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Polyalkylene oxide catalyst with medium-low molecular weight and preparation method thereof

A technology of polyalkylene oxide and low molecular weight, which is applied in the field of medium and low molecular weight polyalkylene oxide catalyst and its preparation, which can solve the problems of unimproved catalyst, difficult and easy control of molecular weight, increase of production process, etc., and achieve high activity at low temperature , short polymerization time, no aging effect

Active Publication Date: 2012-06-13
上海豪胜化工科技有限公司 +1
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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 goal, which increases the production process, poor product quality, low economy, and is difficult to control the molecular weight.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Preparation of ammonium calcium strontium barium solution

[0027] Under the protection of nitrogen, use liquid nitrogen / ethanol as a cold trap, and collect 250 mL of liquid ammonia in a 500 mL four-neck glass flask at -80°C to -40°C. Under stirring conditions, add 7g of calcium, 3g of strontium, and 8g of barium into the flask, and the reaction will immediately generate an organic ammonium calcium, strontium, and barium solution, and the metal will be completely dissolved within 5 minutes.

[0028] (2) Preparation of catalyst

[0029] Add 0.02g of manganese dioxide, 0.3g of cerium oxide, 0.001g of glyceryl stearate, 0.02g of calcium stearate, and 0.02g of zinc stearate to the ammonium calcium strontium barium solution prepared in (1), and stir Under the conditions, use a constant pressure funnel to slowly add propylene oxide and acetonitrile. The molar ratio of propylene oxide, acetonitrile and metallic calcium is 0.3:0.01:1. After reacting for 1 hour, raise the t...

Embodiment 2

[0031] (1) Preparation of ammonium calcium strontium barium solution

[0032] Under the protection of nitrogen, use liquid nitrogen / ethanol as a cold trap, and collect 250 mL of liquid ammonia in a 500 mL four-neck glass flask at -80°C to -40°C. Under stirring conditions, add 7g of calcium, 1g of strontium, and 4g of barium into the flask, and the reaction will immediately generate an organic ammonium calcium, strontium, and barium solution, and the metal will be completely dissolved within 5 minutes.

[0033] (2) Preparation of catalyst

[0034] Add 0.01g dicobalt trioxide, 0.3g lanthanum oxide, 0.003g glyceryl stearate, 0.01g calcium stearate, 0.04g zinc stearate to the ammonium calcium strontium barium solution prepared in (1), and stir Under certain conditions, use a constant pressure funnel to slowly add propylene oxide and acetonitrile. The molar ratio of propylene oxide to calcium metal is 0.5:1, and the molar ratio of acetonitrile to calcium metal is 0.04:1. After rea...

Embodiment 3

[0036] (1) Preparation of ammonium calcium strontium barium solution

[0037] Under the protection of nitrogen, use liquid nitrogen / ethanol as a cold trap, and collect 250 mL of liquid ammonia in a 500 mL four-neck glass flask at -80°C to -40°C. Under the condition of stirring, add 7g of calcium, 2g of strontium, and 3g of barium into the flask, and the reaction will immediately generate an organic ammonium calcium strontium barium solution, and the metal will be completely dissolved within 5 minutes.

[0038] (2) Preparation of catalyst

[0039] Add 0.01g dicobalt trioxide, 0.1g nickel oxide, 0.3g lanthanum oxide, 0.01g calcium stearate, 0.01g zinc stearate to the ammonium calcium strontium barium solution prepared in (1), under stirring, Slowly add propylene oxide and propionitrile with a constant pressure funnel, the molar ratio of propylene oxide, propionitrile and metallic calcium is 0.5:0.05:1, after reacting for 1 hour, raise the temperature to 25°C, and slowly volatil...

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PUM

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Abstract

The invention relates to a polyalkylene oxide catalyst with medium-low molecular weight and a preparation method thereof. The catalyst is characterized by being an organic compound of metal calcium, metal strontium and metal barium in a weight ratio of 1 to (0.01-1.7) to (0.01-2) and being prepared by making alkaline earth metal with high purity, anhydrous liquid ammonia, an active agent and a dispersant react in a liquid-phase environment. Compared with the prior art, the catalyst prepared by the method has the advantages of a plurality of activity centers, high low-temperature activity, high aggregation efficiency, stable and controllable aggregation process and short aggregation time. The catalyst of the invention is utilized to prepare a polyethylene glycol oxide product with a medium-low molecular weight at a 0.2-1 million stage and can adjust the molecular weight according to a catalyst prescription. The catalyst of the invention has easily obtained raw materials, simple and convenient preparation, low cost and safe transportation and storage without aging.

Description

technical field [0001] The invention relates to a preparation method of a catalyst for alkylene oxide polymerization. More specifically, it refers to a medium and low molecular weight polyalkylene oxide catalyst and a preparation method thereof. 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] Starting from metal oxides and their hydrolyzates that can polymerize ethylene oxide and obtain polymers, a series of catalysts for the ring-opening polymerization of alkylene oxides have been developed successively, including the oxidation of alkaline earth metal elements calcium, strontium, and barium. It is an effe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/02
Inventor 杨维成罗勇陆平晔储根初
Owner 上海豪胜化工科技有限公司
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