Salicylaldehyde pyridine imido titanium trichloride complex, its preparation method and application thereof, and polymerization method of ethene

A technology of salicylaldehyde pyridinimine titanium trichloride and pyridinimine, which is applied in the direction of titanium organic compounds to achieve the effect of high catalytic reaction activity

Active Publication Date: 2013-01-02
CHINA PETROLEUM & CHEM CORP
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  • Abstract
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Problems solved by technology

[0006] FI catalysts and PI catalysts can achieve high ethylene polymerization activity, but due to the protection of patents, these catalysts cannot be widely used in the development of my country's polyolefin industry

Method used

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  • Salicylaldehyde pyridine imido titanium trichloride complex, its preparation method and application thereof, and polymerization method of ethene
  • Salicylaldehyde pyridine imido titanium trichloride complex, its preparation method and application thereof, and polymerization method of ethene
  • Salicylaldehyde pyridine imido titanium trichloride complex, its preparation method and application thereof, and polymerization method of ethene

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preparation example Construction

[0048] The preparation method of salicylaldehyde pyridine imine titanium trichloride complex provided by the present invention comprises the following steps:

[0049] (1) Under the aldehyde-amine condensation reaction conditions, the salicylaldehyde of the structure shown in the formula (II) and the 2-aminopyridine type compound of the structure shown in the formula (III) are carried out the first contact reaction, obtain the formula (IV) The shown pyridine imine compound;

[0050]

[0051] Among them, R 1 -R 8 The definition of is the same as the above formula (I).

[0052] (2) Under the protection of an inert gas, the dry solution of the pyridine imine compound represented by the formula (IV) is subjected to a second contact reaction at a temperature of -25°C to 25°C with a metal hydride to obtain a suspension;

[0053] (3) At a temperature of -78°C to 25°C, the above suspension was mixed with TiCl 4 ·(THF) 2 After mixing, the third contact reaction is carried out un...

Embodiment 1

[0079] 1) 2.34g (10mmol) 3,5-di-tert-butyl salicylaldehyde and 0.94g (10mmol) 2-aminopyridine are mixed uniformly, placed in a microwave oven with a frequency of 800MHz, and placed on a medium-high fire (power of microwave irradiation) Heated at 200W) for 1 minute, took it out and cooled to room temperature, and heated at medium-high heat for 1 minute to obtain a red-black liquid. Recrystallized with ethanol to obtain 2.52 g of orange crystals of 3,5-di-tert-butyl salicylaldehyde 2-pyridinimine with a yield of 81.2%.

[0080] with IR, 1 H NMR, 13 C NMR, elemental analysis characterize the product structure of gained, and the results are as follows:

[0081] IR (KBr, cm -1 ): 3000(O-H)(w), 2960(s), 2906(m), 2867(m), 1610(CH=N)(m), 1579(s), 1461(s), 1432(s), 1360(m), 1198(m), 1169(s), 881(m), 791(m), 769(m), 736(m).

[0082] 1 H NMR: (CDCl 3 , 400MHz, ppm): δ13.90(s, 1H, OH), 9.47(s, 1H, CH=N), 8, 50(d, 1H, J=3.60Hz, Py-H), 7.76(t, 1H, J=7.56Hz, Py-H), 7.49(s, 1H, Ar-H),...

Embodiment 2

[0094] 1) Mix 2.34g (10mmol) 3,5-di-tert-butyl salicylaldehyde and 1.08g (10mmol) 2-amino-5-methylpyridine evenly, place it in a microwave oven with a frequency of 800MHz, and set it under medium-high heat After heating for 2 minutes, take it out and cool it to room temperature, and then heat it under medium-high heat for 2 minutes to obtain a red-black liquid. Recrystallized with ethanol to obtain 2.36 g of orange crystals of 3,5-di-tert-butyl salicylaldehyde-2-pyridine-5-methylimine with a yield of 73.8%.

[0095] with IR, 1 H NMR, 13 C NMR, elemental analysis characterize the product structure of gained, the result is as follows:

[0096] IR (KBr, cm -1 ): 2997(w), 2958(s), 2906(m), 2868(m), 1612(CH=N)(m), 1570(s), 1462(s), 1386(m), 1358(m ), 1251(m), 1169(s), 1022(m), 881(m), 828(m), 769(w), 680(w).

[0097] 1 H NMR: (CDCl 3 , 400MHz, ppm): δ13.93(s, 1H, OH), 9.42(s, 1H, CH=N), 8.31(s, 1H, Py-H), 7.56(d, 1H, J=7.88Hz, Py-H), 7.46(s, 1H, Ar-H), 7.34(s, 1H, Ar-H), 7....

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Abstract

The invention discloses a salicylaldehyde pyridine imido titanium trichloride complex, its preparation method and an application thereof, and is characterized in that the complex has a structure as shown in the formula (I), wherein R1-R8 each is hydrogen, a substituted or unsubstituted C1-C8 alkyl group or halogen. The invention also discloses a polymerization method of ethene and an ethene polymer prepared by the method. According to the method, alkene undergoes polymerization in the presence of an organic solvent, a cocatalyst and a main catalyst and under the condition of alkene polymerization, wherein the alkene is ethene or a mixture containing ethene and C4-C10 alpha-alkene. The method is characterized in that the main catalyst is the above salicylaldehyde pyridine imido titanium trichloride complex.

Description

technical field [0001] The invention relates to a salicylaldehyde pyridinimine titanium trichloride complex, a preparation method and application thereof, and a method for ethylene polymerization using the salicylaldehyde pyridinimine titanium trichloride complex. Background technique [0002] Polyethylene resin (PE) is the synthetic resin with the largest output at present. It is cheap and has good performance, and occupies a pivotal position in the plastics industry. Catalyst is an important factor affecting the molecular weight and molecular weight distribution of polyethylene, and the development of a low-cost, high-activity catalyst with good product performance is one of the key directions for the development of the polyolefin industry. [0003] At present, industrialized polyethylene catalysts include Ziegler-Natta type catalyst [DE Pat 889229 (1953); IT Pat 545332 (1956); IT Pat 536899 (1955); Chem.Rev., 2000,100,1169], Phillips type Catalysts [Belg. Pat. 530617 (19...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28C08F10/02C08F4/642
Inventor 华炜孙文华赵丽梅刘淇邴涓林黄伟张文娟陈青葵
Owner CHINA PETROLEUM & CHEM CORP
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