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Organophosphorus based tungsten complex and preparation method and application thereof

A tungsten complex and organic phosphine technology, applied in the field of polymer synthesis, can solve the problems of being unsuitable for industrial production, harsh use conditions, poor stability, etc., and achieve the effects of good promotion and application prospects, low preparation cost, and low price.

Active Publication Date: 2010-03-03
NORTH HUAJIN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalysts used in the current RIM process are mainly aryloxytungsten complexes and ruthenium and osmium carbene catalysts. When the former is used, alkylaluminum is required as a cocatalyst to effectively polymerize dicyclopentadiene (DCPD). It belongs to the two-component complex catalytic system, but it is sensitive to air and water vapor, has poor stability, and has relatively harsh service conditions; the chemical properties of the latter are relatively stable, but the price is relatively high, and it is not suitable for industrial production

Method used

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  • Organophosphorus based tungsten complex and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The structural formula of the organophosphine-based tungsten complex in this embodiment is as follows: [W(OPPh 3 ) 2 ]Cl 6 .

[0032] The preparation method of the organophosphine-based tungsten complex of this embodiment is as follows:

[0033] 1. Take 10g of sodium tungstate hydrate (Na 2 WO 4 ·2H 2 O) In an Erlenmeyer flask, slowly add distilled water at 50℃ and keep stirring until it just dissolves. Under continuous stirring, slowly add concentrated hydrochloric acid until no more yellow precipitate is formed. Add 2ml of concentrated hydrochloric acid, and then continue. Reacted for 8 hours; the precipitate was filtered and washed repeatedly with a large amount of distilled water until the pH value was neutral, and the obtained solid was vacuum dried at 50°C for 4 hours to obtain yellow tungstic acid (H 2 WO 4 ) 6.8g solid powder;

[0034] 2. Weigh 6g of the solid tungstic acid powder obtained in step 1, add 150 mL of concentrated hydrochloric acid under continuous stirrin...

Embodiment 2

[0037] The structural formula of the organophosphine-based tungsten complex in this embodiment is as follows: [W(PPh 3 ) 2 ]Cl 6 .

[0038] The preparation method of the organophosphine-based tungsten complex of this embodiment is as follows:

[0039] 1. Take 12g of hydrated sodium tungstate (Na 2 WO 4 ·2H 2 O) In an Erlenmeyer flask, slowly add distilled water at 60℃ and keep stirring until it just dissolves. Under continuous stirring, slowly add concentrated hydrochloric acid until no more yellow precipitate is formed. Add 2ml of concentrated hydrochloric acid, and then continue. Reacted for 9 hours; the precipitate was filtered and washed repeatedly with distilled water until the pH was neutral. The solid obtained was vacuum dried at 50°C for 4 hours to obtain yellow tungstic acid (H 2 WO 4 ) 8.28g of solid powder.

[0040] 2. Weigh 8 g of the solid tungstic acid powder obtained in step 1, add 160 mL of concentrated hydrochloric acid under continuous stirring, raise the temperatur...

Embodiment 3

[0043] The structural formula of the organophosphine-based tungsten complex in this embodiment is as follows: {W[P(PhC 3 H 7 ) 3 ] 2 }Cl 6 .

[0044] The preparation method of the organophosphine-based tungsten complex of this embodiment is as follows:

[0045] 1. Take 15g of hydrated sodium tungstate (Na 2 WO 4 ·2H 2 O) In an Erlenmeyer flask, slowly add distilled water at 70℃ and keep stirring until it just dissolves. Under continuous stirring, slowly add concentrated hydrochloric acid until no more yellow precipitate is formed. Add 2ml of concentrated hydrochloric acid, and then continue. Reacted for 10 hours; the precipitate was filtered and washed repeatedly with distilled water until the pH value was neutral. The resulting solid was vacuum dried at 50°C for 4 hours to obtain yellow tungstic acid (H 2 WO 4 ) 11g of solid powder.

[0046] 2. Weigh 10g of the solid powder of tungstic acid obtained in step 1, add 158.33mL of concentrated hydrochloric acid under stirring, raise the ...

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Abstract

The invention discloses an organophosphorus based tungsten complex which is bidentate chloride of triphenylphosphine or triphenylphosphine oxide of tungsten. Phenyl in the triphenylphosphine or triphenylphosphine oxide may be alkyl substituted phenyl and the number of the alkyl substituents can be 1-3. The invention also discloses a preparation method of the organophosphorus based tungsten complex and application of the organophosphorus based tungsten complex in synthesizing polydicyclopentadiene. Under the action of organophosphorus ligands, the tungsten complex of the invention has higher catalytic activity in synthesizing polydicyclopentadiene, has high chemical stability and is insensitive to air and water vapors, thus lowering the reaction conditions for synthesizing polydicyclopentadiene. In addition, the raw materials adopted by the organophosphorus based tungsten complex prepared by the invention are low in price and the preparation method is simple; therefore, the tungsten complex is low in preparation cost and has good popularization and application prospect.

Description

Technical field [0001] The present invention relates to an organic phosphine-based tungsten complex, a preparation method of the complex, and an application of the complex in the synthesis of polydicyclopentadiene, belonging to polymer synthesis technology field. Background technique [0002] Polydicyclopentadiene (PDCPD) is an engineering plastic with high impact strength and high flexural modulus. The plastic also has good heat resistance, creep resistance, dimensional stability, and corrosion resistance. It can be used to manufacture various high-performance thin-walled large-scale parts with complex shapes, such as: automobile bumpers, guard plates, side panels, engine hoods and body shells in the transportation industry; motors in electrical equipment , Air conditioners and other large electrical equipment shells; sports equipment such as sleds, surfboards, golf carts and other components, agricultural machinery, civil construction materials, etc. The United States, Japan,...

Claims

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Application Information

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IPC IPC(8): C07F11/00C08F4/622C08F132/08
Inventor 张玉清姜通武郝银鸽陆昶姚大虎赫玉欣高喜平徐华严一楠
Owner NORTH HUAJIN CHEM IND CO LTD
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