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Supported porous metal-organic Pd catalyst, and preparation method and application thereof

A porous metal and catalyst technology, applied in the chemical industry, can solve the problems of high environmental pollution, high energy consumption in production, difficult to separate, etc., and achieve the effects of high mechanical strength, avoiding dehydrogenation reaction, and excellent activity of cyclization reaction

Active Publication Date: 2019-08-16
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many waste acids produced, the post-treatment of waste acids is troublesome, and phosphoric acid is easy to cause emulsification, difficult to separate, and high energy consumption in production.
[0007] In view of the deficiencies in the above process, it is urgent to develop a new type of catalyst for the preparation of 1,1,2,3,3-pentamethylindane, to overcome the serious corrosion of equipment and large environmental pollution in the current production. The post-processing of waste acid is troublesome, difficult to separate, and high energy consumption in production.

Method used

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  • Supported porous metal-organic Pd catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Mix 56.1g of palladium acetate and 266g of 2,2-bipyridine in 500g of distilled water, raise the temperature to 60°C and stir for 4 hours; dissolve 333.7g of copper nitrate in 500g of water to prepare a copper nitrate aqueous solution. Add the copper nitrate aqueous solution to the mixed aqueous solution of palladium acetate and 2,2-bipyridine, and add 126g of 4A molecular sieves under stirring to obtain the slurry A;

[0036] Dissolve sodium carbonate in water to form a 20wt% sodium carbonate solution, which is the alkaline precipitant B, heat the slurry A and the alkaline precipitant B to 60°C, and slowly add the alkaline precipitant B to the slurry A The pH of the system is 7.5, and the reaction temperature of the precipitation process is controlled at 60°C; then the slurry is obtained after aging at 70°C for 3 hours;

[0037] The slurry was filtered, washed with deionized water, and the filter cake was dried at 110° C. for 12 hours, calcined at 350° C. for 3 hours, cru...

Embodiment 2

[0039] Mix 67.4g of palladium acetate and 200g of 2,2-bipyridine in 500g of distilled water, raise the temperature to 60°C and stir for 4 hours; dissolve 406g of zinc acetate in 1000g of water to prepare a zinc acetate aqueous solution. Add the zinc acetate aqueous solution to the mixed solution of palladium acetate and 2,2-bipyridyl, add 155.6g of silicon dioxide under stirring and mix to obtain slurry A;

[0040] Dissolving ammonium bicarbonate in water to form a 20wt% ammonium bicarbonate solution is the alkaline precipitant B, respectively heating the slurry A and the alkaline precipitant B to 70°C, and slowly adding the alkaline precipitant B to In the slurry A until the pH of the system is 8.0, the reaction temperature of the precipitation process is controlled to 70°C; then the slurry is obtained after aging at 70°C for 3 hours;

[0041] The slurry was filtered, washed with deionized water, and the filter cake was dried at 100° C. for 10 h, calcined at 300° C. for 4 h, ...

Embodiment 3

[0043] Mix 88.6g of palladium chloride, 212.8g of 5,10,15,20-tetra(4-amino-phenyl)porphyrin in 500g of distilled water, raise the temperature to 80°C and stir for 4 hours; dissolve 167.7g of silver nitrate in 200g of water to prepare into an aqueous solution of silver nitrate. Silver nitrate aqueous solution was added to palladium chloride, 5,10,15,20-tetrakis(4-amino-phenyl)porphyrin mixed solution, and 159.5 g of neutral alumina was added under stirring to obtain slurry A;

[0044] Dissolving sodium bicarbonate in water to form a 20wt% sodium bicarbonate solution is the alkaline precipitant B, respectively heating the slurry A and the alkaline precipitant B to 60°C, and slowly adding the alkaline precipitant B to In the slurry A, the pH of the system is 8.5, and the reaction temperature of the precipitation process is controlled at 60°C; then aged at 80°C for 2 hours to obtain the slurry;

[0045] The slurry was filtered, washed with deionized water, and the filter cake was...

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Abstract

The invention discloses a preparation method of 1,1,2,3,3-pentamethylindane. The method comprises the following steps: alpha-methylstyrene and2-methyl-2-butene undergo a cycloaddition reaction under the action of a novel supported porous metal-organic Pd catalyst, and the reaction product is continuously rectified to separate the product, wherein the catalyst is represented by Pd-X-Y-Z, X is selected from Cu, Co, Fe, Zn, Ni, W, Re, Ag and Cd, Y is selected from bipyridine, porphyrin, phenanthroline, Schiff bases, triazines and benzonitrile, Z is selected from carbon nanotubes, molecular sieves, neutral alumina, ordered mesoporous carbon and silica, the mass fraction of Pd is 5-20%, X is 20-40%, Y is 30-50%, and Z is 15-45%. The method using the catalyst makes the conversion rate greater than 90% and the selectivity greater than 80%, and the catalyst is stable and is not prone to lose during the cycloaddition reaction. The method of the invention has the advantages of simplicity in operation, and good economic benefits.

Description

technical field [0001] The invention relates to a supported porous metal organic Pd catalyst, a preparation method thereof and an application in the preparation of 1,1,2,3,3-pentamethylindane, belonging to the technical field of chemical industry. [0002] technical background [0003] The fragrance industry has always needed a novel method for preparing fragrance molecules. 1,1,2,3,3-Pentamethylindane is an important intermediate for the synthesis of Carol musk. The current industrialized liquid acid-catalyzed method uses sulfuric acid, phosphoric acid Catalyst, there are unfavorable factors such as serious corrosion of equipment, large environmental pollution, and many side reactions. [0004] Chinese patent CN103772119A discloses a method for preparing 1,1,2,3,3-pentamethylindan by using a sulfuric acid catalyst to catalyze α-methylstyrene and 2-methyl-2-butene. There are many waste acids produced, troublesome post-treatment of waste acids, and high production energy cons...

Claims

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Application Information

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IPC IPC(8): B01J31/28B01J31/32B01J35/10C07C13/45C07C2/42
CPCB01J31/28B01J31/32C07C2/42B01J2231/324B01J35/394B01J35/617B01J35/635C07C13/45
Inventor 刘杰张静郭斌李文滨李晶陈来中张永振
Owner WANHUA CHEM GRP CO LTD
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