Syndiotactic polystyrene sythesizing 2-hydroxy benzophenone titanium catalyst and its preparing method

A technology of hydroxybenzophenone and polystyrene, which is applied in the field of non-cene catalysts and its preparation, can solve the problems of low molecular weight of polymers, achieve the effects of low production cost, easy control, and speed up the process of marketization

Inactive Publication Date: 2004-02-11
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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-10

[0021] Example 1-10: Synthesis of the structure, components and related properties of the catalyst of the present invention, see Table 1 for details.

[0022] Synthesize the structure, components and relevant properties of the catalyst of the present invention Table 1 implementation R R R main catalyst Al / Ti T activity (×10 5 gPS Syndiotacticity T m Mw (×case (°C) / molTi h) % (°C) 10 4 )1 - CH 3 CH 3 A 2 Ti(OPh) 2 1100 20 0.5 96 265 162 CH 3 C 2 h 5 -ATiCl 3 500 80 8.3 93 270 233 C 3 h 7 -CH 3 A 3 TiCl 2000 80 0.9 94 275 184 CH 3 C 3 h 7 C 2 h 5 ATi(OPh) 3700 40 7.1 98 269 175 CH 3 O C 4 h 9 C 3 h 7 A 2 TiCl 2 600 90 4.8 95 267 296C 4 h 9 O CH 3 CH 3 ATi(OEt) 3 800 60 6.4 94 266 307 - C 2 h 5 C 3 h 7 ATi(OPhOMe) 3 400 80 3.2 96 270 248 CH 3 C 4 h 9 CH 3 A 3 TiCl 200 70 7.0 96 268 229 C 3 h ...

Embodiment 1

[0025] N at room temperature 2 Dissolve 0.42 g of ligand A of the structure shown in Table 1, that is, 2-hydroxybenzophenone, in ether and add it to a solution containing 1.5 ml of Ti(OPh) 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 ...

Embodiment 2

[0027] 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 present invention relates to a kind of non-cyclopentadiene catalyst for synthesizing syndiotactic polystyrene. The catalyst includes main catalyst comprising 2-hydroxy benzophenone titanium chloride, alkoxy compound and phenoxy or substituted phenoxy compound in the molar ratio of 2000 to 1-100 to 1; and co-catalyst alkyl alum inoxane. The catalyst has activity of 1E4-1E6 gPS/mol Ti. hr andmay be maintained for 2 hr without lowering; and may be produced through reaction at normal temperature in low cost. When it is used in producing syndiotactic polystyrene, the process is simple and easy to control and the molecular weight of the polymer is 150-300 kD.

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 Applications(China)
IPC IPC(8): C08F4/76C08F212/08
Inventor 阎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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