Preparation method of Ni-based catalyst modified by aid Pt supported by multi-wall carbon nanotube as carrier and application

A multi-walled carbon nanotube, carrier-loaded technology, applied in the preparation of organic compounds, the preparation of aminohydroxy compounds, chemical instruments and methods, etc., can solve the problems of high requirements for reaction devices, catalyst corrosion, environmental pollution, etc. Mass transfer hindering effect, improving hydrogenation activity and reducing production cost

Inactive Publication Date: 2018-02-02
XIANGTAN UNIV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN1283612A discloses a supported Pt / γ-alumina-MEO catalyst, which catalyzes nitrobenzene under sulfuric acid conditions. The loading of active components is 0.5-5%. Although the selectivity of p-aminophenol can reach 70 %, the reaction is carried out under the sulfuric acid system, which needs to be neutralized with alkaline substances, which causes inconvenience to product separation, and will generate some waste water at the same time, which is more serious to environmental pollution and has a certain corrosion effect on the catalyst. Complex and large dosage, high product cost, and high content of metal oxidation waste, it is difficult to be used as medicine
Chinese patent CN103553943A discloses to use Pt / C, Pt-Sn / Al under the condition of carbon dioxide and water system 2 o 3 , Pd-CaCO 3 -PbO / PbAC 2 A series of catalysts, under the pressure of hydrogen 0.3-5MPa, carbon dioxide 0.5-10MPa, temperature 80-170 ℃, reaction time 0.5-12h, selectivity is about 5-70%, but the reaction pressure of hydrogen and carbon dioxide is relatively high , the reaction temperature is high, the reaction time is long, the requirements for the reaction device are very high, the preparation of the catalyst is complicated and the content of the active component of the catalyst is high. If the platinum carbon catalyst is used, the pores of the activated carbon are relatively deep, which is not good for the desorption of the product.
[0005] In summary, the yield of nitrobenzene in the above process routes is not very high, and some process routes have relatively harsh reaction conditions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] First prepare nitric acid mixed acid according to the volume ratio of concentrated nitric acid and concentrated sulfuric acid 3:1. Take 5g of multi-walled carbon nanotubes and place them in a 150mL round bottom flask, add a corresponding volume of nitric acid mixed acid 75mL at a solid-to-liquid mass volume ratio of 1:15g / ml, and stir at 100°C for 16 hours under constant temperature reflux. The carbon nanotubes modified by the mixed acid were repeatedly washed with deionized water until the filtrate was neutral.

[0026]Get 1g of the multi-walled carbon nanotube carrier prepared above, add 0.0218g of chloroplatinic acid hexahydrate, add 0.99g of nickel nitrate hexahydrate, put the above three substances into a 100ml beaker respectively, then add 25ml of deionized water respectively, Under the condition of 25°C, ultrasonically stir for 1h, transfer to a 100ml round bottom flask, stir for 10h at 25°C, pour the stirred solution into a 100ml beaker and put it in a blast dry...

Embodiment 2

[0028] Weigh 0.1g of the Pt-Ni / MWCNT catalyst obtained in Example 1 and place it in a 100mL inner lining of a high-temperature reactor, add 25mL of 15% 1-butyl-3-methylimidazole dihydrogen phosphate aqueous solution, 1.0 g nitrobenzene, 0.03g hexadecyltrimethylammonium bromide, put in a magnet, seal the autoclave, replace the air in the autoclave with nitrogen for 3 times, then disperse under ultrasonic conditions for 1h, and evacuate the autoclave to vacuum with a vacuum pump , and then place the reactor in an oil bath. After rising to the set reaction temperature of 95°C, hydrogen was introduced to pressurize to 1.0 MPa, magnetic stirring was started, and the reaction timing started. After reacting for 4 hours, the temperature was naturally cooled, and the content of each substance in the filtrate was analyzed by liquid chromatography. The conversion rate of nitrobenzene is 94.78%, and the selectivity of p-aminophenol is 53.68%.

Embodiment 3

[0030] Weigh 0.1g of the Pt-Ni / MWCNT catalyst obtained in Example 1 and place it in a 100mL inner lining of a high-temperature reactor, add 25mL of 15% 1-butyl-3-methylimidazole dihydrogen phosphate aqueous solution, 1.0 g nitrobenzene, 0.03g hexadecyltrimethylammonium bromide, put in a magnet, seal the autoclave, replace the air in the autoclave with nitrogen for 3 times, then disperse under ultrasonic conditions for 1h, and evacuate the autoclave to vacuum with a vacuum pump , and then place the reactor in an oil bath. After rising to the set reaction temperature of 105°C, hydrogen was introduced to pressurize to 1.0 MPa, magnetic stirring was started, and the reaction timing started. After reacting for 4 hours, the temperature was naturally cooled, and the content of each substance in the filtrate was analyzed by liquid chromatography. The conversion rate of nitrobenzene is 99.72%, and the selectivity of p-aminophenol is 61.83%.

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PUM

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Abstract

The invention discloses a preparation method of a Ni-based catalyst modified by an aid Pt supported by multi-wall carbon nanotubes as a carrier and application. The preparation method comprises the following steps: firstly, performing acid modification on multi-wall carbon nanotubes by using nitro-sulfuric acid; by taking the multi-wall carbon nanotubes as a carrier, putting precursor salts of platinum and nickel according to the multi-wall carbon nanotubes to hexachloroplatinic acid hexahydrate and nickel nitrate hexahydrate according to a mass ratio of (5-10):(0.1-0.5):(5-10); further addingdeionized water, performing ultrasonic stirring, drying, and performing roasting and reduction, thereby finally obtaining an expected catalyst Pt-Ni/MWCNT. The catalyst prepared by using the method is low in cost, economic and effective, good in universality, good in environmental-friendliness, free of equipment corrosion and good in circulation property, and is relatively high in activity and relatively high in p-aminophenol selectivity under a relative gentle reaction condition in a process that p-aminophenol is prepared from nitrobenzene through one-step hydrogenation rearrangement, the production conditions can be improved, the production cost is reduced, and the product quality is improved.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to a preparation method and application of a Ni-based catalyst modified by using multi-walled carbon nanotubes as a carrier to support Pt as an auxiliary agent. Background technique [0002] P-aminophenol (hereinafter referred to as PAP) is an important chemical raw material and organic intermediate in today's society. It is widely used in medicine, dyes, rubber and photography industries. In my country, PAP is mainly used in the pharmaceutical industry. As a pharmaceutical intermediate, PAP can be used to synthesize paracetamol (paracetamol), paracetamol, clofibrate, vitamin B1, propanol, compound agents nicotinamide, lauanol, 6- Hydroxyquinoline and other drugs, among which paracetamol is the most consumed. In the 1970s, researchers discovered that taking antipyretic and painkillers such as acetanilide and phenethyl ether would decompose into harmful components in the body. The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J35/10C07C213/00C07C215/76
CPCB01J23/892B01J35/1004C07C213/00C07C215/76Y02P20/54
Inventor 刘平乐吕扬熊伟郝芳李军罗和安
Owner XIANGTAN UNIV
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