2-hydroxy benzophenone titanium catalyst for synthesizing syndiotactic polystyrene and its preparing method

The technology of hydroxybenzophenone and polystyrene is applied in the field of non-locene catalyst and its preparation, which can solve the problems of low molecular weight of polymers, and achieve the effects of low production cost, optimized application performance and cheap raw materials

Inactive Publication Date: 2005-07-06
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For the problems referred to above, the present invention also overcomes existing non-metallocene catalysts while overcoming the problems of metallocene catalysts, that is, when the complexes of beta-diketone titanium and 8-hydroxyquinoline titanium carry out styrene syndiotactic polymerization, The relatively low molecular weight problem of the polymer; a catalyst of titanium 2-hydroxybenzophenone is provided; that is, utilizing its unique ligand structure (the electronic effect of the ligand, the larger steric hindrance can stabilize the active center), The molecular weight of the polymer obtained by catalysis is significantly increased; thereby optimizing the application performance of the polymer

Method used

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  • 2-hydroxy benzophenone titanium catalyst for synthesizing syndiotactic polystyrene and its preparing method
  • 2-hydroxy benzophenone titanium catalyst for synthesizing syndiotactic polystyrene and its preparing method

Examples

Experimental program
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Effect test

Embodiment 1-10

[0024] Example 1-10: Synthesis of the structure, components and related properties of the catalyst of the present invention, see Table 1 for details.

[0025] Synthesize structure, component and related performance of catalyst of the present invention Table 1

[0026] Implementation R R R main catalyst Al / Ti T activity (×10 5 gPS Syndiotacticity T m m w (×

[0027] Example (°C) / molTi·h) % (°C) 10 4 )

[0028] 1 - CH 3 CH 3 A 2 Ti(OPh) 2 1100 20 0.5 96 265 16

[0029] 2CH 3 C 2 h 5 -ATiCl 3 500 80 8.3 93 270 23

[0030] 3C 3 h 7 -CH 3 A 3TiCl 2000 80 0.9 94 275 18

[0031] 4CH 3 C 3 h 7 C 2 h 5 ATi(OPh) 3 700 40 7.1 98 269 17

[0032] 5CH 3 O C 4 h 9 C 3 h 7 A 2 TiCl 2 600 90 4.8 95 267 29

[0033] 6C 4 h 9 O CH 3 CH 3 ATi(OEt) 3 800 60 6.4 94 266 30

[0034] 7-C 2 h 5 C 3 h 7 ATi(OPhOMe) 3 400 80 3.2 96 270 24 ...

Embodiment 1

[0040] N at room temperature 2 Among them, 0.42 g of ligand A of the structure shown in Table 1, that is, 2-hydroxybenzophenone 0.42 g, was dissolved in ether and added to the 4 Carry out complex coordination in the diethyl ether solution, then heat up to the solvent reflux temperature, reflux for 6 hours, filter and wash the precipitate, and vacuum dry to obtain the main catalyst A 2 Ti(OPh) 2 0.51g. In a 100ml two-necked flask replaced by nitrogen and equipped with a stirrer, add 15ml of toluene distilled by reflux of metal sodium, stir and raise the temperature to 20°C, add the main catalyst A 2 Ti(OPh) 2 .0.47mg (the concentration is 1.53×10 -5 mol / L), according to the molar ratio of cocatalyst and main catalyst, namely Al / Ti=1100 plus cocatalyst triisobutylaluminoxane 6.8ml, add 20ml of dried styrene. After 1 h of reaction, 10% acidified ethanol solution was added to terminate the reaction. The reactant was continuously stirred in excess ethanol for 2 h, filtered an...

Embodiment 2

[0042] N at room temperature 2 Dissolve 0.49 g of ligand A, that is, 2-hydroxybenzophenone with the structure shown in Table 1, in ether and add it to a solution containing 1.7 ml of TiCl 4 Carry out complexation and coordination in the diethyl ether solution, then raise the temperature to the solvent reflux temperature, reflux for 6 hours, filter and wash the precipitate, and vacuum dry to obtain the main catalyst ATiCl 3 0.36g. In a 100ml two-necked flask replaced by nitrogen and equipped with a stirrer, add 15ml of toluene distilled by reflux of metal sodium, heat up to 80°C under stirring, add the main catalyst ATiCl 3 20.6mg (concentration is 1×10 -3 mol / L), the cocatalyst is methylaluminoxane (MAO). According to the molar ratio of co-catalyst and main catalyst, ie Al / Ti=500, add 3.7 ml of co-catalyst and 20 ml of dried styrene. After 1 h of reaction, 10% acidified ethanol solution was added to terminate the reaction. The reactant was continuously stirred in excess ...

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Abstract

The invention discloses a 2-hydroxybenzophenone titanium catalyst for synthesizing syndiotactic polystyrene and a preparation method thereof, belonging to non-cene catalysts for synthesizing syndiotactic polystyrene. It solves the problem of low molecular weight in the syndiotactic polymerization of styrene with non-cene catalysts, and provides 2-hydroxybenzophenone titanium catalysts. It includes a cocatalyst and a main catalyst, the cocatalyst is an alkyl aluminoxane, and the main catalyst is a chloride, an alkoxy compound, a phenoxy compound, or a substituted phenoxy compound of 2-hydroxybenzophenone titanium; its molar ratio is 2000 :1~100:1. The catalytic activity of this catalyst is 1×10 4 ~1×10 6 gPS / molTi·h, and can be maintained for two hours; and the production raw materials are cheap, the reaction can be carried out at room temperature, and the production cost is low; when using it to synthesize syndiotactic polystyrene, the process is simple and easy to control, and the obtained polymer The molecular weight is 150,000 to 300,000. The catalyst of the invention promotes the industrialization process of syndiotactic polystyrene.

Description

technical field [0001] The invention belongs to a non-cene catalyst for synthesizing syndiotactic polystyrene and a preparation method thereof, in particular to a 2-hydroxybenzophenone complex containing titanium as the main catalyst, which can make syndiotactic polystyrene have a relatively high molecular weight. The cocatalyst is the catalyst of alkyl aluminoxane and its preparation method. technical background [0002] Syndiotactic polystyrene (sPS) is a new polyolefin material with good application prospect and important value. In 1986, Japan's Idemitsu Chemical Company first successfully developed a new type of syndiotactic polystyrene (sPS) (Macromolecues, 1986, 19: 2464) with a metallocene catalyst, which has a high melting point, fast crystallization speed, high elastic modulus, insulation and Due to its excellent solvent resistance, sPS can be used in almost all engineering plastic applications such as PET, PBT, PA, and PPS, such as medical devices, magnetic films ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/76C08F212/08
Inventor 闫卫东杨敏沈晓莉丁会利刘盘阁黄英娟李海青李贺新
Owner HEBEI UNIV OF TECH
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