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Catalyst for olefin oligomerization and polymerization and preparation method thereof

A catalyst and olefin technology, applied in the field of catalysts for oligomerization and polymerization of olefins and their preparation, can solve the problem of low activity and the like

Inactive Publication Date: 2012-07-18
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Structural formula C is another phosphinoguanidine ligand structure compound and iron complex reported by Tang Yong and his collaborators in Chinese patent CN1364818A and US patent US 2005 / 0004331 A1. This compound has ethylene catalytic activity, but the activity is not high

Method used

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  • Catalyst for olefin oligomerization and polymerization and preparation method thereof
  • Catalyst for olefin oligomerization and polymerization and preparation method thereof
  • Catalyst for olefin oligomerization and polymerization and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1, the synthesis of catalyst C-1

[0049] I. Preparation of Ligands

[0050] 1) In a 1000mL Schlenk bottle, add 29.98g N-2,6-diisopropylphenyl-2-phenyl-2-chloro-imine (100mmol), 27.73g o-diphenylphosphinoaniline (100mmol) and 400mL toluene. After replacing the atmosphere in the bottle with nitrogen, heat to reflux at 120° C. for 20 h to obtain the hydrochloride of the prepared ligand.

[0051] 2) The hydrochloride was dissolved in 300 mL of 95% ethanol, and neutralized by adding 300 mL of 25% ammonia water dropwise. The resulting solid was collected by filtration, dried under vacuum for 4 h, and recrystallized in toluene to give a white crystalline product 1 LH45.9g, yield 85%. Elemental analysis results: calculated value: N, 5.18; C, 82.19; H, 6.71; found value: N, 5.06; C, 81.88; H, 6.67.

[0052] 1 H NMR (400MHz, CDCl 3 ): δ=7.51-6.48 (m, 2H), 6.25 (s, 1H), 3.06 (sept, 2H), 1.15 (d, 6H), 1.14 (d, 6H) ppm.

[0053] 31 P NMR (376MHz, CDCl 3 ): δ = ...

Embodiment 2

[0060] Embodiment 2, the synthesis of catalyst C-2

[0061] I. Ligand 1 Preparation of LH

[0062] Ligand 1 The preparation process of LH is as described in Example 1.

[0063] II. Synthesis of Ligand Transition Metal Complex Catalysts

[0064] In a 100 mL Schlenk bottle, under nitrogen atmosphere, add 0.54 g ligand 1 LH (1mmol), 0.13g CoCl 2 (1 mmol) and 50 mL THF solvent. The reaction solution turned blue-green. After stirring for 12 h, the solvent was removed in vacuo, and the crude product was washed several times with n-hexane to obtain 20.62 g of blue-green solid product C-2, with a yield of 92.5%.

[0065] Elemental analysis results: calculated value: N, 4.18; C, 66.28; H, 5.41; found value: N, 4.09; C, 66.40; H, 5.45.

[0066] IR (KBr pellet, cm -1 ): 3253.61 (v N-H ), 2964.06, 1590.53 (v C＝N ),1555.22,1496.88,1463.11,1438.11,1404.60,1364.17,1324.37,1269.52,1255.13,1184.07,1159.03,1123.56,1101.88,1063.87,1026.26,998.06,923.85,833.85,805.62,795.85,768.64,761....

Embodiment 3

[0068]Embodiment 3, the synthesis of catalyst C-3

[0069] I. Ligand 1 Preparation of LH

[0070] Ligand 1 The preparation process of LH is as described in Example 1.

[0071] II. Synthesis of Ligand Transition Metal Complex Catalysts

[0072] In a 100 mL Schlenk bottle, under nitrogen atmosphere, add 0.54 g ligand 1 LH (1mmol), 0.37g CrCl 3 (THF) 3 (1 mmol) and 50 mL THF solvent. The reaction solution turned dark green. After stirring for 25 h, the solvent was removed in vacuo, and the crude product was washed several times with n-hexane to obtain 0.65 g of dark green solid product C-3 with a yield of 92.9%.

[0073] Elemental analysis results: calculated value: N, 4.01; C, 63.57; H, 5.19; found value: N, 3.91; C, 62.79; H, 5.38.

[0074] IR (KBr pellet, cm -1 ): 3283.34 (v N-H ), 2922.94, 2853.17, 2725.19, 2669.36, 2405.52, 1589.82 (v C＝N ),1555.57,1460.61,1377.12,1305.37,1156.82,1100.32,1078.45,1026.03,997.56,965.96,934.11,891.87,871.63,846.39,830.84,805.35,793....

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Abstract

A catalyst for olefin oligomerization and polymerization and a preparation method thereof relate to a catalyst. Hydrochloride is formed by reacting phosphonic base guanidine ligands with amine chloride and adjacent-diphenyl phosphonic base aniline of different nitrogen substituent in the atmosphere of nitrogen according to molar ratio of 1:1 in an organic solvent at the temperature of 20-150 DEG C within 5-100 hours; further neutraling the hydrochloride through alkali, and enabling the total yield to be larger than 60%. The catalyst is combined with an assistant catalyst with Lewis acidity or with both the Lewis acidity and alkyl exchange performance to form a catalyst system capable of catalyzing ethylene to polymerize or to both polymerize and oligomerize. The polymerization activity can be as high as 2.51*106g mol-1 (metal) -1. The selectivity of alpha- olefin C6-12 in an oligomer is 45.0%-60.6%. The molecular weight of a molymerizer is widely distributed (4.5-120.50), and the catalyst is suitable for industrial processing.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for olefin oligomerization and polymerization and a preparation method thereof. Background technique [0002] Late transition metal iron complex catalysts are used for olefin polymerization initially by Brookhart (J.Am.Chem.Soc., 1998,120:7143; U.S. Patent US 6103946) of the United States and Gibbson (Chem.Commun., 1998 , 849; WO Patent-99 / 02472) independently discovered. The ligand used in the complex is pyridinediimine-NNN compound. The system composed of the catalyst and the cocatalyst alkyl aluminum compound can efficiently catalyze the oligomerization of ethylene to generate alpha-olefin oligomers, and can also catalyze the polymerization of ethylene to generate high polymers. Its structural formula is respectively: [0003] [0004] In these late-transition metal iron-based complex catalysts, the steric space and electronic structure of the ligands play an important role in re...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F4/70C08F4/69C08F4/642
Inventor 朱红平朱孔涛朱涛谭庚文李岩万惠霖
Owner XIAMEN UNIV
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