Composite metal photocatalysis system and preparation method and application thereof

A composite metal and photocatalysis technology, applied in the chemical industry, can solve the problems of difficult separation of catalysts, many post-processing steps, and complicated post-processing steps, and achieves the promotion of photo-generated electrons and holes separation, low overpotential and charge transfer resistance, The effect of promoting free radical cycloaddition reaction

Active Publication Date: 2020-04-10
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] Chinese patent CN106632217A mentions the method of preparing chiral (4S, 7RS) musk musk using Grignard reagent and tetramethoxysilane, etc., there are products that produce magnesium salts, silane and other pollutants, which are not friendly to the environment, and There are many post-processing steps, etc.
[0005] U.S. Patent No. 4,440,966 mentions the method for preparing 1,1,2,3,3-pentamethylindane using phosphoric acid catalysts to catalyze α-methylstyrene and 2-methyl-2-butene, and there is waste acid produced More, the post-treatment of waste acid is troublesome and the phosphorus-containing substances are not friendly to the environment, and phosphoric acid is easy to cause emulsification and is not easy to separate, etc.
[0006] In view of the deficiencies in the above-mentioned process, it is urgent to develop a novel preparation method of 1,1,2,3,3-pentamethylindane to overcome the fact that the catalyst existing in the current production process is not friendly to the environment and the product yield is low , the post-treatment steps are cumbersome, there are many pollutants, and the catalyst is not easy to separate, etc.

Method used

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  • Composite metal photocatalysis system and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 70.4g Ni(π-C 3 h 5 ) 2 , 73.4g triphenylphosphine mixed in 500g distilled water, heated to 40°C and stirred for 6h; 115.6g AgNO 3 , Mix 58.7g of diphenyl disulfide in 1000g of distilled water, raise the temperature to 50°C and stir for 7 hours, then mix the two aqueous solutions, add 58.7g of carbon nanorods in the state of stirring the mixed salt solution and mix to obtain a suspension A ;

[0037]Dissolve sodium carbonate in water to form a 20wt% sodium carbonate solution, which is the alkaline precipitant B, heat the suspension A and alkaline precipitant B to 40°C, and slowly add the alkaline solution B to the slurry A During the precipitation process, the reaction temperature was controlled at 40°C and the pH of the system was 8; after the precipitation reaction was completed, the slurry was obtained after aging at 70°C for 3 hours;

[0038] The slurry was filtered, washed with deionized water, and the filter cake was dried at 115° C. for 10 h, and calcined at 3...

Embodiment 2

[0042] 137.5g Ni(COD) 2 , 63.7g tributylphosphine mixed in 1000g distilled water, heated to 45°C and stirred for 6h; 128.8g Cd(NO 3 ) 2 1. Mix 36.8g of dicumyl peroxide in 1000g of distilled water, raise the temperature to 55°C and stir for 8h, then mix the two aqueous solutions, add 53.9g of 5A molecular sieve to mix under the state of stirring the mixed salt solution to obtain suspension A;

[0043] Dissolve sodium bicarbonate in water to form a 30wt% sodium bicarbonate solution, which is the alkaline precipitant B. Heat the suspension A and the alkaline precipitant B to 30°C, and slowly add the lye B dropwise to In the slurry A, control the reaction temperature of the precipitation process to 30°C and the pH of the system to 9; after the precipitation reaction is completed, age at 80°C for 4 hours to obtain the slurry;

[0044] The slurry was filtered, washed with deionized water, and the filter cake was dried at 120° C. for 11 h, and calcined at 350° C. for 10 h to obtai...

Embodiment 3

[0048] Mix 110.5g Ni(CDT) and 48.9g tri-tert-butylphosphine in 500g distilled water, raise the temperature to 50°C and stir for 5h; mix 107.4g SnCl 4 , Mix 29.4g of dicumyl peroxide in 1000g of distilled water, raise the temperature to 60°C and stir for 8 hours, then mix the two aqueous solutions, add 39.2g of ordered mesoporous carbon in the state of stirring the mixed salt solution and mix to obtain a suspension Liquid A;

[0049] Dissolve ammonium carbonate in water to form a 20wt% ammonium carbonate solution, which is the alkaline precipitant B, heat the suspension A and alkaline precipitant B to 35°C, and slowly add the alkaline solution B to the slurry A During the precipitation process, the reaction temperature was controlled at 35°C and the pH of the system was 9; after the precipitation reaction was completed, the slurry was obtained after aging at 80°C for 5 hours;

[0050] The slurry was filtered, washed with deionized water, and the filter cake was dried at 130° C...

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Abstract

The invention discloses a composite metal photocatalysis system which is represented by Ni-M-X-Y-Z, wherein M is selected from the group consisting of Al, Ag, Bi, Cd, Ge, Sb and Sn; x is selected fromthe group consisting of triphenylphosphine, triethylphosphine, tributylphosphine, tri-tert-butylphosphine and tricyclohexylphosphine; Y is selected from the group consisting of carbon nanorods, molecular sieves, ordered mesoporous carbon and silicon dioxide; Z is selected from the group consisting of diphenyl disulfide, dicumyl peroxide, hydrazine and 2,4-dinitrophenylhydrazine; the mass fractionof Ni is 10-20%; the mass fraction of M is 20-30%; the mass fraction of X is 20-40%; the mass fraction of Y is 15-40%,; and the mass fraction of Z is 10-30%. The catalytic system is used for preparing 1,1,2,3,3-pentamethylindane through free radical cycloaddition of alpha-methylstyrene and 2-methyl-2-butene, an conversion rate is larger than 90%, and selectivity is larger than 85%; and a catalystis stable and not prone to loss in the free radical cycloaddition reaction. A method provided by the invention is easy to operate and good in economic benefit.

Description

technical field [0001] The invention relates to a novel composite metal photocatalytic system, its preparation method and its application in the preparation of 1,1,2,3,3-pentamethylindane, belonging to the technical field of chemical industry. [0002] technical background [0003] Jiale musk is a kind of heterochromatic full-color musk successfully developed and put into production by the American International Perfume Company. It is a widely used musk-type synthetic fragrance. At present, the process of synthesizing Carole musk in my country generally has problems such as high production cost and unfriendly catalysts to the environment. 1,1,2,3,3-Pentamethylindan is an important intermediate for the synthesis of Carole musk, and its synthesis The improvement of the process is of great significance for the synthesis of Jiale musk. Therefore, it is of great significance to study new, efficient and environmentally friendly methods for synthesizing 1,1,2,3,3-pentamethylindane. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/24B01J31/02C07B61/00C07C2/42C07C13/465
CPCB01J35/004B01J35/1023B01J35/1038B01J35/1028B01J35/1042B01J31/2409B01J31/2414B01J31/24B01J31/0217B01J31/0201C07B61/02C07C2/42B01J2531/847B01J2531/17B01J2531/27B01J2531/42B01J2231/324C07C2602/08C07C13/465
Inventor 刘杰郭斌李建锋李文滨陈来中张永振
Owner WANHUA CHEM GRP CO LTD
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