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Caliper type chromium complex and preparation method and application thereof

A chromium complex, pincer type technology, applied to catalysts containing pincer chromium complexes, catalyzing isoprene or butadiene trans-1 field, can solve the problems of different polymer ratios, difficulties, etc., and achieve a narrow molecular weight distribution. , the effect of fast polymerization reaction and convenient preparation

Inactive Publication Date: 2011-07-20
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the ratio of various polymers obtained by using different catalysts is different, and it is very difficult to selectively control the ratio of each polymer in actual operation

Method used

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  • Caliper type chromium complex and preparation method and application thereof
  • Caliper type chromium complex and preparation method and application thereof
  • Caliper type chromium complex and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Preparation of clamp-type chromium complex (chromium complex 1)

[0038]

[0039] At -78°C, a hexane solution of butyllithium (1.2mL, 1.88mmol) was slowly added dropwise to 2,6-bis(N-2,6-phenyl)iminobromobenzene (0.6690g , 1.84mmol) in 30mL tetrahydrofuran solution, add CrCl to it after 30 minutes of low temperature reaction 3 (THF) 3 (0.7043g, 1.88mmol), naturally warmed to room temperature and continued to react for 4 hours, the solvent was removed in vacuo, the residue was extracted with toluene, and the toluene solution was concentrated to obtain 0.52 g of bright green crystal complex 1 with a yield of 60%. Elemental analysis, its molecular formula is C 24 h 23 Cl 2 CrN 2 O (%): C, 60.26; H, 4.85; N 5.86.

Embodiment 2

[0040] Example 2 Preparation of clamp-type chromium complex (chromium complex 2)

[0041]

[0042] At -78°C, a hexane solution of butyllithium (0.86mL, 1.35mmol) was slowly added dropwise to 2,6-bis(N-2,6-dimethylphenyl)iminobromobenzene (0.5625g, 1.34mmol) in 30mL tetrahydrofuran solution, add CrCl to it after 30 minutes of low temperature reaction 3 (THF) 3 (0.5148g, 1.37mmol), naturally warmed to room temperature and continued to react for 4 hours, the solvent was removed in vacuo, the residue was extracted with toluene, and the toluene solution was concentrated to obtain 0.50 g of bright green crystal complex 2 with a yield of 71%. Elemental analysis, its molecular formula is C 28 h 31 Cl 2 CrN 2 O (%): C, 62.92; H, 5.85; N, 5.24.

Embodiment 3

[0043] Example 3 Preparation of clamp-type chromium complex (chromium complex 3)

[0044]

[0045] At -40°C, a hexane solution of butyl lithium (1.33 mL, 1.33 mmol) was slowly added dropwise to 2,6-bis(N-2,6-diethylphenyl)iminobromobenzene (0.5773g, 1.21mmol) in 30mL tetrahydrofuran solution, add CrCl to it after 30 minutes of low temperature reaction 3 (THF) 3 (0.5100g, 1.36mmol), naturally warmed to room temperature and continued to react for 4 hours, the solvent was removed in vacuo, the residue was extracted with toluene, and the toluene solution was concentrated to obtain 0.42 g of bright green crystal complex 3 with a yield of 56%. Elemental analysis, its molecular formula is C 32 h 39 Cl 2 CrN 2 O (%): C, 65.08; H, 6.66; N, 4.74.

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Abstract

The invention relates to a caliper type chromium complex and a preparation method and application thereof, and belongs to the technical field of catalysts. The caliper type chromium complex is a [NCN]-ligand-based caliper type chromium complex. The preparation method comprises the following steps of: adding hexane solution of butyl lithium into tetrahydrofuran solution of a ligand dropwise for reaction; adding a tetrahydrofuran adduct of chromium trichloride or chromium dichloride; and heating the mixture to room temperature naturally and reacting to obtain the caliper type chromium complex. The ligand can be 2,6-bis(N-2,6- phenyl)imido bromobenzene. The caliper type chromium complex, alkyl aluminum and organic boron salt serving as catalysts are used for catalyzing selective polymerization of isoprene or butadiene. The caliper type chromium complex has high stability and is convenient to prepare; the catalytic system can be used for selectively catalyzing polymerization of the isoprene or the butadiene, and has low using amount of a cocatalyst, high polymerization speed, high conversion rate and high anti-1,4 selectivity; and the caliper type chromium complex can be applied actually by replacing natural trans-1,4 rubber.

Description

technical field [0001] The invention belongs to the technical field of catalysts, in particular to a catalyst containing pincer chromium complexes, which is used to catalyze the reverse 1,4-selective polymerization of isoprene or butadiene. Background technique [0002] Trans-1,4-polyisoprene is a kind of isoprene rubber. Its chemical composition is the same as that of the familiar cis-1,4-polyisoprene. The two polymers are isomers. However, the spatial orientation of the groups on the double bond unit in the polymer chain is different. In trans-1,4-polyisoprene molecular chain, the double bonds in the trans structure are absolutely dominant, while in the cis-1,4-polyisoprene molecular chain, the double bonds in the cis structure are dominant. These two different arrangements lead to a huge difference in performance. cis-1,4-isoamyl rubber has typical elastomer properties, and its properties are similar to natural rubber, such as slow crystallization at room temperature an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F11/00C08F4/69C08F136/08C08F136/06
Inventor 母瀛高伟刘志周
Owner JILIN UNIV
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