Tridentate Schiff base titanium-based olefin polymerization catalyst and preparation method and application thereof

A Schiff base titanium-based olefin and polymerization catalyst technology, applied in the direction of titanium organic compounds, etc., can solve the problems of uncontrollable polymer structure and performance, and achieve the effects of high yield, simple synthesis route and good catalytic activity

Inactive Publication Date: 2013-02-20
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this kind of solid catalyst with multiple active sites cannot control the

Method used

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  • Tridentate Schiff base titanium-based olefin polymerization catalyst and preparation method and application thereof
  • Tridentate Schiff base titanium-based olefin polymerization catalyst and preparation method and application thereof
  • Tridentate Schiff base titanium-based olefin polymerization catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 Preparation of 1,3-dimethyl-5-acetyl-barbituric acid (DAB)

[0026] The structural formula of 1,3-dimethyl-5-acetyl-barbituric acid (DAB) is:

[0027]

[0028] Put 6.40 grams of 1,3-dimethylbarbituric acid and 150 ml of acetic anhydride into a dry round-bottomed flask, add 5 drops of concentrated sulfuric acid dropwise under the condition of vigorous stirring, distill the acetic anhydride after reflux for 2 hours, cool The precipitated solid was washed successively with hot water and acetone, and vacuum-dried to obtain 5.90 g of yellow powder with a yield of 65%. (T. Arai et al., Org. Lett., 2007, 9, 3595)

Embodiment 2

[0029] Example 2 Preparation of unilaterally protected diphenylethylenediamine

[0030] The structural formula of unilaterally protected diphenylethylenediamine is:

[0031]

[0032] Under nitrogen protection, 2 g of diphenylethylenediamine, 1.87 g of DAB, and 20 ml of anhydrous tetrahydrofuran were added, and stirred at room temperature for 48 hours. After removal of the solvent, column chromatography yielded 3.14 g of a white solid with a yield of 94%. (T. Arai et al., Org. Lett., 2007, 9, 3595)

Embodiment 3

[0033] Example 3 Preparation of 1,2-diphenyl-1-isoindolyl-2-amine-DAB

[0034] The structural formula of 1,2-diphenyl-1-isoindolyl-2-amine-DAB is:

[0035]

[0036] Add 2.27 grams of unilaterally protected diphenylethylenediamine, 1.76 grams of o-dibenzyl bromide, 2ml of diisopropylethylenediamine, and 20ml of N,N-dimethylformamide under nitrogen protection, and stir at 40°C for 48 After one hour, water was added to stop the reaction, and the product was extracted with ethyl acetate. After removal of the solvent, column chromatography gave 2.39 g of a yellow solid, with a yield of 78%.

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Abstract

The invention belongs to the technical field of chemical catalysts and specifically provides a tridentate Schiff base titanium-based olefin polymerization catalyst and a preparation method and application thereof. Diphenyl ethylenediamine obtained through modification and substituted salicylaldehyde perform condensation reaction to synthesize an N,N,O tridentate organic ligand, strong base is used to perform dehydrogenation treatment and then react with titanium tetrachloride, and accordingly a monometallic-centered titanium olefin polymerization catalyst is formed. A component expression of the catalyst is [Comp(M-NNO)], wherein the Comp represents a complex, the M represents an early-transition metal titanium, and the NNO represents substituted Schiff base type nitrogen, nitrogen and oxygen ligand. The catalyst has high catalytic activity on olefin polymerization, and the catalytic effect of a catalytic system can be improved obviously after carbon-nitrogen double bonds are reduced to be a single bond.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysts, and in particular relates to a preparation method of an olefin polymerization catalyst system and its application in ethylene polymerization. Background technique [0002] Since the discovery of the Ziegler-Natta catalyst in the 1950s, highly active MgCl 2 The supported titanium catalyst shows good catalytic performance. The application of this catalyst simplifies the production process, thereby saving energy and raw materials, and improving the performance of the polymer (K. Ziegler, et al., Angew. Chem. 1995, 67, 424 ; K. Ziegler et al., Angew. Chem. 1995, 67, 541). Industrially, this catalyst has been used in the production of polymers of high-density polyethylene (HDPE), linear low-density ethylene (LLDPE), and syndiotactic polypropylene (i-PP). However, this kind of solid catalyst with multi-active sites cannot control the structure and performance of the polymer by adjusting th...

Claims

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Application Information

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IPC IPC(8): C08F10/02C08F4/64C07F7/28
CPCC08F10/02C08F4/64C08F10/00C08F4/64117
Inventor 张道万莉王全瑞
Owner FUDAN UNIV
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