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Organic phosphonium molybdenum complex, preparation method and application

A technology of organic phosphine and complexes, applied in the field of preparation of organic phosphine-molybdenum complexes, can solve the problems of not being able to meet high-efficiency production, insolubility, and low catalytic efficiency, and achieve suitable for large-scale industrial production, low cost, and high catalytic efficiency high effect

Active Publication Date: 2015-11-18
张玉清
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this type of compound cannot be dissolved in dicyclopentadiene monomer, and the heterogeneous system formed during catalysis makes the catalytic efficiency low and cannot meet the requirements of high-efficiency production

Method used

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  • Organic phosphonium molybdenum complex, preparation method and application
  • Organic phosphonium molybdenum complex, preparation method and application
  • Organic phosphonium molybdenum complex, preparation method and application

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Embodiment 1

[0042] The organophosphine molybdenum complex of this embodiment is a propyl diphenylphosphine molybdenum complex, which has the following molecular formula:

[0043] Mo[P(Ph) 2 CH 2 CH 2 CH 3 ] 2 Cl 5 Formula I-1;

[0044] In Formula I-1, P(Ph) 2 CH 2 CH 2 CH 3 For propyl diphenyl phosphine.

[0045]The preparation method of the organophosphine-molybdenum complex of this embodiment is to add 273.2g (1mol) of molybdenum pentachloride into 500ml of dry chloroform under nitrogen protection, stirring and 30°C, and wait until the molybdenum pentachloride is completely dissolved. Finally, the chloroform solution of molybdenum pentachloride is obtained; the chloroform solution of the propyl diphenylphosphine that is dissolved in 456.38g (2mol) is added dropwise in the chloroform solution of molybdenum pentachloride, 30 ℃ of insulation reaction 5h, obtain the concentration of 1mol / L chloroform solution of propyl diphenylphosphine molybdenum complex.

[0046] The chlorofor...

Embodiment 2

[0052] The organophosphine-molybdenum complex of this embodiment is a hexyldiphenylphosphine-molybdenum complex, which has the following molecular formula:

[0053] Mo[P(Ph) 2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 3 ] 2 Cl 5 Formula I-2;

[0054] In formula I-2, P(Ph) 2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 3 For hexyl diphenyl phosphine.

[0055] The preparation method of the organophosphine-molybdenum complex of the present embodiment is to add 218.56 g (0.8 mol) of molybdenum pentachloride into 500 ml of dry toluene under nitrogen protection, stirring and 50° C., and wait until the molybdenum pentachloride is completely After dissolving, the toluene solution of molybdenum pentachloride was obtained; the toluene solution dissolved with 432.3g (1.6mol) of hexyldiphenylphosphine was added dropwise to the toluene solution of molybdenum pentachloride, and the temperature was kept at 50°C for 4h to obtain the concentration It is a toluene solution of 0.8mol / L hexyl diphenylphosphine...

Embodiment 3

[0062] The organophosphine-molybdenum complex of this embodiment is an octyldiphenylphosphine-molybdenum complex, which has the following molecular formula:

[0063] Mo[P(Ph) 2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 3 ] 2 Cl 5 Formula I-3;

[0064] In formula I-3, P(Ph) 2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 2 CH 3 For octyl diphenyl phosphine.

[0065] The preparation method of the organophosphine-molybdenum complex of the present embodiment is to add 136.6 g (0.5 mol) of molybdenum pentachloride into 500 ml of dry ethylbenzene under nitrogen protection, stirring and 60° C. After molybdenum was completely dissolved, the ethylbenzene solution of molybdenum pentachloride was obtained; the ethylbenzene solution of octyldiphenylphosphine that was dissolved in 298.19g (1mol) was added dropwise in the ethylbenzene solution of molybdenum pentachloride, The reaction was carried out at 60°C for 3 hours to obtain an ethylbenzene solution of octyl diphenylphosphine molyb...

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Abstract

The invention discloses an organic phosphonium molybdenum complex, a preparation method and application. The organic phosphonium molybdenum complex has the following general formula: Mo[P(Ph)2R]2Cl5, wherein the P(Ph)2R is alkyldiphenylphosphine; the R is linear-chain alkyl with the carbon atom number of 3-10. According to the organic phosphonium molybdenum complex provided by the invention, alkyldiphenylphosphine is adopted as the ligand, and the organic phosphonium molybdenum complex can be dissolved in dicyclopentadiene, and can form a homogeneous system with dicyclopentadiene when used as a main catalyst to catalyze dicyclopentadiene for ring opening polymerization, so that the catalytic efficiency is greatly improved, and the production efficiency of polydicyclopentadiene is improved; the organic phosphonium molybdenum complex is relatively high in catalytic activity, and the polydicyclopentadiene product prepared through adopting the organic phosphonium molybdenum complex as the main catalyst is high in quality and excellent in the mechanical properties, such as, tensile strength and impact strength; the organic phosphonium molybdenum complex is relatively high in chemical stability, insensitive to air and moisture, simple in preparation, low in cost and suitable for popularization and application.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and specifically relates to an organic phosphine-molybdenum complex, and also relates to a preparation method of the organic phosphine-molybdenum complex and the application of the above-mentioned organic phosphine-molybdenum complex in catalyzing the ring-opening polymerization of dicyclopentadiene . Background technique [0002] Polydicyclopentadiene (PDCPD) is a thermosetting engineering plastic with a three-dimensional network structure obtained by ring-opening metathesis catalyst and reaction injection molding process. It is a homopolymer or copolymer of dicyclopentadiene (DCPD). Its good comprehensive mechanical properties and high-efficiency and energy-saving process characteristics can be used to manufacture various thin-walled large-scale parts with high performance and complex shapes, and are widely used in transportation, machinery manufacturing, chemical industry, civil engi...

Claims

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Application Information

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IPC IPC(8): C07F11/00C08F132/08C08F4/69
Inventor 张玉清
Owner 张玉清
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