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Catalytic agent for preparing p-aminophenol by using nitrobenzene catalytic hydrogenation and preparation method thereof

A technology for catalytic hydrogenation of p-aminophenol, which is applied in the preparation of amino hydroxyl compounds, organic compounds, metal/metal oxide/metal hydroxide catalysts, etc., and can solve the problems of poor selectivity of PAP, carrier loss, and intolerable electrode materials Corrosion and other problems, to achieve the effect of improved activity and selectivity, good catalytic performance, and good hydrogen absorption effect

Inactive Publication Date: 2012-09-12
ANHUI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The p-aminophenol synthetic method disclosed in US6403833 and CN1075489C has used nickel / ZSM-5 or Pt / nylon, although catalytic stability is better, but the selectivity of PAP is poor
In CN1562465A, Pt is loaded on the acidic bifunctional carrier, and there is a problem that the carrier is dissolved and lost by the acidic solution, and the life of the catalyst is unstable
CN1061808A electrolytically reduces nitrobenzene in acidic medium to generate p-aminophenol without using expensive catalysts. The disadvantage of this method is that the electrode material is difficult to resist corrosion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Immerse 40-60g of activated carbon purified by nitric acid in 15-20ml of chloroplatinic acid aqueous solution with a volume concentration of 4-8%, keep the temperature at 50°C for 4-6h, and cool to 20°C; prepare saturated aqueous sodium carbonate solution , adjust the impregnation solution to be alkaline; add excess hydrazine hydrate dropwise while stirring, and then keep warm on a water bath for 1-4 hours to completely reduce the chloroplatinic acid; filter the solid phase components, wash with deionized water until there is no chloride ion, Place in a vacuum dryer and dry to obtain 40-60g of Pt / C catalyst, which is ready for use; dissolve 8-12g of ammonium tetrathiomolybdate crystals (ATTM) in deionized water, add spare Pt / C, and stir magnetically under immersion conditions 1-3h, stand still for 4-8h, and dry at 60-90°C to obtain the catalyst precursor ATTM-Pt / C(I); put ATTM-Pt / C(I) into a quartz tube and place it in a tube furnace Medium roasting, the temperature is ...

Embodiment 2

[0022] In a stirred reactor at normal pressure, add 100ml of distilled water, 10ml of concentrated sulfuric acid with a mass fraction of 98%, 0.05ml of dimethyl sulfoxide, and 0.3g of MoS 2 - Pt / C catalyst, 20ml nitrobenzene. Pass N 2 , replace the air in the device, and check the airtightness. Heat up to about 87°C, keep the temperature constant, pass H 2 . Stop heating after 5 h of reaction, pass N 2 Purge, cool to room temperature, and recover the catalyst. According to GC-MS analysis, the yield of p-aminophenol is 86%.

Embodiment 3

[0024] Using the catalyst in Example 2, the reaction conditions were the same as above, and after 22 cycles, the yield of p-aminophenol in the 23rd reaction solution was determined to be 83%.

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Abstract

The invention relates to a novel catalytic agent for preparing p-aminophenol by using nitrobenzene catalytic hydrogenation and a preparation method thereof. The catalytic agent enables active carbon to serve as a carrier, enables Pt to serve as a main catalytic agent and enables MoS2 to serve as an auxiliary catalytic agent. The preparation step of the catalytic agent comprises (1) preparing Pt / C catalytic agent, namely enabling the Pt to be loaded on the activated carbon through an infusion process; and (2) restoring the auxiliary catalytic agent MoS2 through steeping and roasting under certain H2, loading on the Pt / C, and finally obtaining the catalytic agent for preparing the p-aminophenol. The catalytic agent for synthesizing the p-aminophenol is high in productivity and high in selectivity, and the catalytic agent is good in stability. After 23 times of circulation, the catalytic agent keeps good activity, yield coefficient of the p-aminophenol is above 83%, and the catalytic agent has good industrial application prospect.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a catalyst for preparing p-aminophenol from nitrobenzene and a preparation method thereof. Background technique [0002] P-aminophenol (abbreviated as PAP) is a widely used intermediate in organic synthesis. The traditional production route is the chlorobenzene route. Chlorobenzene is nitrated to obtain p-nitrochlorobenzene, then hydrolyzed to obtain p-nitrophenol, and finally undergoes a reduction method (iron powder, alkali sulfide or hydrogen) and other three-step chemical reactions and a series of separations. Process for the production of p-aminophenol. [0003] The route using nitrobenzene as a raw material, first, nitrobenzene is reduced by zinc powder, electrolysis or catalytic hydrogenation to generate p-hydroxyaniline, which can be directly rearranged by Bamberge to generate p-aminophenol under acidic conditions without separation. Among them, due to the low yield a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42C07C215/76C07C213/00
Inventor 李广学姜丰李家鸣卜佳赵明珠褚杨詹华露
Owner ANHUI UNIV OF SCI & TECH
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