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Preparation of supported porous nano platinum-ruthenium alloy catalyst and application of supported porous nano platinum-ruthenium alloy catalyst in preparation of chloroaniline through chloronitrobenzene hydrogenation

A technology of platinum-ruthenium alloy and p-chloronitrobenzene is applied in the field of preparation of a supported porous nano-platinum-ruthenium alloy catalyst, which can solve the problem that the conversion rate of the substrate is not high enough for the target product selectivity and the molar ratio of the active component to the substrate is low. , the reaction conditions are too mild, etc., to achieve excellent substrate conversion, excellent target product selectivity, and the effect of promoting desorption

Pending Publication Date: 2021-11-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] To sum up, for the various catalysts commonly used in current research, there are the following problems: 1. The conversion rate of the obtained substrate and the selectivity of the target product are not high enough; 2. The molar ratio of the active component to the substrate is too low, so the The amount of catalyst required is too large; 3. Most of the reaction conditions are too mild, which is not suitable for further scale-up applications; 4. Most of the reports require the use of dechlorination inhibitors, which brings difficulties to the subsequent product separation

Method used

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  • Preparation of supported porous nano platinum-ruthenium alloy catalyst and application of supported porous nano platinum-ruthenium alloy catalyst in preparation of chloroaniline through chloronitrobenzene hydrogenation
  • Preparation of supported porous nano platinum-ruthenium alloy catalyst and application of supported porous nano platinum-ruthenium alloy catalyst in preparation of chloroaniline through chloronitrobenzene hydrogenation
  • Preparation of supported porous nano platinum-ruthenium alloy catalyst and application of supported porous nano platinum-ruthenium alloy catalyst in preparation of chloroaniline through chloronitrobenzene hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Dissolve 124 mg of potassium tetrachloroplatinate and 20 mg of ruthenium trichloride hydrate in 20 mL of deionized water, and then add 0.16 g of PVP with a molecular weight of 10,000. The above solution was mixed under the condition of ultrasonic at 30°C, then 12 mL of 0.4 mol / L ascorbic acid was added, and the ultrasonic was continued for 2 h. After sonication, centrifuge, wash three times with a large amount of deionized water in an 80°C water bath, and dry under vacuum at 30°C.

[0035] (2) Weigh 13 mg of the obtained particles, disperse them in 25 mL of deionized water, then add 2 g of alumina, load for 12 h, and then vacuum-dry.

[0036] (3) Calcinate the obtained catalyst at 500°C for 10h in a nitrogen atmosphere to obtain the catalyst Pt-Ru / Al 2 o 3 .

Embodiment 2

[0038] (1) Dissolve 83 mg of potassium tetrachloroplatinate and 20 mg of ruthenium trichloride hydrate in 20 mL of deionized water, and then add 0.4 g of PVP with a molecular weight of 24,000. The above solution was mixed under the condition of ultrasonic at 30°C, and then 4 mL of 0.4 mol / L ascorbic acid was added, and the ultrasonic was continued for 6 hours. After ultrasonication, centrifuge, wash three times with a large amount of deionized water in a water bath at 40°C, and dry under vacuum at 30°C.

[0039] (2) Weigh 13 mg of the obtained particles, disperse them in 25 mL of deionized water, then add 2 g of titanium dioxide, load them for 2 hours, and then dry them in vacuum.

[0040] (3) Calcinate the obtained catalyst at 300°C for 4h in an air atmosphere to obtain the catalyst Pt-Ru / TiO 2 .

Embodiment 3

[0042] (1) Dissolve 83 mg of potassium tetrachloroplatinate and 40 mg of ruthenium trichloride hydrate in 20 mL of deionized water, and then add 0.4 g of PVP with a molecular weight of 24,000. The above solution was mixed under the condition of ultrasonic at 30°C, and then 2 mL of 0.4 mol / L ascorbic acid was added, and the ultrasonic was continued for 3 h. After ultrasonication, centrifuge, wash three times with a large amount of deionized water in a water bath at 25°C, and dry under vacuum at 30°C.

[0043] (2) Weigh 13 mg of the obtained particles, disperse them in 25 mL of deionized water, then add 2 g of activated carbon, load for 4 h, and then vacuum-dry.

[0044] (3) Calcining the obtained catalyst at 400° C. for 2 h in an air atmosphere to obtain a catalyst Pt-Ru / C.

[0045] The mapping diagram of the prepared porous nano-platinum-ruthenium alloy shows that Ru is enriched on the surface of the alloy. The ICP characterization results show that the content of Pt is much...

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Abstract

The invention provides an application of a supported porous nano platinum-ruthenium alloy catalyst in preparation of o-(m-, p-) chloroaniline by hydrogenation of o-(m-, p-) chloronitrobenzene. The catalyst takes a metal oxide or a carbon material as a carrier and a porous nano platinum-ruthenium alloy as an active component, and the porous nano platinum-ruthenium alloy is formed by mutually connecting platinum-ruthenium alloy particles; in the porous nano platinum-ruthenium alloy, ruthenium is enriched on the outer layer of the porous nano platinum-ruthenium alloy. The preparation process of the catalyst comprises the following steps: (1) preparing the porous nano platinum-ruthenium alloy; (2) loading the porous nano platinum ruthenium alloy; and (3) post-treating the catalyst. The optimized catalyst is obtained by optimizing the preparation conditions of the porous nano platinum-ruthenium alloy, screening the carrier and optimizing the operation method of post-treatment. The catalyst prepared by the invention can catalyze the hydrogenation of ortho (m, p) chloronitrobenzene to prepare ortho (m, p) chloroaniline with high conversion rate and high selectivity under the reaction conditions of no use of a dechlorination inhibitor and wide range.

Description

technical field [0001] The invention belongs to the field of noble metal catalysis, and in particular relates to a preparation method of a supported porous nano-platinum-ruthenium alloy catalyst and its application in hydrogenation of o-(m-, p-) chloronitrobenzene to prepare o-(m-, p-) chloroaniline. [0002] technical background [0003] As an important fine chemical intermediate, chlorinated aromatic ammonia is widely used in dyes, medicines, pigments and other fields. Among various methods for producing chlorinated aromatic amines, catalytic hydrogenation has attracted extensive attention due to its various advantages. For the selection of catalysts, there are mainly palladium-based, platinum-based, nickel-based and other catalysts. Because palladium itself has a strong ability to decompose hydrogen, palladium-based catalysts often lead to side reactions, which make the key chlorine groups removed. In this regard, researchers have adopted various methods to suppress the ...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J23/63C07C209/36C07C211/52
CPCB01J23/462B01J23/63C07C209/365B01J35/393B01J35/23C07C211/52
Inventor 杨洋黄家辉刘超
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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