Organic molybdenum complex compound, preparation method and application thereof

A technology of organic molybdenum and complexes, applied in organic molybdenum complexes, the application of the organic molybdenum complexes in the synthesis of polydicyclopentadiene, the preparation field of the organic molybdenum complexes, can solve the synthesis conditions Harsh, difficult to popularize and apply, low cost and other issues, to achieve the effect of low cost, high chemical stability and low price

Inactive Publication Date: 2010-03-03
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The former is easy to prepare, low in cost, and uses alkylaluminum as a cocatalyst, but it is sensitive to air and water vapor, which makes the synthesis

Method used

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  • Organic molybdenum complex compound, preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0037] The organic molybdenum complex of this embodiment is [MoO 2 (NPh 3 ) 2 ]Cl 2 .

[0038] The preparation method of the organomolybdenum complex of the present embodiment is as follows:

[0039] Weigh 6g of molybdic acid (H 2 MoO 4 ), add 21ml of concentrated hydrochloric acid under constant stirring at 50°C, increase the temperature and reflux until clarified, then cool down to 40°C to obtain a hydrochloric acid solution of molybdic acid;

[0040] Weigh 18.15g of triphenylamine, add 181ml of ethanol and stir to dissolve, then slowly add it dropwise into the above-mentioned hydrochloric acid solution of molybdic acid at 40°C under vigorous stirring, a precipitate is formed, and then continue to stir for 6 hours, and then filter the precipitate with suction The cake was washed three times with acetone and then three times with ether, and the washed filter cake was vacuum-dried at 50° C. for 8 hours to obtain 17.4 g of organic molybdenum complex.

Embodiment 2

[0042] The organic molybdenum complex of the present embodiment is {MoO 2 [N(PhC 4 h 9 ) 3 ] 2} Cl 2 .

[0043] The preparation method of the organomolybdenum complex of the present embodiment is as follows:

[0044] Weigh 6g of molybdic acid (H 2 MoO 4 ), add 21ml of concentrated hydrochloric acid under constant stirring at 40°C, increase the temperature and reflux until clarified, then cool down to 40°C to obtain a hydrochloric acid solution of molybdic acid;

[0045] Weigh 24.6g of tris(4-n-butylphenyl)amine, add 126ml of ethanol and stir to dissolve, then slowly add dropwise to the above-mentioned hydrochloric acid solution of molybdic acid at 40°C under vigorous stirring, a precipitate is formed, and then continue to stir for 6 After the precipitate was suction filtered, the filter cake was washed three times with acetone and then three times with ether, and the washed filter cake was vacuum-dried at 60° C. for 8 hours to obtain 23.3 g of an organic molybdenum com...

Embodiment 3

[0047] The organic molybdenum complex of this embodiment is [MoO 2 (PPh 3 ) 2 ]Cl 2 .

[0048] The preparation method of the organomolybdenum complex of the present embodiment is as follows:

[0049] Weigh 6g of molybdic acid (H 2 MoO 4 ), add 21ml of concentrated hydrochloric acid under constant stirring at 80°C, increase the temperature and reflux until clarified, then cool down to 40°C to obtain a hydrochloric acid solution of molybdic acid;

[0050] Weigh 19.43g of triphenylphosphine, add 65ml of ethanol and stir to dissolve, then slowly add dropwise to the above-mentioned hydrochloric acid solution of molybdic acid at 40°C under vigorous stirring, a precipitate is formed, and then continue to stir for 5 hours, and then filter the precipitate with suction The cake was washed three times with acetone and then three times with ether, and the washed filter cake was vacuum-dried at 80° C. for 8 hours to obtain 22.1 g of organic molybdenum complex.

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Abstract

The invention discloses an organic molybdenum complex compound; organic ligand containing nitrogen group elements can be adopted to be matched with molybdenum to form metal organic compound, wherein the organic ligand includes triphenyl phosphine or alkyl-substituted derivative of the triphenyl phosphine, triphenyl phosphine oxide or alkyl-substituted derivative of the triphenyl phosphine oxide, triphenyl amine or alkyl-substituted derivative of the triphenyl amine, triphenyl amine oxide or alkyl-substituted derivative of the triphenyl amine oxide, triphenyl arsine or alkyl-substituted derivative of the triphenyl arsine, and triphenyl arsine oxide or alkyl-substituted derivative of the triphenyl arsine oxide. Meanwhile, the invention further discloses a preparation method of the organic molybdenum complex compound and the application of taking the organic molybdenum complex compound as catalyst in synthesizing poly-dicyclo-pentadiene. The organic molybdenum complex compound has higherchemical stability, is not sensitive for air and water vapor, can be taken as the catalyst to be applied in synthesizing the poly-dicyclo-pentadiene with higher catalytic activity, reduces the reaction conditions required by synthesizing the poly-dicyclo-pentadiene due to the chemical stability, and has good popularization and application prospects.

Description

technical field [0001] The present invention relates to a kind of metal organic compound, especially a kind of organic molybdenum complex, relate to a kind of preparation method of this organic molybdenum complex at the same time, also relate to a kind of this organic molybdenum complex in synthesizing polydicyclopentadiene in the application. Background technique [0002] Dicyclopentadiene (DCPD) can be polymerized by ring-opening metathesis to obtain a cross-linked thermosetting polydicyclopentadiene (PDCPD) plastic. The plastic has good heat resistance, creep resistance, dimensional stability, corrosion resistance and other properties. The production of PDCPD adopts the reaction injection molding (RIM) process, which has the advantages of fast molding speed, low processing temperature, and low injection pressure. It can be used to manufacture various thin-walled large parts with high performance and complex shapes, such as transportation. Automobile bumpers, guard plate...

Claims

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Application Information

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IPC IPC(8): C07F11/00C08F4/622C08F132/08
Inventor 张玉清郝银鸽李俊贤姜通武赫玉欣姚大虎徐华严一楠
Owner HENAN UNIV OF SCI & TECH
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