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Preparation of rhodium loaded porous siphonate carbon nitride photocatalyst, and hydrodechlorination catalytic reaction of parachlorophenol of rhodium loaded porous siphonate carbon nitride photocatalyst

A hydrodechlorination and catalytic reaction technology, applied in the preparation of organic compounds, catalysts for physical/chemical processes, and preparation of carbon-based compounds, etc., can solve problems such as incomplete oxidation, and achieve simple preparation methods, increased light radiation, chemical The effect of selective enhancement

Active Publication Date: 2019-10-29
CHONGQING TECH & BUSINESS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method is not completely oxidized and will produce more toxic chlorine intermediate pollutants

Method used

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  • Preparation of rhodium loaded porous siphonate carbon nitride photocatalyst, and hydrodechlorination catalytic reaction of parachlorophenol of rhodium loaded porous siphonate carbon nitride photocatalyst
  • Preparation of rhodium loaded porous siphonate carbon nitride photocatalyst, and hydrodechlorination catalytic reaction of parachlorophenol of rhodium loaded porous siphonate carbon nitride photocatalyst
  • Preparation of rhodium loaded porous siphonate carbon nitride photocatalyst, and hydrodechlorination catalytic reaction of parachlorophenol of rhodium loaded porous siphonate carbon nitride photocatalyst

Examples

Experimental program
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Effect test

Embodiment example 1

[0028] The preparation method of the porous tubular carbon nitride Rh / PCN of loaded rhodium shown in the embodiment of the present invention may further comprise the steps:

[0029] 1) Add 10g of melamine into a porcelain crucible, heat it to 550°C in air at a heating rate of 5°C / min and keep it for 4h to obtain PCN.

[0030] 2) Ultrasonic disperse 0.5g of pure carbon nitride in the mixed solution of ethanol and water, add rhodium chloride into the mixed solution, stir at room temperature for 24 hours, add NaBH under vigorous stirring 4 solution, lasted overnight, the solution was centrifuged, washed with water and ethanol three times, and the obtained solid was vacuum-dried to obtain a rhodium-loaded porous tubular carbon nitride photocatalyst Rh / PCN. Simultaneously prepared without NaBH 4 Reduced catalyst, abbreviated as RhCl 3 / PCN.

[0031] figure 1 is the NaBH in the above step (2) 4 The SEM image of the reduced Rh / PCN, from which it can be seen that the reduced Rh / P...

Embodiment example 2

[0035] Implementation Case 2 (response see Table 1, entry 4)

[0036] Place 5 mg of porous tubular carbon nitride supported rhodium catalyst Rh / PCN in a closed glass reaction tube, use hydrogen to replace the air in the tube several times, equip a balloon filled with hydrogen, add 5 ml of a mass concentration of 1.5 g / L 4-chlorophenol aqueous solution, The reaction temperature was controlled by a water bath at 30°C, and the reaction was performed for 30 min under the irradiation of a 30W red LED lamp. The conversion rate and product selectivity of p-chlorophenol were analyzed by GC and GC-MS. The conversion rate of 4-chlorophenol was 100.0%, and the selectivity of cyclohexanone and cyclohexanol was 52.2%.

[0037] Table 1. Condition optimization for photocatalytic 4-chlorophenol hydrodechlorination [a] .

[0038]

[0039] Implementation Case 2 (response see Table 1 entry 10)

[0040] Place 5 mg of porous tubular carbon nitride supported rhodium catalyst Rh / PCN in a close...

Embodiment example 3

[0041] Implementation Case 3 (response see Table 1 entry 11)

[0042] Place 5 mg of porous tubular carbon nitride supported rhodium catalyst Rh / PCN in a closed glass reaction tube, use hydrogen to replace the air in the tube several times, equip a balloon filled with hydrogen, add 5 ml of a mass concentration of 1.5 g / L 4-chlorophenol aqueous solution, The reaction temperature was controlled by a water bath at 30°C, and the conversion rate and product selectivity of p-chlorophenol were analyzed by GC and GC-MS after reacting for 30 min under sunlight irradiation. The conversion rate of 4-chlorophenol was 84.8%, and the selectivity of cyclohexanone and cyclohexanol was 36.1%.

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Abstract

The invention discloses preparation of a rhodium loaded porous siphonate carbon nitride photocatalyst, and a hydrodechlorination catalytic reaction of parachlorophenol of the rhodium loaded porous siphonate carbon nitride photocatalyst. The preparation method of the photocatalyst comprises the steps of taking melamine as a precursor to prepare carbon nitride by a thermal polymerization method, andthen in a mixed solution of ethyl alcohol and water (v / v 1 to 1), taking sodium borohydride as a reducing agent to prepare the rhodium loaded porous siphonate carbon nitride photocatalyst. The methodof hydrodechlorination of the parachlorophenol by photocatalyzing comprises the steps of putting a certain amount of catalyst and a certain concentration of chlorophenol aqueous solution to a glass reactor with a hydrogen balloon, reacting under illumination, and mainly generating phenol, cyclohexanone, cyclohexanol and other products. According to the preparation, the preparation method of the catalyst is simple, operation is easy, the catalyst can be used for photocatalysis chlorophenol to conduct the efficient hydrodechlorination, reaction conditions are mild, chemical selectivity of the cyclohexanol and the cyclohexanone is high, and the catalyst is easy to recycle.

Description

technical field [0001] The invention relates to the technical field of carbon nitride self-assembly and chlorophenol hydrodechlorination, and more specifically relates to the preparation of a rhodium-supported porous tubular carbon nitride photocatalyst and its hydrodechlorination catalytic reaction to chlorophenol. Background technique [0002] Chlorinated organic compounds are important chemical raw materials, widely used in the pharmaceutical industry and fuel industry, etc., and their emissions in the environment are quite large. [0003] Chlorinated organic compounds have mutagenic, carcinogenic and teratogenic effects, are difficult to degrade in the environment, and are easily accumulated by organisms. Chlorophenols are typical chlorinated organic compounds. The main treatment methods of chlorophenols are adsorption, ultrasonic, biological, advanced oxidation and chemical reduction. Among them, the advanced oxidation method converts chlorophenols into carbon dioxide,...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/02C07C29/58C07C45/51C07C35/08C07C49/403
CPCB01J27/24C07C29/58C07C45/512C07C2601/14B01J35/00B01J35/30B01J35/39C07C35/08C07C49/403Y02P20/584Y02P20/52
Inventor 蒋和雁徐洁吴豪边凤霞
Owner CHONGQING TECH & BUSINESS UNIV
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