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Bimetallic compound with limited configuration as well as preparation method and application of bimetallic compound

A compound and bimetallic technology, applied in the field of configuration-limited bimetallic compounds and their preparation, can solve the problems of long synthesis route of catalyst and expensive raw materials, achieve good catalytic activity and copolymerization ability, easy separation and purification, and short synthesis route. Effect

Inactive Publication Date: 2018-02-02
NANJING XIAOZHUANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The synthetic route of above-mentioned catalyst is long, and raw material is expensive

Method used

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  • Bimetallic compound with limited configuration as well as preparation method and application of bimetallic compound
  • Bimetallic compound with limited configuration as well as preparation method and application of bimetallic compound
  • Bimetallic compound with limited configuration as well as preparation method and application of bimetallic compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] This embodiment provides a bimetallic compound in a restricted configuration, the molecular formula of the complex C1 is: [(o-O(C 6 h 4 )CH=N)(TiCl 3 )] 2 (p-C 6 h 4 ).

[0059] The synthetic route of complex C1 is as follows:

[0060]

[0061] The specific preparation process of complex C1 is:

[0062] (1) Under argon protection, a reflux condenser was connected to a 250mL three-necked flask equipped with a magnetic stirrer, and at room temperature, salicylaldehyde (4.88g, 0.04mol), p-phenylenediamine (2.16 g, 0.02mol) and 120mL ethanol, 1mL methanesulfonic acid, heated to reflux for 6-8h, an orange-yellow solid was produced. Stop stirring, return to room temperature, suction filter, wash the solid with ethanol, and dry to obtain orange-yellow solid L1, 5.82 g, yield 92.0%.

[0063] 1 H NMR (400MHz, d-DMSO, ppm) δ9.03 (s, 1H, -CH=N); 13.07 (s, 1H, -OH); 6.98 (d, J = 8.4Hz, 1H, Ar-H) ;7.00(t,J=7.6Hz,1H,Ar-H);7.43(t,J=7.6Hz,1H,Ar-H);7.67(d,J=7.2Hz,1H,Ar-H);7...

Embodiment 2

[0068] The present embodiment provides a bimetallic compound in a restricted configuration, and the molecular formula of the complex C2 is: [(o-O(C 6 h 3 )-3-Me)CH=N)(TiCl 3 )] 2 (p-C 6 h 4 ).

[0069] The preparation process of complex C2 is the same as the preparation process of complex C1 in Example 1, the difference is only that salicylaldehyde is replaced by 3-allyl salicylaldehyde, and methanesulfonic acid is replaced by benzenesulfonic acid. Yield 76.0%.

[0070] 1 H NMR (400HMz, DMSO): δ9.07(s, 1H, -CH=N); 2.23(s, 3H, -CH 3 ); 6.91(t,1H,Ar-H); 7.33(d,1H,Ar-H); 7.53(d,1H,Ar-H); 7.60(s,2H,Ar-H). 13 C NMR (100HMz, DMSO): δ163.76, 158.94, 145.90, 134.56, 130.62, 125.31, 122.62, 118.80, 118.27, 15.31. Anal. Calcd for C 22 h 18 Cl 6 N 2 o 2 Ti 2 :C,43.20;H,3.62;N,3.87.Found:C,43.19;H,4.02;N,3.46.IR.(KBr,cm -1 )3330.9(s),1638.3(s),1597.6(s),1560.1(m),1516.3(w),1491.5(w),1384.7(m),1269.4(m),1190.8(m),873.9(m ), 894.7(m), 864.6(m), 783.8(w), 742.2(w), 428.3(w). ...

Embodiment 3

[0072] The present embodiment provides a bimetallic compound in a restricted configuration, and the molecular formula of the complex C3 is: [(o-O(C 6 h 3 )-3-allyl)CH=N)(TiCl 3 )] 2 (p-C 6 h 4 ).

[0073] The preparation process of complex C3 is the same as the preparation process of complex C1 in Example 1, the difference is only that salicylaldehyde is replaced by 3-allyl salicylaldehyde, and methanesulfonic acid is replaced by p-toluenesulfonic acid. Yield 59.6%.

[0074] 1H NMR (400HMz, DMSO): δ9.07(s, 1H, -CH=N); 3.41(d, 2H, -CH 2 ); 5.05(m,1H,=CH a ); 5.08(m,1H,=CH b ); 6.01(m,1H,=CH); 6.95(t,1H,Ar-H); 7.30(d,1H,Ar-H); 7.54(d,1H,Ar-H); 7.59(s,2H ,Ar-H). 13 C NMR (100HMz, DMSO): δ163.80, 158.48, 145.95, 136.50, 133.70, 131.17, 127.39, 122.64, 118.95, 118.60, 115.86, 33.10. 26 h 22 Cl 6 N 2 o 2 Ti 2 : C, 45.10; H, 4.33; N, 3.01.Found: C, 45.57; H, 4.30; N, 3.04.IR.(KBr, cm -1 )3359.9(m),1637.8(s),1595.3(s),1556.8(s),1491.4(w),1437.3(w),1385.2(m),1245.0(w)...

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Abstract

The invention discloses a bimetallic compound with a limited configuration as well as a preparation method and application of the bimetallic compound. The compound shown in the description has doublecenters, not only has the activity of a single-site catalyst, but also conveniently controls the electronic environments and the space environments of two metal centers through adjusting a substituentto further regulate and control the molecular weight distribution of a polymer, so that the polyolefin with a high molecular weight and wide distribution is produced, and the compound is applied to preparation of an ethylene / 1-octene copolymer; and the preparation method provided by the invention has the advantages of a short synthetic route, a simple synthetic process and low industrial costs.

Description

technical field [0001] The invention relates to the technical field of polyolefin catalysts, in particular to a constrained configuration bimetallic compound and its preparation method and application. Background technique [0002] As the core of the polyolefin industry, polyolefin catalysts have been widely concerned by academic and industrial circles at home and abroad. The FI catalyst developed by Mitsui Chemicals in 1998 is a new type of non-metallocene catalyst [Weiser M S, Thomann Y, Heinz L C, et al.Polymer.2006,47(13):4505- 4512], the catalyst structure contains ligands of phenoxyimine structure or similar structure, and the ligand structure is many, so that its steric hindrance and electronic effect can be adjusted in a wide range, thereby obtaining steric performance and electronic Catalyst with unique properties. [0003] In 2002, the FI catalyst successfully developed by Mitsui Chemicals was used to industrialize the production of new materials single-end doubl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28C07F7/00C08F10/00C08F110/02C08F210/16C08F293/00C08F4/645C08F4/656C08F4/651
CPCC07F7/003C07F7/28C08F10/00C08F110/02C08F210/16C08F293/00C08F2410/04C08F4/6457C08F4/656C08F4/651C08F2500/01C08F2500/04C08F210/14
Inventor 王林张翠余舟捷夏紫薇许胜张艺镡
Owner NANJING XIAOZHUANG UNIV
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