Ethylene oligomerization after-trasition metal coordination catalyst and its application

A late-transition metal and coordination catalyst technology, applied in organic chemistry, hydrocarbons, hydrocarbons, etc., can solve the problems of complex synthesis steps and preparation methods, and achieve wide distribution of catalytic activity, high catalytic activity, and easy purification Effect

Inactive Publication Date: 2003-02-05
INST OF CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis steps and preparation methods of the above-mentioned catalysts are relatively complicated, and the catalytic activity is between 10 4 to 10 6 g ethylene / (mole Ni·hour)

Method used

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  • Ethylene oligomerization after-trasition metal coordination catalyst and its application
  • Ethylene oligomerization after-trasition metal coordination catalyst and its application
  • Ethylene oligomerization after-trasition metal coordination catalyst and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Synthesis of ligand 2,6-bis(2,6-diisopropylphenylimino)-4-tert-butylphenol: under nitrogen protection, 4-tert-butyl-2,6-dimethyl Acylphenol (1.76g, 6mmol) was dissolved in absolute ethanol solution (25mL), then 3 drops of acetic acid were added, then the temperature was raised to 50°C, and 2,6-diisopropylaniline (2.16g , 13.2mmol) in absolute ethanol (15mL). After dripping, heat to reflux, continue to stir for 2 hours, cool to room temperature, evaporate most of the solvent under reduced pressure, and place the product mother liquor in the refrigerator overnight, 2.8 g of yellow crystals precipitate out, yield: 70%. m.p.192.5-193℃.IR(KBr): 3414(m), 3063(m), 2963, 2869(s), 1629, 1586(vs), 1540(s), 1460(s), 1360, 1313, 1282 , 1227, 1179(s), 819, 758(s); 1 H NMR (CDCl 3 ): δ1.27 (24H, d, J=6.8Hz), 1.49 (9H, s), 3.04-3.14 (4H, m), 7.24 (6H, m), 7.5 (1H, br), 8.37-8.80 ( 3H, br); EI-MS (m / z): 524 (M + , 7.8%), 509 (5.1%), 349 (23.6%), 348 (100%), 319 (5.5%); 176 (12.3%)...

Embodiment 2

[0026] The synthesis of ligand is the same as in Example 1

[0027] Preparation of 2,6-bis(2,6-diisopropylphenylimino)-4-tert-butylphenol nickel complex (2) catalyst:

[0028] Under nitrogen, to a 30 mL Schlenk tube was added 2,6-bis(2,6-diisopropylphenylimino)-4-tert-butylphenol (167 mg, 0.32 mmol), (DME)NiBr 2 (77mg, 0.25mmol), then inject freshly treated dichloromethane (10mL), stir at 25°C for 18 hours, distill off excess dichloromethane, add 5mL of anhydrous ether, filter the precipitated solid, and wash with ether (3×2 mL). Vacuum drying gave 124 mg of dark green solid powder, yield: 73%. m.p.238℃(dec.).IR(KBr): 3389(br), 2964(m), 1637(s), 1538(s), 1463(m), 1390(m), 1363, 1328, 1289, 1234 , 1177(m), 1060(m); FAB-MS(m / z): 663(M + -Br), 582 (M + -2Br), 525 (M + -NiBr 2 ); Anal.Calcd.for C 36 h 48 N 2 ONiBr 2 ·H 2 O: C, 56.80; H, 6.62; N, 3.68. Found: C, 56.80; H, 6.37; N, 3.52%.

[0029] Oligomerization of ethylene under normal pressure: put a stirring magnet ...

Embodiment 3

[0034] Synthesis of ligand 2,6-bis(2,6-dimethylphenylimino)-4-tert-butylphenol: Synthesis of ligand 2,6-bis(2,6-bis isopropylphenylimino)-4-tert-butylphenol method, to obtain yellow solid 2,6-two (2,6-dimethylphenylimino)-4-tert-butylphenol, yield Rate: 79%. m.p: 162.5-163°C. IR(KBr): 3368(Br), 2962(s), 1630, 1588(s), 1469(s), 1369(s), 1310, 1284, 1263, 1232, 1190(m), 1091, 1034, 1006 (m), 858, 765 (m); 1 H NMR (CDCl 3 ): δ1.44 (9H, s), 2.24 (12H, s), 6.95-7.14 (6H, m), 7.3-8.60 (4H, br); EI-MS (m / z): 412 (M+, 6.6 %), 411 (4.4%), 292 (100%), 291 (85.4%), 290 (8.3%), 277 (6.6%), 206 (5.1%), 132 (8.2%), 120 (6.9%) , 105 (10.1%); Anal.Calcd.for C 28 h 32 N 2 O: C, 81.51; H, 7.82; N, 6.79. Found: C, 81.22; H, 8.21; N, 6.34%.

[0035] Preparation of 2,6-bis(2,6-dimethylphenylimino)-4-tert-butylphenol cobalt complex (3) catalyst:

[0036] Using Example 1 to synthesize 2,6-bis(2,6-isopropylphenylimino)-4-tert-butylphenol CoCl 2 method using ligands 2,6-bis(2,6-dimethylphen...

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Abstract

The present invention discloses a transition metal coordinate catalyst after oligomerization of ethylene and its application in the oligomerization of ethylene. Said ivnention provides the structure formula of said catalyst. Said catalyst is simple in preparation process, easy to purify, its compound stability if good, and is convenient for large-scale production, and its activity reproducibility is good.

Description

Technical field: [0001] The present invention relates to a post-ethylene oligomerization transition metal coordination catalyst and its use for ethylene oligomerization. Background technique: [0002] Catalytic ethylene oligomerization can produce linear olefins on a large scale. The products are important organic chemical intermediates and have become an independent branch of the petrochemical industry. In recent years, the research on late transition metal olefin polymerization and oligomerization catalysts has developed rapidly (Angew. Chem. Int. Ed. 1999, 38, 428-447; Chem. Rev. 2000, 100, 1169-1203). In addition, the development of olefin polymerization has prompted people to copolymerize ethylene with other olefins to obtain polyolefin materials with different structures and properties. It is urgent to prepare C 4 、C 6 、C 8 Ethylene oligomers. [0003] Since the 1970s, the homogeneous catalysis of olefin polymerization and oligomerization by transition metal comple...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C2/22
Inventor 孙文华王乐勇韩玲芹李子龙胡友良李秀华
Owner INST OF CHEM CHINESE ACAD OF SCI
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