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Preparation method of Pt-C (platinum-carbon) catalyst for nitrobenzene hydrogenation

A catalyst, a technology for nitrobenzene, which is applied in the reaction field of hydrogenation reduction of nitrobenzene to generate p-aminophenol, can solve the problems of catalyst poisoning, low catalyst activity, etc., and achieves improved adsorption capacity, high catalytic activity and strong Coulomb effect. Effect

Inactive Publication Date: 2014-02-05
昆明贵研催化剂有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Many domestic manufacturers have started to develop the catalytic hydrogenation process of nitrobenzene, but the situation is not ideal. The main problems are catalyst poisoning, low catalyst activity, recovery and regeneration of Pt, etc.

Method used

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  • Preparation method of Pt-C (platinum-carbon) catalyst for nitrobenzene hydrogenation
  • Preparation method of Pt-C (platinum-carbon) catalyst for nitrobenzene hydrogenation
  • Preparation method of Pt-C (platinum-carbon) catalyst for nitrobenzene hydrogenation

Examples

Experimental program
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Effect test

example 1

[0017] Example 1: Accurately weigh 5 kg of modified activated carbon, add 50 L of distilled water, and stir for 3 hours to obtain suspension A of activated carbon. At the same time, the prepared ethanolamine hydroxyplatinum containing 0.100 kg of Pt was dissolved in 1 L aqueous solution containing 0.365 kg of sodium dodecylbenzenesulfonate, and stirred for about 5 hours to completely disperse the platinum precursor to obtain solution B. Then, pass hydrogen gas into solution B through an aeration device similar to a sand core funnel and control the gas intake rate to 50-60ml / min for about 10 minutes. At this time, the color of the solution is dark brown, and the aeration is stopped to obtain hydrosol C. Add A to the C system, stir for about 24 hours, so that the active component Pt is completely adsorbed on the surface of the carrier in the form of particles and ions; then use a micro peristaltic pump to dissolve 0.255kg Sodium borohydride solution (according to the mass ratio ...

example 2

[0018] Example 2: Accurately weigh 5 kg of modified activated carbon, add 50 L of distilled water, and stir for 3 hours to obtain suspension A of activated carbon. At the same time, the prepared ethanolamine hydroxyplatinum containing 0.150 kg of Pt was dissolved in 1 L aqueous solution containing 0.554 kg of sodium dodecylbenzenesulfonate, and stirred for about 5 hours to completely disperse the platinum precursor to obtain solution B. Then, through an aeration device similar to a sand core funnel, inject hydrogen into B and control the intake rate to 50-60ml / min for about 10 minutes. At this time, the color of the solution is dark brown, stop the aeration to obtain hydrosol C; add A to C In the system, stirring for about 24h, the active component Pt is completely adsorbed on the surface of the carrier in the form of particles and ions, and then the 0.388kg sodium borohydride solution ( According to the mass ratio of ethanolamine hydroxyplatinum: sodium hydroxide = 1:1.5, add...

example 3

[0019] Example 3: Accurately weigh 5 kg of modified activated carbon, add 50 L of distilled water, and stir for 3 hours to obtain suspension A of activated carbon. At the same time, the prepared ethanolamine hydroxyplatinum containing 0.200kg of Pt was dissolved in 1L aqueous solution containing 0.743kg of sodium dodecylbenzenesulfonate, and stirred for about 5 hours to completely disperse the platinum precursor to obtain solution B. Then, pass hydrogen into solution B through an aeration device similar to a sand core funnel and control the gas intake rate to 50-60ml / min for about 10 minutes. At this time, the color of the solution is dark brown, stop the aeration to obtain hydrosol C; add A to In system C, stir for about 24 hours, so that the active component Pt is completely adsorbed on the surface of the carrier in the form of particles and ions, and then use a micro peristaltic pump to dissolve 0.520kg of sodium borohydride solution in 1L of water at a flow rate of 10ml / min...

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Abstract

The invention discloses a preparation method of a Pt-C (platinum-carbon) catalyst for nitrobenzene hydrogenation, which is applied to a high-activity Pt-C catalyst for nitrobenzene hydrogenation reduction to generate p-aminophenol. In order to avoid the problems of chloride oil poison and the like in the preparation of a catalyst by taking chloroplatinic acid as a precursor, ethanolamine hydroxyl platinum is used as a precursor; meanwhile, sodium dodecyl benzene sulfonate is used as a protective agent to control the particle size of the Pt particles and is prepared through two-step reduction by H2 and NaBH4. The dispersity of the active component Pt particles is good, the mass percentage is 2-5%, and the particle size of the particles is less than or equal to 5nm. The catalyst prepared by the method shows perfect catalytic activity and reaction selectivity in a reaction of generating p-aminophenol through nitrobenzene hydrogenation, wherein the conversion rate is 99.09%, and the selectivity reaches 92%.

Description

technical field [0001] The invention relates to a preparation method of a woody powdery platinum carbon catalyst for organic hydrogenation reaction. The catalyst prepared by the method is especially suitable for the reaction of nitrobenzene hydrogenation reduction to generate p-aminophenol. Background technique [0002] Para-aminophenol (PAP for short) is an important raw material for organic synthesis, and the global annual consumption in the pharmaceutical and rubber industries alone reaches hundreds of thousands of tons. In addition, it is also widely used in dyes, developing and anti-oxidation (Liu Suying, Wang Xudong. Development and application of p-aminophenol. Shijiazhuang Chemical Industry. 1995(2):22-25). In the pharmaceutical industry, PAP is also a synthetic intermediate of 4 to 5 common drugs. [0003] At present, there are three main process routes for producing PAP with nitrobenzene as the starting material: the reduction method of light and heavy metals, the...

Claims

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Application Information

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IPC IPC(8): B01J23/42B01J37/16C07C215/76C07C213/00
Inventor 顾永万刘锋栗云彦张慧峰覃庆高张爱敏白屏张彦明赵云昆
Owner 昆明贵研催化剂有限责任公司
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