WO2021120467A1 - 一种氮改性钙钛矿复合分子筛的光催化剂及其制备方法与应用方法 - Google Patents

一种氮改性钙钛矿复合分子筛的光催化剂及其制备方法与应用方法 Download PDF

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WO2021120467A1
WO2021120467A1 PCT/CN2020/084904 CN2020084904W WO2021120467A1 WO 2021120467 A1 WO2021120467 A1 WO 2021120467A1 CN 2020084904 W CN2020084904 W CN 2020084904W WO 2021120467 A1 WO2021120467 A1 WO 2021120467A1
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photocatalyst
nitrogen
molecular sieve
composite molecular
perovskite composite
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PCT/CN2020/084904
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English (en)
French (fr)
Chinese (zh)
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吴敏
刘颖
厉明升
王传传
李志豪
赵颖丹
张仲琨
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东南大学
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
    • B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
    • B01J29/76—Iron group metals or copper
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/005—Spinels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/64—Pore diameter
    • B01J35/647—2-50 nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
    • B01J2229/10—After treatment, characterised by the effect to be obtained
    • B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C02F2101/345—Phenols
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Definitions

  • the invention relates to a photocatalyst and a preparation method and application thereof, in particular to a photocatalyst of a nitrogen-modified perovskite composite molecular sieve and a preparation method and application thereof.
  • Aromatic compounds are a class of compounds with a benzene ring structure. They have a stable structure, are difficult to decompose, and are highly toxic. Aromatic compounds come from the lignin and secondary metabolic processes of higher plants on the one hand, and on the other hand come from various chemical products synthesized in industry, such as pesticides, herbicides, dyes, explosives and so on. Aromatic compounds such as benzene, benzonitriles, and phenols are being produced in the amount of one million tons per year. These compounds are widely used in fuels and industrial solvents, and they, together with polycyclic aromatic compounds and chlorinated biphenyls, are used in the production of medicines. , Pesticides, plastic polymers, explosives and other daily necessities.
  • the existing treatment methods for aromatic wastewater mainly include physical treatment, chemical treatment, biological treatment and other methods such as low-temperature plasma technology, nano-photocatalytic technology, etc.
  • biodegradation method has a mature treatment process and low cost, it is only suitable for the treatment of low-concentration aromatic compounds; chemical oxidation and advanced oxidation technology methods refer to adding a certain amount of oxidants (oxygen, hydrogen peroxide, Ozone, etc.), under certain conditions, a strong oxidant is produced, which makes the aromatic compounds be oxidized and degraded, and finally completely mineralized into carbon dioxide and water.
  • oxidants oxygen, hydrogen peroxide, Ozone, etc.
  • the adsorption method is a more effective method for the treatment of aromatic compounds, mainly using porous materials to adsorb pollutants in the wastewater.
  • the pollutants in the adsorbent will enter the inside of the adsorbent through the pore structure of the adsorbent, and then the adsorbent can be treated to a certain extent, so that the adsorbent can be recycled.
  • cold plasma treatment of wastewater is a new wastewater treatment technology that combines high-energy electron radiation, ozone oxidation, and ultraviolet photolysis.
  • nano-photocatalytic technology has mild reaction conditions, can use ultraviolet light and sunlight and other conditions, directly and indirectly pollutants into CO2, water and other harmless substances, and consumes little energy and does not produce Secondary pollution.
  • Commonly used photocatalysts such as TiO2 have wide band gap, can not make full use of visible light, low quantum efficiency and other shortcomings, while perovskite catalyst has narrow band gap and small band gap, it is a better photocatalyst, but calcium Titanium ore has the problem of high electron-hole recombination rate, and does not respond well to a wide range of visible light.
  • the first object of the present invention is to provide an efficient, convenient, energy-saving and environmentally friendly nitrogen-modified perovskite composite molecular sieve photocatalyst.
  • the second object of the present invention is to provide a method for preparing the photocatalyst.
  • the third objective is to provide the application of the photocatalyst.
  • the photocatalyst of the nitrogen-modified perovskite composite molecular sieve of the present invention is N-LaFeO 3 @MCM-41.
  • the preparation method of the photocatalyst of the present invention includes the following steps:
  • step (1) a soft template agent is added to the A solution.
  • the soft template is cetyltrimethylammonium bromide (CTAB), which controls the size of the material and increases the specific surface area of the material.
  • CTAB cetyltrimethylammonium bromide
  • the complexing agent is any one of tartaric acid, malic acid, aspartic acid or lactic acid.
  • the aromatic compound is one of benzonitrile, p-methoxybenzonitrile, terephthalonitrile or bisphenol A.
  • the application of the photocatalyst of the present invention includes the following steps: adding a photocatalyst, a hole trapping agent, and aromatic compound organic wastewater to a photocatalytic reactor to perform a photocatalytic reaction, wherein the hole trapping agent and the aromatic
  • the volume ratio of the compound is 1:8-16, and the dosage of the photocatalyst per liter of the mixture of the hole trapping agent and the aromatic compound is 0.2-0.6g.
  • dark adsorption is performed before the photocatalytic reaction.
  • the hole trapping agent is one of methanol or ammonium oxalate.
  • the photocatalytic reaction provides visible light through a xenon lamp.
  • the photocatalyst of the present invention uses nitrogen-modified perovskite to reduce the forbidden band width of the catalyst and increase the visible light absorption area, thereby improving the efficiency of degrading aromatic compound organic wastewater; using molecular sieve MCM-41 as a carrier, Significantly increase the contact area between the catalyst and organic wastewater, and promote rapid catalytic degradation;
  • the preparation method of the photocatalyst of the present invention is easy to operate and has low cost; the method has simple equipment, flexible process, high purity of the material and easy control of the particle size; the method can use chemical reactions in the solution to make the raw materials at the molecular level Uniform mixing, so as to obtain a product with high uniformity, the uniformity of which can reach the size of molecules or atoms;
  • the photocatalyst of the present invention does not use various oxidants during the application process, and there is no need to worry about the problem of oxidant recovery, which greatly saves costs; does not produce sludge and secondary pollution; reacts under low temperature and normal pressure, and makes full use of visible light, saving energy.
  • Figure 1 shows the photocatalytic degradation mechanism of the present invention.
  • N-LaFeO 3 @MCM-41-1 catalyst methanol and bisphenol A wastewater to the photocatalytic reactor for photocatalytic reaction.
  • the volume ratio of methanol and bisphenol A wastewater is 1:8, per liter of methanol and bisphenol
  • the dosage of the photocatalyst in the mixture of wastewater A is 0.2g; first carry out the dark adsorption reaction for 30 minutes, after reaching the adsorption equilibrium, then provide visible light through the xenon lamp, and carry out the catalytic reaction at room temperature. At the same interval, take the supernatant and pass After 0.45 ⁇ m filter membrane, it was determined that the removal rate of bisphenol A reached more than 90% and the COD removal rate in the reaction system was 90%.
  • N-LaFeO 3 @MCM-41-2 catalyst methanol and benzonitrile wastewater to the photocatalytic reactor for photocatalytic reaction.
  • the volume ratio of methanol and benzonitrile wastewater is 1:16, which is equivalent to that per liter of methanol and benzonitrile wastewater.
  • the dosage of the photocatalyst in the mixture is 0.6g; first carry out the dark adsorption reaction for 30 minutes, after reaching the adsorption equilibrium, then provide visible light through the xenon lamp, and carry out the catalytic reaction at room temperature. At the same interval, take the supernatant and filter through 0.45 ⁇ m. After the membrane, it was determined that the removal rate of benzonitrile reached more than 90% and the COD removal rate in the reaction system was 92%.
  • N-LaFeO 3 @MCM-41-3 catalyst methanol and p-methoxybenzonitrile wastewater into the photocatalytic reactor for photocatalytic reaction.
  • the volume ratio of methanol and p-methoxybenzonitrile wastewater is 1:12.
  • the dosage of photocatalyst per liter of the mixture of methanol and p-methoxybenzonitrile wastewater is 0.4g; first carry out 30min dark adsorption reaction, after reaching adsorption equilibrium, then provide visible light through xenon lamp to carry out catalytic reaction, the same interval time period After taking the supernatant and passing through a 0.45 ⁇ m filter membrane, it was determined that the removal rate of p-methoxybenzonitrile reached more than 90% and the COD removal rate in the reaction system was 91%.
  • N-LaFeO 3 @MCM-41-4 catalyst methanol and bisphenol A wastewater to the photocatalytic reactor for photocatalytic reaction.
  • the volume ratio of methanol and bisphenol A wastewater is 1:8, per liter of methanol and bisphenol
  • the dosage of the photocatalyst in the mixture of A wastewater is 0.2g; first carry out the dark adsorption reaction for 30 minutes, after reaching the adsorption equilibrium, then provide visible light through the xenon lamp, and carry out the catalytic reaction at room temperature. At the same interval, take the supernatant and pass After 0.45 ⁇ m filter membrane, it was determined that the removal rate of bisphenol A reached more than 90% and the COD removal rate in the reaction system was 91%.
  • N-LaFeO 3 @MCM-41-5 catalyst methanol and bisphenol A wastewater to the photocatalytic reactor for photocatalytic reaction.
  • the volume ratio of methanol and bisphenol A wastewater is 1:8, per liter of methanol and bisphenol
  • the dosage of the photocatalyst in the mixture of A wastewater is 0.2g; first carry out the dark adsorption reaction for 30 minutes, after reaching the adsorption equilibrium, then provide visible light through the xenon lamp, and carry out the catalytic reaction at room temperature. At the same interval, take the supernatant and pass After 0.45 ⁇ m filter membrane, it was determined that the removal rate of bisphenol A reached more than 90% and the COD removal rate in the reaction system was 94%.
  • N-LaFeO 3 @MCM-41-6 catalyst oxalic acid and terephthalonitrile waste water to the photocatalytic reactor for photocatalytic reaction.
  • the volume ratio of oxalic acid and terephthalonitrile waste water is 1:8, per liter of oxalic acid and
  • the dosage of the photocatalyst in the mixture of terephthalonitrile wastewater is 0.2g; first carry out the dark adsorption reaction for 30 minutes, and after reaching the adsorption equilibrium, then provide visible light through the xenon lamp to carry out the catalytic reaction. After passing through a 0.45 ⁇ m filter membrane, it was determined that the removal rate of terephthalonitrile reached more than 90% and the COD removal rate in the reaction system was 93%.
  • N-LaFeO 3 @MCM-41-7 catalyst methanol and bisphenol A wastewater to the photocatalytic reactor for photocatalytic reaction.
  • the volume ratio of methanol and bisphenol A wastewater is 1:8, per liter of methanol and bisphenol
  • the dosage of the photocatalyst in the mixture of wastewater A is 0.2g; first carry out the dark adsorption reaction for 30 minutes, after reaching the adsorption equilibrium, then provide visible light through the xenon lamp, and carry out the catalytic reaction at room temperature. At the same interval, take the supernatant and pass After 0.45 ⁇ m filter membrane, it was determined that the removal rate of bisphenol A did not reach 80% and the COD removal rate in the reaction system was 70%.
  • N-LaFeO 3 @MCM-41-8 catalyst methanol and bisphenol A wastewater to the photocatalytic reactor for photocatalytic reaction.
  • the volume ratio of methanol and bisphenol A wastewater is 1:8, per liter of methanol and bisphenol
  • the dosage of the photocatalyst in the mixture of A wastewater is 0.2g; first carry out the dark adsorption reaction for 30 minutes, after reaching the adsorption equilibrium, then provide visible light through the xenon lamp, and carry out the catalytic reaction at room temperature. At the same interval, take the supernatant and pass After 0.45 ⁇ m filter membrane, it was determined that the removal rate of bisphenol A did not reach 80% and the COD removal rate in the reaction system was 78%.
  • any one of tartaric acid, malic acid, aspartic acid and lactic acid was used as a complexing agent, urea was used as a mineralizer, and MCM-41 was used as a carrier.
  • Nitrogen was successfully prepared by a sol-gel method.
  • the carrier of Comparative Example 2 is ⁇ -Al 2 O 3 , and the prepared catalyst N-LaFeO 3 @ ⁇ -Al 2 O 3 is not efficient in degrading aromatic compounds because the specific surface area of ⁇ -Al 2 O 3 is not as good as that of MCM- 41 is large, the contact area during degradation is not sufficient, so the removal rate is not ideal.
  • Comparative Example 3 uses citric acid as the complexing agent synthesis catalyst for a longer reaction time, and the entire experimental period is significantly longer than the complexing agent used in this patent.
  • the catalyst obtained by this method has an unsatisfactory effect on the degradation of aromatic compounds, and neither the concentration of waste water nor the removal rate of COD reaches 90%.

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PCT/CN2020/084904 2019-12-16 2020-04-15 一种氮改性钙钛矿复合分子筛的光催化剂及其制备方法与应用方法 WO2021120467A1 (zh)

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CN114700104A (zh) * 2022-05-06 2022-07-05 济南大学 一种以石墨相氮化碳为模板的掺碳多孔微球无铅双钙钛矿复合光催化剂的制备方法
CN115445605A (zh) * 2022-09-20 2022-12-09 中国地质大学（武汉） 铝掺杂镧锰系钙钛矿催化剂的应用
CN115676850A (zh) * 2022-10-11 2023-02-03 电子科技大学 一种Fe(Ⅱ)EDTA辅助光催化NO合成氨的方法

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CN112023975B (zh) * 2020-08-18 2022-11-25 东南大学 一种用于处理垃圾渗滤液的掺杂型光催化剂及其制备方法与应用
CN115520952B (zh) * 2021-06-24 2024-06-28 中国石油化工股份有限公司 一种有机废水的芬顿氧化处理方法
CN114105757B (zh) * 2021-11-23 2023-11-10 天津理工大学 一种将水体中的有害芳烃废物再利用的方法
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CN114700104B (zh) * 2022-05-06 2023-12-19 济南大学 一种以石墨相氮化碳为模板的掺碳多孔微球无铅双钙钛矿复合光催化剂的制备方法
CN115445605A (zh) * 2022-09-20 2022-12-09 中国地质大学（武汉） 铝掺杂镧锰系钙钛矿催化剂的应用
CN115445605B (zh) * 2022-09-20 2023-06-23 中国地质大学（武汉） 铝掺杂镧锰系钙钛矿催化剂的应用
CN115676850A (zh) * 2022-10-11 2023-02-03 电子科技大学 一种Fe(Ⅱ)EDTA辅助光催化NO合成氨的方法

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