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Nano composite quaternary phosphonium salt resin

A nano-composite, quaternary phosphonium salt technology, applied in the direction of organic compound/hydride/coordination complex catalysts, organic chemistry, physical/chemical process catalysts, etc., can solve the problem of rapid activity decline, low catalyst activity, easy resin swelling, etc. problem, to achieve the effect of good technical effect

Active Publication Date: 2013-05-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is that in the prior art, the catalyst activity is low, the resin is easy to swell, and the activity declines quickly. A new nanocomposite quaternary phosphonium salt resin is provided.

Method used

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  • Nano composite quaternary phosphonium salt resin
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 58.0 grams of styrene, 0.6 grams of divinylbenzene, 30 grams of polystyrene and 0.6 grams of benzoyl peroxide initiator in a 500 milliliter three-necked flask, and stir for 2.0 hours at 60°C; then add 2.8 grams of multi-walled carbon Nanotubes, continue stirring for 1 hour for pre-polymerization. 260 mL of deionized water in which 2.5 g of polyvinyl alcohol had been dissolved was added. Adjust the stirring speed while gradually raising the temperature to 80°C and react for 5 hours; then raise the temperature to 90°C and react for 5 hours; finally raise the temperature to 98°C and react for 6 hours. After the reaction, pour out the upper liquid, wash with 85°C hot water, then wash with cold water, then filter, put in an oven to dry at 80°C, sieve, and collect composite microspheres with a particle size within the range of 0.35 to 0.60 mm a.

[0023] Chloromethylation of composite microspheres: In a 500-ml three-necked flask, add 50 grams of composite microspheres A...

Embodiment 2

[0026] In a 500 ml three-necked flask, add 20 grams of the composite chlorine ball A obtained in [Example 1], 150 milliliters of benzonitrile, 35.0 grams of dimethylphenylphosphine and 10.0 grams of nickel bromide, and stir and react under reflux for 30 hours After the reaction, the mother liquor was removed by filtration, washed with dichloromethane, acetone and water successively, and dried under vacuum to obtain the nanocomposite quaternary phosphonium salt resin A2.

Embodiment 3

[0028] Add monomer mixture solution (60.0 gram styrene, 1.7 gram divinylbenzene, 60 gram polystyrene, 1.6 gram multi-walled carbon nanotube and 1.0 gram benzoyl peroxide containing initiator in 500 milliliters of three-necked flasks, The solution was first stirred and reacted at 70°C for 0.5 hours), started the agitator, added a mixed solution of 200 milliliters of deionized water and 5 grams of gelatin, raised the temperature to 85°C, reacted for 3 hours, then raised the temperature to 90°C, reacted for 9 hours, and finally The temperature was raised to 100° C., and the reaction was carried out for 10 hours. After the reaction, pour out the upper liquid, wash with 85°C hot water, then wash with cold water, then filter, put in an oven to dry at 80°C, sieve, and collect composite microspheres with a particle size within the range of 0.35 to 0.60 mm b.

[0029] Chloromethylation of composite microspheres: In a 500-ml three-necked flask, add 50 grams of composite microspheres B ...

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Abstract

The invention relates to a nano-composite quaternary phosphonium salt resin, which mainly solves the problems that in the prior art, catalyst activity is low, resin is easy to swollen, and the activity of the resin is rapidly reduced. A preparation method of the nano composite quaternary phosphonium salt resin comprises the following steps: (1) preparing an aiding agent I into an aqueous solution A; (2) preparing a monomer, a comonomer and a nano material, an initiating agent and an aiding agent II into a solution B; (3) mixing the solution B with the solution A and reacting, thereby obtaining a composite microsphere; (4) adding a chloromethylation reagent and zinc chloride into the composite microsphere, thereby obtaining a composite chlorine sphere; and (5) adding a quaternary phosphorization reagent into the composite chlorine sphere and reacting, thereby obtaining the nano composite quaternary phosphonium salt resin. According to the adopted technical scheme, the problem is solved well. The nano composite quaternary phosphonium salt resin can be applied to the industrial production of alkyl carbonate.

Description

technical field [0001] The invention relates to a nanocomposite quaternary phosphonium salt resin. Background technique [0002] Alkylene carbonates such as ethylene carbonate and propylene carbonate are organic chemical raw materials with a wide range of uses and are widely used as solvents and diluents in industry. Ethylene carbonate can be used as a solvent in textiles, printing, polymer synthesis and electrochemistry, as well as a raw material for cosmetics and medicines and an intermediate for corresponding diols. [0003] Industrially, alkylene carbonate is generally prepared by reacting carbon dioxide with the corresponding alkylene oxide under the action of a catalyst. Many catalysts have been found to have a catalytic effect on this reaction, such as transition metal complexes, main group element complexes, quaternary ammonium salts, quaternary phosphonium salts and alkali metal salts, ionic liquids, supercritical carbon dioxide and other catalytic systems. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F212/36C08F2/44C08F8/40C08F8/24B01J31/28C07D317/38C07D317/36
Inventor 俞峰萍何文军
Owner CHINA PETROLEUM & CHEM CORP
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