Titanium catalyst as well as preparation method and application of titanium catalyst

A titanium-based catalyst and catalyst technology, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, titanium organic compounds, etc., can solve the problem that polycarbonate materials are difficult to popularize in the fields of food and medical packaging, and cannot be applied to actual industries. Production and other issues, to achieve the effect of good selectivity

Active Publication Date: 2014-12-24
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, cobalt, as a toxic metal, is strictly restricted in various international standards, making it difficult for polycarbonate materials produced by cobalt-based catalytic systems to be applied in the fields of food and medical packaging. Schiff base cobalt complex catalysts have not been able to be applied to actual industrial production

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0064] The present invention also provides a preparation method of titanium series catalyst, comprising:

[0065] 1) reacting the aldehyde compound represented by formula (VI-a) with the diamine represented by formula (VI-b) to obtain a tetradentate bis-Schiff base ligand;

[0066] Formula (VI-a), Formula (VI-b);

[0067] Among them, R 1 C1-C20 alkylene, C1-C20 alkyleneoxy, C6-C20 arylene, C6-C20 substituted arylene;

[0068] R 2 , R 3 , R 4 independently selected from: H, C1-C20 alkyl, C1-C20 alkoxy or fluorine-substituted C1-C20 alkyl,

[0069] or R 2 and R 3 and their adjacent carbons together form a closed ring;

[0070] or R 3 and R 4 and their adjacent carbons together form a closed ring;

[0071] 2) Combine tetradentate double Schiff base ligands with TiCl 3 .(THF) 3 React in the presence of a base to obtain a titanium-based catalyst.

[0072] According to the present invention, the aldehyde compound shown in formula (VI-a) is reacted with the diamine ...

Embodiment 1

[0084] Example 1: Trivalent titanium tetrahydrofuran complex TiCl 3 .(THF) 3 preparation of

[0085] Add 5.0g (25mmol) purple 3TiCl to the 100mL single-necked flask 3 .AlCl 3 , with 4 mL of refined toluene, put it into a dry ice-acetone bath at -78 ° C, and slowly drop into 5 mL of refined THF. After the dropwise addition, the system was slowly heated to 70°C and refluxed for 20 hours. After the reflux was completed, it was cooled to room temperature and filtered. The filter residue was washed three times with refined n-hexane, and the residual solvent was removed under reduced pressure to obtain 7.59 g of a light blue solid product. The yield was 82%.

[0086] By elemental analyzer, to the TiCl prepared in embodiment 1 3 .(THF) 3 Carry out analysis, its element analysis result is: C, 38.55, H, 6.64; Actual calculation result is: C, 38.68, H, 6.50; Visible, the embodiment preparation is indeed TiCl 3 .(THF) 3 .

Embodiment 2

[0087] Example 2: Preparation of complexes with the structure of formula (VII).

[0088] 4.68 g of 3,5-di-tert-butyl salicylaldehyde (20 mmol) was dissolved in 100 mL of dry ethanol, and 1.08 g of 1,2-phenylenediamine (10 mmol) was dissolved in 20 mL of dry ethanol. Then, under the condition of stirring, the ethanol solution of 1,2-o-phenylenediamine was added dropwise to the ethanol solution of 3,5-di-tert-butyl water aldehyde, heated to reflux and stirred for 14 hours, then cooled the reaction mixture to room temperature, rotated Volatile substances were removed by evaporation to obtain a solid, which was recrystallized from ethanol and dried in vacuo to obtain 5.05 g of yellow needle-shaped tetradentate bis-Schiff base ligand III with a yield of 93%.

[0089] Tetradentate double Schiff base ligand III;

[0090] Dissolve the above-mentioned tetradentate bis-Schiff base ligand III in refined 20mL THF, cool to 0°C and add 4 equivalents of NaH (60% dispersed in mineral oil),...

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Abstract

The invention provides a titanium catalyst with a structure represented by the formula (I). The catalyst can be efficiently copolymerized with a catalytic epoxy compound and carbon dioxide and is high in selectivity; furthermore, polycarbonate prepared by the catalyst provided by the invention has a non-toxic effect and can be applied to the field of food and medical packaging.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to titanium series catalysts, preparation methods and applications. Background technique [0002] Carbon dioxide is the main gas that causes the greenhouse effect, and it is also one of the most abundant carbon sources on the earth, and it is also a cheap carbon and oxygen resource. Carbon dioxide as a carbon and oxygen resource is an important research topic in the synthesis of bulk basic chemicals, fuels and polymer materials. Among them, aliphatic polycarbonate, which is copolymerized with carbon dioxide and epoxy as raw materials under the action of a catalyst, is a fully degradable polymer material with good transparency and excellent oxygen and water barrier properties. It can be used as engineering plastics, biodegradable non-polluting materials, disposable pharmaceutical and food packaging materials, adhesives and composite materials, and has wide application potential in the field...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07F7/28C08G64/34
Inventor 王勇秦玉升郭洪辰王献红王佛松
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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