Catalyst used in the catalytic hydrogenation of p-nitrophenol and its preparation method

A p-nitrophenol and catalyst technology, applied in the field of supported palladium-based amorphous alloy catalysts and its preparation, can solve problems such as uneven dispersion, and achieve the effects of simple process, low loading capacity and low cost

Active Publication Date: 2007-08-01
NANJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of catalyzer of the p-nitrophenol hydrogenation with high dispersibility, high activity supported type palladium series amorphous alloy in order to overcome the uneven dispersion of active substa

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 Amorphous alloy catalyst Pd-B / TiO 2 preparation:

[0023] At 25 °C, 1 g of TiO 2 Disperse in 9.0ml PdCl 2 (0.005M) solution, adjust the total volume of the solution to be 50ml, disperse under the action of ultrasonic waves (frequency is 80kHz), and the dispersion time is 20min; under magnetic stirring, the above-mentioned solution is vacuumized to make the vacuum reach- 0.1MPa; under the vacuum condition of -0.1MPa, continue to impregnate for 1h; in the vacuum state, quickly add 5ml of KBH dropwise 4 (0.1M) solution, keep stirring until no bubbles come out; after the reaction, filter and wash with water until there is no Cl - present; washed twice with ethanol. Catalyst No. S-1

Embodiment 2

[0038] The temperature of vacuum reduction was changed to 0° C., and other conditions were the same as in Example 1. Activity evaluation results showed that its H 2 The consumption rate was 20.65 mmol / g / min.

Embodiment 3

[0040] Preparation of Amorphous Alloy Pd-B / MCM-41

[0041] At room temperature, 1 g of MCM-41 was dispersed in 2.4 ml of Pd(AC) 2(0.01M) solution, adjust the total volume of the solution to be 40ml, disperse under the action of ultrasonic waves (frequency is 40kHz), and the dispersion time is 1h; under magnetic stirring, the above-mentioned solution is vacuumized to make the vacuum reach -0.05MPa; under the vacuum condition of -0.05MPa, continue to impregnate for 8h; in the state of vacuum, quickly drop 5ml NaBH 4 (0.25M) solution, keep stirring until no bubbles emerge; filter, wash with water and ethanol for 3 times respectively. Activity evaluation results showed that its H 2 The consumption rate was 17.89 mmol / g / min.

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Abstract

The invention involves a load palladium amorphous alloy catalyst used for nitrophenol hydrogenation and preparation method and belongs to catalyst technology field. Said catalyst uses NaY, MCM-41, molecular screen, Al2O3, TiO2, SiO2 or MgO as carrier, and is loaded with Pd-B amorphous alloy, the quality of Pd is 0.1-0.5% of toatl quality of catalyst. The preparation process includes ultrasonic dispersion, vacuum impregnation, KBH4 chemical reduction under vacuum conditions, filtration and washing of carriers; it is characterized by introducing vacuum and ultrasonic radiation conditions. The advantages of the invention lies in its high activity of catalyst, low preparation cost and simple preparation process, it could widely apply to the preparation of p-aminophenol through nitrophenol catalysis and hydrogenation.

Description

technical field [0001] The invention relates to a catalyst for hydrogenation of p-nitrophenol and a preparation method thereof, in particular to a supported palladium-based amorphous alloy catalyst for hydrogenation of p-nitrophenol and a preparation method thereof. Background technique [0002] p-Aminophenol is an important intermediate in fine chemical industry, especially in synthetic medicine. Chemical reduction is one of the main methods for preparing aromatic amines. The reduction method of p-nitrophenol iron powder is a traditional preparation method, but this method not only has a low yield, but also produces a large amount of waste residue (iron sludge) and waste water to pollute the environment, and has been eliminated in developed countries. The electrolytic reduction method disclosed in patents CN1061808, CN1064900, CN1101951, CN1342785 and CN1429932 uses nitrobenzene as a raw material to directly electrolytically reduce p-aminophenol. Patents CN1087623A, CN128...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J21/02B01J32/00C07C213/02C07C215/76
Inventor 徐南平马振叶张利雄陈日志邢卫红
Owner NANJING UNIV OF TECH
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