium calcium-strontium solution, and the metal will be completely dissolved within 5 minutes.

[0026] (2) Preparation of calcium strontium ammonia / propylene oxide catalyst

[0027] Slowly add propylene oxide to the calcium strontium ammonia solution prepared in step (1) with constant pressure funnel under stirring. The molar ratio of propylene oxide to bimetal is 1:1. After reacting for 1 hour, heat up to 25°C , Slowly volatilize the ammonia gas, during this process, add 200ml No. 90 solvent oil for slurry treatment, until the excess ammonia gas is completely volatilized and removed, that is, the catalyst ca...

Embodiment 2

[0031] According to the method of step (1) of Example 1, calcium strontium ammonia solution was prepared. Under constant stirring, propylene oxide was slowly added. The molar ratio of propylene oxide to metal was 1:1. After reacting for 0.5 hours, slowly Add acetonitrile, the molar ratio of acetonitrile to bimetal is 0.5:1, continue to react for 1 hour, heat up to volatilize excess liquid ammonia, and add 200ml90 solvent oil for slurry treatment during this process, until excess ammonia gas is completely volatilized and removed, That is, the catalyst cat-2 is prepared for the polymerization of ethylene oxide.

[0032] By the method of embodiment 1 step (3), 0.08g catalyst cat-2, No. 2L solvent oil and ethylene oxide 800g were added respectively in the 10L polymerization kettle that had been purged by nitrogen to carry out polymerization reaction, and the polymerization time was 22 hours. The polymerized product was separated and vacuum dried to obtain 620 g of polyethylene oxi...

Embodiment 3

[0034] According to the step (1) of Example 1, calcium strontium ammonia solution was prepared. Under constant stirring, slowly add the mixture of propylene oxide and acetonitrile. The molar ratio of propylene oxide and metal was 1:1, and The molar ratio is 0.5:1. After reacting for 2 hours, heat up to volatilize excess liquid ammonia, and add 200ml No. 90 solvent oil for slurry treatment during the process, until the excess ammonia gas is completely volatilized and removed, the catalyst cat-3 is prepared For the polymerization of ethylene oxide.

[0035] According to the method of embodiment 1 step (3), 24g catalyst cat-3, 2L No. 90 solvent oil and 800g of ethylene oxide are added respectively in the 10L polymerization kettle that has been purged by nitrogen to carry out polymerization reaction, polymerization time 24 hours, separate The polymerization product was vacuum-dried to obtain 720 g of polyethylene oxide with a yield of 90% and a molecular weight of 335,000.

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PUM

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Abstract

The invention relates to a method for preparing an alkylene oxide ring-opening polymerization catalyst, and the application thereof. The method comprises steps as follows: under the protection of inertia gas, the temperature is controlled to be minus 70 DEG C to minus 33.5 DEG C; two metals of high-purity alkali soil calcium metal and strontium metal with the mol ratio of 1:0.1 to 1:1.5 are dissolved in liquid ammonia; the mol ratio betwen the liquid ammonia and the metals is 50:1 to 100:1; the reaction lasts for 30min to 90min so as to form an organic ammonia calcium and strontium solution; then the alkylene oxide is added and the mol ratio between the alkylene oxide and the two metals is 0.5:1 to 1.5:1; or two compounds, nitrile and the alkylene oxide with the mol ratio of 0.1:1 to 0.8:1 are added, the mol ratio between the nitrile and the two metals is 0.1:1 to 0.8:1; and the reaction lasts for 60min to 120min; the temperature is raised to normal so as to volatilize the residual liquid ammonia in the reaction product; meanwhile, a dissolvent is added and slurrying is carried out to obtain the catalyzed product. Compared with the prior art, the invention is characterized by simple method, high economic benefit, excellent product properties, and the like.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a preparation method and application of an alkylene oxide ring-opening polymerization catalyst. Background technique [0002] Alkylene oxide polymer is a water-soluble polymer with excellent coagulation, dispersion and thickening effects. Because of these excellent effects, alkylene oxide polymers are widely used in pulp dispersants, resin modifiers, binders, coagulants, detergents, food, personal care products, sanitary materials, cosmetics, medical supplies and quasi- in the field of pharmaceuticals. [0003] Alkylene oxide can be polymerized by various polymerization catalysts such as alkali, boron trifluoride, alkaline earth metal oxides and organic metal compounds to form polymers. The polymerization degree and reaction speed of the alkylene oxide polymerization reaction are determined by the type of catalyst used. For example, when the products obtained by the action of alkaline ...

Claims

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Application Information

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IPC IPC(8): C08G65/12
Inventor 姜晓东罗勇陆平晔宋家龙
Owner SHANGHAI RES INST OF CHEM IND