CN-121972236-A - Preparation method and application of module integrated type visible light catalytic carbon sheet composite material

Abstract

The invention discloses a preparation method and application of a module integrated type visible light catalytic carbon sheet composite material, which takes pretreated waste paper fiber as a carrier, and after the pretreated waste paper fiber is compounded with Fe 2 O 3 and melamine, a structured carbon sheet composite material with high specific surface area, high efficient charge separation efficiency and strong visible light response capability is successfully constructed by a program temperature control carbonization process in a nitrogen atmosphere, the process flow is simple, the raw materials are green and economical, the large-scale expansion is easy, the obtained composite material can flexibly expand a reaction interface through modularized integrated design, and the high-efficient selective reduction dechlorination of chlorophenols pollutants is realized by utilizing photo-generated electrons and active oxygen species generated by activating oxygen thereof.

Inventors

• LIANG SHENG
• YANG XIN
• HE LIANG
• ZHANG PUMING
• MA XIN
• MING QI
• DENG XIAOYONG
• WANG YINGJUN

Assignees

• 昆明理工大学

Dates

Publication Date

20260505

Application Date

20260129

Claims (9)

1. 1. The preparation method of the module integrated type visible light catalytic carbon sheet composite material is characterized by comprising the following steps of: (1) Mixing ferric nitrate nonahydrate, sodium acetate, absolute ethyl alcohol and deionized water, heating and aging the mixed solution, cooling to obtain a precipitate, washing, drying and grinding the precipitate to obtain ferric oxide powder; (2) Shredding waste paper, soaking and stirring for more than 8 hours by using deionized water, then fluffing, filtering and drying to obtain pulp fibers; (3) Adding deionized water into the pulp fibers obtained in the step (2), stirring, and pulping to a high degree to obtain fine fiber pulp; (4) Adding the ferric oxide powder and melamine in the step (3) into absolute ethyl alcohol, uniformly stirring, adding the fine fiber pulp in the step (3), stirring, dispersing, performing suction filtration molding, drying, and performing roll molding to obtain block paper fibers; (5) And (3) carbonizing the block paper fiber in the step (4) under the nitrogen atmosphere to obtain the carbon sheet composite material.
2. 2. The method for preparing the module integrated visible light catalytic carbon sheet composite material according to claim 1, wherein in the step (1), the molar ratio of ferric nitrate nonahydrate to sodium acetate is 1:14-1:15, the volume mass ratio of absolute ethyl alcohol to solute is mL:20:3-20:5, and the volume ratio of absolute ethyl alcohol to deionized water is 25:1-25:2.
3. 3. The preparation method of the module integrated type visible light catalytic carbon sheet composite material is characterized in that in the step (1), heating aging temperature is 160-180 ℃, heat preservation time is 10-12 h, washing is carried out by sequentially washing with absolute ethyl alcohol and deionized water, and drying is carried out under vacuum at 60 ℃ for 5-8 h.
4. 4. The preparation method of the module integrated type visible light catalytic carbon sheet composite material is characterized in that the mass ratio of deionized water to waste paper in the step (2) is not lower than 20:1, the fluffing is 8000-15000 turns, the drying temperature is 60-80 ℃, and the drying time is 15 hours.
5. 5. The method for preparing the module integrated type visible light catalytic carbon sheet composite material, which is characterized in that in the step (3), the volume mass ratio of deionized water to pulp fiber is mL, g is 8:1-10:1, and the pulp is highly beaten to 80-90 ° SR.
6. 6. The method for preparing the module integrated type visible light catalytic carbon sheet composite material according to claim 1, wherein in the step (4), the mass ratio of ferric oxide powder to melamine is 1:50-1:14, and the volume mass ratio of absolute ethyl alcohol to solute is 150:1-200:1.
7. 7. The preparation method of the module integrated type visible light catalytic carbon sheet composite material is characterized in that the volume mass ratio mL of absolute ethyl alcohol in the step (4) to the dry weight of fine pulp fibers in the fine fiber slurry in the step (3) is 50:1-75:2, and drying is carried out at 60 ℃ for 10 hours.
8. 8. The method for preparing the module integrated type visible light catalytic carbon sheet composite material according to claim 1, wherein in the step (5), the carbonization temperature is 500-700 ℃ under the nitrogen atmosphere, the time is 1-3 h, and the heating rate is 2.5-5 ℃ per minute.
9. 9. The carbon sheet composite material prepared by the preparation method of claim 1 is used as a photocatalyst to photodegradation organic matters in wastewater.

Description

Preparation method and application of module integrated type visible light catalytic carbon sheet composite material Technical Field The invention relates to the technical field of water pollution control and environmental catalysis, in particular to a preparation method of a module integrated visible light catalytic carbon sheet composite material Fe 2O3 @NCP and application thereof in selective reduction dechlorination of chlorophenol-containing organic pollutant wastewater. Background Chlorophenols (e.g., 4-chlorophenol, 2, 4-dichlorophenol, and 2,4, 6-trichlorophenol) are a typical and serious contaminant of interest in the paper industry, mainly from the chlorination reaction between chlorine-containing bleaching agents (e.g., clO 2) and lignin during pulp bleaching. The substances have stable chemical properties, have the characteristics of high toxicity, difficult degradation, easy bioaccumulation and the like, and once entering a water body, the substances form a long-term threat to the ecological system and human health. The strong electron-withdrawing effect of chlorine atoms in chlorophenol molecules obviously reduces the electron cloud density of benzene rings to form an electron-deficient system, so that the electron-deficient system is difficult to generate conventional electrophilic reaction, and the degradation difficulty of the traditional water treatment technology is increased. At present, although the advanced oxidation process represented by an electrochemical method, a Fenton method and a persulfate oxidation method can effectively degrade chlorophenol, the advanced oxidation process still faces a plurality of challenges in practical application, namely the reaction process usually takes ring opening and mineralization as main paths, the energy consumption is high, byproducts with stronger toxicity are easy to generate when a system containing high-concentration chloride ions is treated, and the dechlorination efficiency of the polychlorinated phenol is limited. Therefore, an economic, green and high-selectivity chlorophenol treatment technology is developed, and the method has important significance for realizing sustainable treatment of industrial wastewater. In contrast, the reductive dechlorination technology gradually converts high-toxicity chlorophenols into low-toxicity intermediates or even thoroughly mineralizes by directly breaking C-Cl bonds, and shows higher reaction selectivity and environmental friendliness. The visible light catalytic reduction dechlorination technology is driven by clean light energy, utilizes photo-generated electrons to target and attack C-Cl bond under mild conditions, has the advantages of low energy consumption, mild conditions, potential utilization of solar energy and the like, and has been paid attention to in recent years. However, the development of the technology is still limited by some key problems of the photocatalytic material, such as limited visible light response range, low photo-generated charge separation efficiency, insufficient catalytic activity, difficult material recovery, potential secondary pollution and the like. Therefore, developing a novel photocatalytic material with high visible light response, high efficient charge separation and transmission capability, excellent reduction dechlorination performance and easy separation and recovery has become a key point for pushing the technology to practical application, and is also an important research point for urgent breakthrough in the current environmental pollution control field. Disclosure of Invention Aiming at the defects of the existing chlorophenol treatment technology, the invention provides a preparation method and application of a module integrated visible light catalytic carbon plate composite material, the method takes recycled waste paper fiber as a structural substrate, by doping ferric oxide and melamine as functional precursors, the composite carbon sheet material with a multistage structure, good mechanical strength and fluffy characteristic is constructed through controllable carbonization in nitrogen atmosphere. The material shows excellent reduction dechlorination activity and circulation stability on chlorophenols pollutants in pulping and bleaching wastewater under visible light irradiation, and has good practical application potential. The invention is realized by the following technical scheme: a preparation method of a module integrated type visible light catalytic carbon sheet composite material comprises the following steps: (1) Mixing ferric nitrate nonahydrate, sodium acetate, absolute ethyl alcohol and deionized water, placing the mixed solution into a polytetrafluoroethylene lining with a stainless steel sleeve, heating, aging and cooling to obtain a precipitate, washing, drying and grinding the precipitate to obtain ferric oxide powder; (2) Shredding waste paper, soaking and stirring for more than 8 hours by using deionized water, then fluffing, f