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Preparation method and application of copper/silicon oxide xerogel catalyst

A technology of dry gel catalyst and silicon oxide, which is applied in the preparation of organic compounds, chemical instruments and methods, preparation of amino hydroxyl compounds, etc., to achieve the effects of improved catalytic activity, low equipment requirements, and good stability

Inactive Publication Date: 2017-04-26
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cu-SiO prepared by sol-gel method 2 There are still reports on the use of xerogel catalysts to catalyze the hydrogenation of p-nitrophenol

Method used

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  • Preparation method and application of copper/silicon oxide xerogel catalyst
  • Preparation method and application of copper/silicon oxide xerogel catalyst
  • Preparation method and application of copper/silicon oxide xerogel catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) At room temperature, weigh 7.9172g of zirconium oxychloride octahydrate and add it to 9mL of absolute ethanol, stir and mix well to obtain mixed solution A;

[0043] (2) Weigh 0.76g of copper nitrate trihydrate and add it to 3mL of deionized water, stir until uniform to obtain mixed solution B;

[0044] (3) The mixed solution B was slowly added dropwise to the mixed solution A, and after reacting for 8 hours under magnetic stirring, the stirring was stopped to obtain the mixed solution C;

[0045] (4) Measure 1 mL of nitric acid and slowly add it to the mixed solution C drop by drop, stir for 5 minutes, stop stirring, and wait for gelation at room temperature;

[0046] (5) The wet gel obtained in step (4) was aged in the air for 10 hours, then dried in a vacuum oven at 60°C for 24 hours, and then dried at normal pressure: first dried at 60°C for 4 hours, then at 80°C for 2 hours, and finally at 120°C Dry at ℃ for 2h;

[0047] (6) Calcinate the massive solid obtain...

Embodiment 2

[0055] (1) At room temperature, weigh 8.709g of zirconium oxychloride octahydrate and add it to 9mL of absolute ethanol, stir and mix well to obtain mixed solution A;

[0056] (2) Weigh 0.076g of copper nitrate trihydrate and add it to 3mL of deionized water, stir until uniform to obtain mixed solution B;

[0057] (3) The mixed solution B was slowly added dropwise to the mixed solution A, and after reacting for 8 hours under magnetic stirring, the stirring was stopped to obtain the mixed solution C;

[0058] (4) Measure 1 mL of nitric acid and slowly add it to the mixed solution C drop by drop, stir for 3 minutes, stop stirring, and wait for gelation at room temperature;

[0059] (5) The wet gel obtained in step (4) was aged in the air for 10 hours, then dried in a vacuum oven at 45°C for 24 hours, and then dried at normal pressure: first dried at 60°C for 4 hours, then at 80°C for 2 hours, and finally at 120°C Dry at ℃ for 2h;

[0060] (6) Calcinate the massive solid obtain...

Embodiment 3

[0062] (1) At room temperature, weigh 7.4774g of zirconium oxychloride octahydrate and add it to 9mL of absolute ethanol, stir and mix well to obtain mixed solution A;

[0063] (2) Weigh 0.8048g cupric chloride dihydrate and add it to 5mL deionized water, stir until uniform to obtain mixed solution B;

[0064] (3) The mixed solution B was slowly added dropwise to the mixed solution A, and after reacting for 10 h under magnetic stirring, the stirring was stopped to obtain the mixed solution C;

[0065] (4) Measure 1.5mL of nitric acid and slowly add it to the mixed solution C dropwise, stir for 5min, stop stirring, and wait for gelation at room temperature;

[0066] (5) The wet gel obtained in step (4) was aged in the air for 12 hours, then dried in a vacuum oven at 60°C for 24 hours, and then dried at normal pressure: first dried at 60°C for 4 hours, then at 80°C for 2 hours, and finally at 120°C Dry at ℃ for 2h;

[0067] (6) Calcinate the massive solid obtained in step (5) ...

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Abstract

The invention belongs to the field of energy chemical industry and discloses a preparation method and an application of a copper / silicon oxide xerogel catalyst. The preparation method includes the steps of: 1) at room temperature, adding tetraethyl orthosilicate to anhydrous ethanol, and fully stirring and mixing the components; 2) adding a copper salt to deionized water, stirring the mixture uniformly, dropwise slowly adding the mixture to a silicon solution, magnetically stirring the mixed solution for 8-10 h and stopping stirring; 3) dropwise slowly adding nitric acid to the mixed solution, stirring the solution for 3-5 min, stopping stirring and allowing the solution to stand at room temperature to await gelatinization; 4) aging the gel in air, vacuum-drying and normal-pressure-drying the gel, calcining the gel in air and feeding H2 / Ar mixed gas to reduce the gel to prepare the copper / silicon oxide xerogel catalyst. The method is simple, is low in raw material cost, is low in demand on equipment, is free of pollution during synthesis and is environment-friendly, and is suitable for industrial production. The catalyst can be used for catalytically reducing paranitrophenol to prepare p-aminophenol at room temperature with water as a solvent and sodium borohydride as a hydrogen source. The process is low in usage amount of catalyst, is short in reaction time, and is high in conversion rate.

Description

technical field [0001] The invention relates to a copper / silicon oxide xerogel and a preparation method thereof, belonging to the field of energy and chemical industry. Background technique [0002] Para-nitrophenol (PNP) is a non-biodegradable and toxic environmental pollutant, while para-aminophenol (PAP) is an important chemical raw material and pharmaceutical intermediate. With the increase in the demand for para-aminophenol, the use of The direct catalytic hydrogenation of p-nitrophenol to p-aminophenol has become the main synthetic route because of its high efficiency and environmental protection. [0003] Catalysts used in the catalytic hydrogenation of p-nitrophenol generally include noble metal catalysts (Au, Pt, Pd, Ru, Rh), and non-noble metal nickel-based catalysts (Ni). Precious metal catalysts have good catalytic activity and high temperature stability, but the production cost is high, and they are easy to sinter during use, and the recovery rate is low, so in...

Claims

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Application Information

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IPC IPC(8): B01J23/72C07C213/02C07C215/76
CPCB01J23/72C07C213/02C07C215/76
Inventor 谢吉民张银龙冯金范东亮朱建军汪强马丽蓉阮义杰宋佳宁
Owner JIANGSU UNIV