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Salicylaldehyde pyridine imine titanium trichloride complex, its preparation method and application, and the method of ethylene polymerization reaction

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: 2015-12-09
CHINA PETROLEUM & CHEM CORP
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 imine titanium trichloride complex, its preparation method and application, and the method of ethylene polymerization reaction
  • Salicylaldehyde pyridine imine titanium trichloride complex, its preparation method and application, and the method of ethylene polymerization reaction
  • Salicylaldehyde pyridine imine titanium trichloride complex, its preparation method and application, and the method of ethylene polymerization reaction

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preparation example Construction

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

[0049] (1) Under the conditions of the aldoamine condensation reaction, the salicylaldehyde of the structure represented by formula (II) and the 2-aminopyridine compound of the structure represented by formula (III) are subjected to the first contact reaction to obtain formula (IV) The pyridine imine compound shown;

[0050]

[0051] Where 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 formula (IV) and the metal hydride are subjected to a second contact reaction at a temperature of -25°C to 25°C to obtain a suspension;

[0053] (3) Make the above suspension and TiCl at a temperature of -78℃ to 25℃ 4 ·(THF) 2 After mixing, the third contact reaction is carried out under the conditions of the coor...

Embodiment 1

[0079] 1) Mix 2.34g (10mmol) of 3,5-di-tert-butylsalicylic aldehyde and 0.94g (10mmol) of 2-aminopyridine evenly, and place them in a microwave oven with a frequency of 800MHz. After heating at 200W) for 1 minute, take it out and cool it to room temperature, and then heat it under medium-high fire for 1 minute to obtain red and black liquid. It was recrystallized with ethanol to obtain 2.52 g of orange-yellow crystals of 3,5-di-tert-butylsalicylic aldehyde 2-pyridineimine with a yield of 81.2%.

[0080] Use IR, 1 HNMR, 13 CNMR and elemental analysis were used to characterize the structure of the obtained product. The results are as follows:

[0081] IR(KBr, cm -1 ): 3000(OH)(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 HNMR: (CDCl 3 , 400MHz, ppm): δ 13.90 (s, 1H, OH), 9.47 (s, 1H, CH=N), 8, 50 (d, 1H, J= 3.60 Hz, Py-H), 7.76 (t, 1H, J = 7.56 Hz, Py-H), 7.49 (s, 1H, Ar-H), 7.35 (d, 1H...

Embodiment 2

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

[0095] Use IR, 1 HNMR, 13 CNMR and elemental analysis were used to characterize the structure of the obtained product. The results are 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 HNMR: (CDCl 3 , 400MHz, ppm): δ 13.93 (s, 1H, OH), 9.42 (s, 1H, CH=N), 8.31 (s, 1H, Py-H), 7.56 (d, 1H, J=7.88 Hz, Py-H), 7.46...

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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 pyridine imine titanium trichloride complex, a preparation method and application thereof, and an ethylene polymerization method using the salicylaldehyde pyridine imine titanium trichloride complex. Background technique [0002] Polyethylene resin (PE) is currently the synthetic resin with the largest output. Its price is cheap and its performance is good. It occupies a pivotal position in the plastics industry. The catalyst is an important factor affecting the molecular weight and molecular weight distribution of polyethylene. The development of a low-cost, high-activity and good product performance catalyst is one of the key directions for the development of the polyolefin industry. [0003] At present, the industrialized polyethylene catalysts include Ziegler-Natta type catalysts [DEPat889229 (1953); ITPat545332 (1956); ITPat536899 (1955); Chem. Rev., 2000, 100, 1169], Phillips type catalysts [Belg.Pat. 530617 (...

Claims

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Application Information

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Patent Type & Authority Patents(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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