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Substituted indenyl metal titanium compound and its preparation method and use

A technology of titanium compounds and base metals, applied in the direction of titanium organic compounds, etc., can solve the problem of low catalytic activity

Inactive Publication Date: 2003-04-30
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] One of the technical problems to be solved by the present invention is to overcome the defect that the indenyl compound obtained in the prior art is used in the syndiotactic polymerization of styrene, and the catalytic activity is low, and to provide a new substituted indenyl metal titanium compound
[0008] The second technical problem to be solved by the present invention is to solve the preparation method required to obtain substituted indenyl metal titanium compounds

Method used

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  • Substituted indenyl metal titanium compound and its preparation method and use

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Experimental program
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Effect test

Embodiment 2

[0033] All operations are the same as in Example 1, except that methanol is used instead of ethanol to finally obtain 1-CH 3 IndTiCl 2 (OMe) red crystals, yield 73.6%, m.p.=110-115°C. The analysis test results are as follows

[0034] Molecular formula: C 11 h 12 Cl 2 OTi;

[0035] M.S. (EI): 278 (6, M + ).

[0036] 1 H NMR (CDCl 3 , δ): 7.76~7.68 (m, 2H, IndH 2 ), 7.47~7.44 (m, 2H, IndH 2 ), 6.72 (d, IH, J=3.3, IndH), 6.61 (d, 1H, J=3.3, IndH), 4.36 (s, 3H, OCH 3 ), 2.64(s, 3H, IndH 3 )

[0037] E.A.: Measured, C: 52.37% H: 5.65%

Embodiment 3

[0039] All operations are the same as in Example 1, except that isopropanol is used instead of ethanol to finally obtain 1-CH 3 IndTiCl 2 (O i Pr) Red crystals, yield 32.3%, m.p.=59-61°C. The analysis test results are as follows

[0040] Molecular formula: C 13 h 16 Cl 2 OTi;

[0041] M.S. (EI): 306 (6, M + ).

[0042] 1 H NMR (CDCl 3 , δ): 7.75~7.73 (m, 2H, IndH 2 ), 7.45~7.41 (m, 2H, IndH 2 ), 6.68 (d, 1H, J=3.3, IndH), 6.57 (d, 1H, J=3.3, IndH), 4.97 (m, 1H, J=6.1, OCH (CH 3 ) 2 ), 2.63(s, 3H, IndH 3 ), 1.31 (d, 6H, J=6.1, OCH (CH 3 ) 2 )

[0043] E.A.: Measured, C: 50.87% H: 5.25%

Embodiment 4

[0045] All operations are the same as in Example 1, except that ethanol is replaced by cyclohexyl, and finally 1-CH is obtained 3 IndTiCl 2 Red crystals, yield 37.3%, m.p.=84-86°C. The analysis test results are as follows

[0046] Molecular formula: C 16 h 20 Cl 2 OTi;

[0047] M.S. (EI): 346 (1, M + ).

[0048] 1 H NMR (CDCl 3 , δ): 7.76~7.73 (m, 2H, IndH 2 ), 7.48~7.42 (m, 2H, IndH 2 ), 6.68(d, 1H, J=3.3, IndH), 6.58(d, 1H, J=3.3, IndH), 4.75(m, 1H, ), 2.63(s, 3H, IndH 3 ), 1.90~1.28(m, 10H, )

[0049] E.A.: Measured, C: 55.36% H: 5.81%

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Abstract

A substituted indenyl metal titanium compound is prepared through reaction of relative alcohol solution with alkyllithium or Grignard reagent, adding relative substituted indenyl titanium trichloride solution, reaction, filter, concentrating and crystallizing. It has high catalytic activity to the syndiotactive polymerization of p-styrene.

Description

technical field [0001] The invention relates to a substituted indenyl metal titanium compound and a preparation method and use thereof. Background technique [0002] Atactic Polystyrene (aPS), obtained by free radical polymerization of styrene, has the advantages of hardness, transparency, insulation, and easy processing, and has been widely used in packaging, construction, medicine, electronics, automobiles, and daily necessities and other industries. However, due to the randomness of the structure, its softening temperature is about 100°C, which makes it brittle and poor in heat resistance and chemical corrosion resistance. [0003] In 1955, Natta et al. used TiCl 4 / AlEt 3 The catalytic system obtained isotactic polystyrene (isotactic Polystyrene, iPS), with a melting point of 240°C and high crystallinity, but its crystallization rate was too slow to achieve industrialization. [0004] Recently, Ishihara et al obtained syndiotactic polyst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28C08F4/76
Inventor 钱延龙钱贤苗张浩陈斌黄吉玲沈志刚
Owner CHINA PETROLEUM & CHEM CORP
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