A kind of constrained configuration double metal compound and its preparation method and application

A compound and bimetallic technology, which is applied in the field of constrained configuration bimetallic compounds and their preparation, can solve the problems of long catalyst synthesis route and expensive raw materials, achieve good catalytic activity and copolymerization ability, easy separation and purification, and simple synthesis process Effect

Inactive Publication Date: 2018-05-18
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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  • A kind of constrained configuration double metal compound and its preparation method and application
  • A kind of constrained configuration double metal compound and its preparation method and application
  • A kind of constrained configuration double metal compound and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] This example provides a constrained configuration bimetallic compound, and 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 the protection of argon, a reflux condenser was attached 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) were added to the flask. g, 0.02mol) and 120mL of ethanol, 1mL of methanesulfonic acid, heated to reflux for 6-8h, an orange-yellow solid was produced. Stop stirring, return to room temperature, filter with suction, wash the solid with ethanol, and dry to obtain an orange-yellow solid L1, 5.82 g, with a yield of 92.0%.

[0063] 1 H NMR (400MHz, d-DMSO, ppm) δ 9.03 (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,A...

Embodiment 2

[0068] This embodiment provides a constrained configuration bimetallic compound, 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, except that 3-allyl salicylaldehyde is used instead of salicylaldehyde, and benzenesulfonic acid is used instead of methanesulfonic acid. Yield 76.0%.

[0070] 1 H NMR (400HMz, DMSO): δ 9.07 (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] This embodiment provides a constrained configuration bimetallic compound, 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, except that 3-allyl salicylaldehyde is used instead of salicylaldehyde, and p-toluenesulfonic acid is used instead of methanesulfonic 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),1148.7(w),1012.5(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 restricted configuration bimetallic compound and a preparation method and application thereof. Background technique [0002] As the core of the polyolefin industry, polyolefin catalysts have always received extensive attention from academia and industry at home and abroad. The FI catalyst developed by Mitsui Chemicals in 1998, as a new class of non-metallocene catalysts with high performance for the coordination polymerization of olefins [Weiser M S, Thomann Y, Heinz L C, et al. Polymer. 2006, 47(13): 4505- 4512], its catalyst structure contains ligands of phenoxyimine structure or similar structure, and there are many ligand structures, so that its steric hindrance and electronic effects can be adjusted in a wide range, so as to obtain steric properties and electronic effects. Unique performance catalyst. [0003] In 2002, the FI catalyst successfully developed ...

Claims

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Application Information

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Patent Type & Authority Patents(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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