Binuclear beta-diketone catalyst for synthesizing syndiotactic polystyrene and its preparation method

A polystyrene and catalyst technology, applied in the field of dual-nuclear catalyst and its preparation, can solve the problems of low polymerization activity, and achieve the effects of low production cost, inhibition of bimolecular deactivation, and cheap raw materials

Inactive Publication Date: 2005-08-24
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention overcomes the problem of relatively low polymerization activity when using a single active center catalyst, i.e., complexes of β-diketone titanium for syndiotactic polymerization of styrene

Method used

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  • Binuclear beta-diketone catalyst for synthesizing syndiotactic polystyrene and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-12

[0026] Examples 1-12: Synthesis of catalyst components of the present invention, and their properties are shown in Table 1.

[0027]

Reality

Example

R

R’

-Y-

main catalyst

Al / T

i(Ni)

T

(℃)

activity

(10 5 gPS /

molTi(Ni) h)

between

gauge

%

T m

(℃)

1

2

3

4

5

7

8

9

10

11

12

CH 3

CH 3

CH 3

CH 3

CH 3

CH 3

C 6 h 5

C 6 h 5

C 6 h 5

C 6 h 5

C 6 h 5

C 6 h 5

CH 3

CH 3

CF 3

CH 3

CH 3

CH 3

C 6 h 5

C 6 h 5

CF 3

C 6 h 5

C 6 h 5

C 6 h 5

-(CH 2 ) 6 -

-

-C 6 h 4 -

-(CH 2 ) 10 -

-(1,4-(CH 2 ) 2 C 6 h 4 )-

-(2,6-dmp)-

-

-(2,4-dmp)-

-C 6 h 4 -

-C 6 h 4 - ...

Embodiment 1

[0032] In a 100ml two-necked flask equipped with a stirrer, add 20ml of ethanol and 2.3g of alkali metal sodium, under the reflux temperature of ethanol, add 1.5g of acetylacetone and 2g of dichlorohexane respectively, react for 2 hours, filter and dry to obtain the ligand ( CH 3 CO) 2 CH-(CH 2 ) 6 -CH(COCH 3 ) 2 0.85g. N at 0°C 2 Dissolve 0.5g of the ligand in ether solution and add to the solution containing 1.5ml of Ti(OPh) 4 Carry out complex coordination in the diethyl ether solution, when the temperature reaches room temperature, 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 A 2 [Ti(OPh) 2 ] 2 (A=(CH 3 CO) 2 CH-(CH 2 ) 6 -CH(COCH 3 ) 2 ) 0.46g. 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 [...

Embodiment 2

[0034] In a 100ml two-necked flask equipped with a stirrer, add 20ml of ethanol and 2.3g of alkali metal sodium, and at the reflux temperature of ethanol, add 1.5g of acetylacetone and 2g of potassium iodide respectively, react for 2 hours, filter and dry to obtain the ligand (CH 3 CO) 2 CH-CH (COCH 3 ) 2 0.63g. N at 0°C 2 Dissolve 0.4g of the ligand in ether and add to the solution containing 1.5ml of TiCl 4 Carry out complexation and coordination in the diethyl ether liquid, when the temperature reaches room temperature, 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 A (TiCl 3 ) 2 (A=(CH 3 CO) 2 CH-CH (COCH 3 ) 2 ) 0.26g. In a 100ml two-necked flask replaced by nitrogen and equipped with a stirrer, add 15ml of toluene distilled by metal sodium reflux, heat up to 80°C under stirring, add the main catalyst A (TiCl 3 ) 2 19.69mg (the concentration is 1×10...

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Abstract

The present invention relates to a binuclear beta-diretone catalyst for synthesizing syndiotactic polystyrene and its preparation method. Said catalyst incldues cocatalyst and maincatalyst, its mole ratio is 2000:1-200:1, in which its main catalyst is chloride of binuclear beta-diketone titanium or nickel, oxyalkyl compound and phenoxy or substituted phenoxy compound. The raw materials for synthesizing said catalyst are cheap, can be reacted at zero deg.c to normal temp., and its production cost is low.

Description

technical field [0001] The invention belongs to a dinuclear catalyst for synthesizing syndiotactic polystyrene and a preparation method thereof, in particular to a syndiotactic synthesis in which the main catalyst is a dinuclear β-diketone complex containing titanium or nickel, and the cocatalyst is aluminoxane Polystyrene catalyst and preparation method. technical background [0002] Syndiotactic polystyrene (sPS) is a new type of polyolefin material with good application prospects and important value in engineering plastics. 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. It has excellent performance and has extremely broad application prospects. Its high melting point, fast crystallization speed, high elastic modulus, excellent insulation and solvent resistance make it enter the ranks of engineering plastics, compete with polyester, nylon and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/642C08F112/08
Inventor 闫卫东杨敏刘盘阁丁会利曹晨刚黄英娟李贺新李海青
Owner HEBEI UNIV OF TECH
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