CN115337931A - Preparation method of rare earth composite catalyst for degrading organic pollutants - Google Patents
Preparation method of rare earth composite catalyst for degrading organic pollutants Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 53
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 44
- 239000003054 catalyst Substances 0.000 title claims abstract description 35
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 26
- 230000000593 degrading effect Effects 0.000 title claims abstract description 21
- 239000002957 persistent organic pollutant Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- -1 rare earth metal salt Chemical class 0.000 claims abstract description 27
- 239000011259 mixed solution Substances 0.000 claims abstract description 24
- 239000012153 distilled water Substances 0.000 claims abstract description 15
- 239000012716 precipitator Substances 0.000 claims abstract description 14
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 13
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 150000003839 salts Chemical class 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000000654 additive Substances 0.000 claims description 8
- 230000000996 additive effect Effects 0.000 claims description 8
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 8
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 7
- 239000001099 ammonium carbonate Substances 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 4
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 3
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 3
- 229940099596 manganese sulfate Drugs 0.000 claims description 3
- 239000011702 manganese sulphate Substances 0.000 claims description 3
- 235000007079 manganese sulphate Nutrition 0.000 claims description 3
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 3
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 12
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 6
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 8
- 229940012189 methyl orange Drugs 0.000 description 8
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- 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
- C02F1/302—Treatment of water, waste water, or sewage by irradiation with microwaves
-
- 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
- C02F1/722—Oxidation by peroxides
-
- 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
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
-
- 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
Abstract
The embodiment of the invention provides a preparation method of a rare earth composite catalyst for degrading organic pollutants, belonging to the technical field of catalyst preparation. Wherein, the preparation method comprises the following steps: dissolving rare earth metal salt and transition metal salt in a certain metering ratio in distilled water with a certain volume, and controlling the water bath at a certain temperature to obtain a mixed solution; under the condition of continuous stirring, dropwise adding a certain proportion of composite precipitator into the mixed solution, and controlling the pH of the mixed solution to a certain range; aging for a certain time, performing solid-liquid separation, washing the precipitate with distilled water for several times, and drying at a certain temperature to constant weight; roasting for a certain time at a certain temperature to obtain the rare earth composite catalyst. The invention can reduce the operation cost, improve the catalytic activity and effectively increase the degradation efficiency of organic pollutants.
Description
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to a preparation method of a rare earth composite catalyst for degrading organic pollutants.
Background
High-concentration and difficult-to-degrade organic wastewater is widely generated in the industries of pharmacy, petrochemical industry, papermaking, bioengineering, sugar manufacturing, synthetic fiber, dye, medicine and the like, and a series of problems of water body pollution, ecological environment deterioration, human health threat and the like caused by the high-concentration and difficult-to-degrade organic wastewater become serious.
Among various organic wastewater treatment processes, the heterogeneous catalytic oxidation process is an advanced process for treating organic wastewater and is always the focus of attention of researchers. The technology is characterized in that the organic waste is catalytically degraded under the action of a high-oxidation activity and high-stability catalyst, so that the aim of heterogeneous catalytic oxidation is fulfilled, and the COD content is reduced. The reaction does not need to be carried out at high temperature and high pressure, and can meet the reaction requirement under the common conditions, thereby obtaining high oxidation treatment efficiency. The research and development and production of the high-efficiency catalytic material are always the key of the treatment process, and the treatment efficiency and the application prospect are directly determined.
The active component adopted by the catalyst system usually comprises precious metals (such as Pd, pt, au, and the like), non-precious metals (such as Cu, mn, fe, and the like), and rare earth elements such as Ce, la, and the like, and can be composed of one metal or metal oxide, or can be composed of multiple metals, oxides or composite oxides. However, the current research on water treatment catalysts also faces certain problems, such as difficulty in separating and recovering a part of the catalyst, excessively rapid reduction of catalytic activity, and high running cost.
Disclosure of Invention
The embodiment of the invention aims to provide a preparation method of a rare earth composite catalyst for degrading organic pollutants, and aims to reduce the operation cost, improve the catalytic activity and effectively increase the degradation efficiency of the organic pollutants.
The embodiment of the invention provides a preparation method of a rare earth composite catalyst for degrading organic pollutants, which comprises the following steps:
s10: dissolving rare earth metal salt and transition metal salt in a certain metering ratio in distilled water with a certain volume, and controlling the water bath at a certain temperature to obtain a mixed solution;
s20: dropwise adding a certain proportion of composite precipitator into the mixed solution under the condition of continuous stirring, and controlling the pH value of the mixed solution to a certain range;
s30: aging for a certain time, performing solid-liquid separation, washing the precipitate with distilled water for several times, and drying at a certain temperature to constant weight;
s40: roasting for a certain time at a certain temperature to obtain the rare earth composite catalyst.
Further, the rare earth metal salt is one of cerium nitrate, zirconium sulfate and lanthanum chloride, and the transition metal salt is one of ferric nitrate, cupric nitrate, nickel nitrate, zinc sulfate, titanium sulfate and manganese sulfate.
Further, the rare earth metal salt and the transition metal salt are mixed to form a composite metal salt, and the content of the rare earth metal salt is 0.1-5% of the content of the composite metal salt.
Further, the volume of the distilled water is 100ml, and the temperature of the water bath is controlled to be 20-60 ℃.
Further, the composite precipitator comprises a precipitator and an additive, the precipitator is one of ammonia water, sodium carbonate, sodium hydroxide, ammonium carbonate and ammonium bicarbonate, and the additive is one of polyethylene glycol 400, hexamethylenetetramine, urea and sodium citrate.
Further, the additive accounts for 1 to 10 percent of the content of the composite precipitator.
Further, the pH range of the mixed solution is controlled to be 6.5-9.5, and the aging time is 2-8h.
Further, the drying temperature in the step S30 is 80 to 120 ℃.
Furthermore, the roasting temperature in the step S40 is 250-450 ℃, and the roasting time is 2-6h.
The invention has the beneficial effects that:
according to the preparation method of the rare earth composite catalyst for degrading the organic pollutants, provided by the embodiment of the invention, the rare earth metal salt and the transition metal salt are dissolved, a water bath is controlled at a certain temperature to obtain a mixed solution, a composite precipitator is added into the mixed solution, the pH range is controlled, and the steps of aging, drying, roasting and the like are sequentially carried out to obtain the rare earth composite catalyst. The catalytic characteristics of the rare earth element and the transition metal element are combined, so that the operation cost is reduced and the catalytic activity is improved.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of embodiments of the invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention.
Example 1
The embodiment of the invention provides a preparation method of a rare earth composite catalyst for degrading organic pollutants, which comprises the following steps:
step S10: dissolving rare earth metal salt and transition metal salt in a certain metering ratio in distilled water with a certain volume, and controlling the water bath at a certain temperature to obtain a mixed solution.
Wherein the rare earth metal salt is one of cerium nitrate, zirconium sulfate and lanthanum chloride. The transition metal salt is one of ferric nitrate, cupric nitrate, nickel nitrate, zinc sulfate, titanium sulfate and manganese sulfate.
When the method is implemented, the rare earth metal salt and the transition metal salt are mixed to form the composite metal salt, and the content of the rare earth metal salt accounts for 0.1-5% of the content of the composite metal salt. The volume of the distilled water is 100ml, and the temperature of the water bath is controlled to be 20-60 ℃.
Step S20: under the condition of continuous stirring, dropwise adding a certain proportion of composite precipitator into the mixed solution, and controlling the pH value of the mixed solution to a certain range.
Wherein the composite precipitator comprises a precipitator and an additive. The precipitant is one of ammonia water, sodium carbonate, sodium hydroxide, ammonium carbonate and ammonium bicarbonate. The additive is one of polyethylene glycol 400, hexamethylenetetramine, urea and sodium citrate.
In implementation, the additive accounts for 1 to 10 percent of the content of the composite precipitator. The pH range of the mixed solution is controlled to be 6.5-9.5.
Step S30: aging for a certain time, performing solid-liquid separation, washing the precipitate with distilled water for several times, and drying at a certain temperature to constant weight.
Wherein the aging time is 2-8h. The drying temperature is 80-120 ℃.
Step S40: roasting for a certain time at a certain temperature to obtain the rare earth composite catalyst.
Wherein the roasting temperature is 250-450 ℃, and the roasting time is 2-6h.
Example 2
The embodiment of the invention provides a preparation method of a rare earth composite catalyst for degrading organic pollutants, which comprises the following steps:
step S10: a composite metal salt of cerium nitrate and copper nitrate was dissolved in 100ml of distilled water and subjected to water bath to obtain a mixed solution.
Wherein the cerium nitrate accounts for 1% of the weight of the composite metal salt, and the water bath temperature is controlled at 40 ℃.
Step S20: and dropwise adding a composite precipitator of ammonia water and sodium citrate into the mixed solution under the condition of continuous stirring.
Wherein the weight ratio of the sodium citrate is 10 percent, and the pH of the mixed solution is controlled to be 7.2.
Step S30: aging for 6 hr, performing solid-liquid separation, washing the precipitate with distilled water for several times, and drying at 105 deg.C to constant weight.
Step S40: roasting for 2 hours at 350 ℃ to obtain the high-activity CuO/CeO2 composite catalyst capable of degrading organic wastewater.
Example 3
The embodiment of the invention provides a preparation method of a rare earth composite catalyst for degrading organic pollutants, which comprises the following steps:
step S10: dissolving the composite metal salt of lanthanum chloride and ferric nitrate in 100ml of distilled water, and obtaining a mixed solution after water bath.
Wherein, the cerous nitrate accounts for 0.5 percent of the weight of the composite salt, and the water bath temperature is controlled at 60 ℃.
Step S20: and dropwise adding a composite precipitant of ammonium carbonate and urea into the mixed solution under the condition of continuous stirring. Wherein the weight of the urea accounts for 15%, and the pH value of the solution is controlled to be 8.
Step S30: aging for 8 hr, performing solid-liquid separation, washing the precipitate with distilled water for several times, and drying at 120 deg.C to constant weight.
Step S40: roasting for 4 hours at 320 ℃ to obtain the high-activity Fe2O3/La2O3 composite catalyst capable of degrading organic wastewater.
Activity evaluation example:
methyl orange is taken as a target pollutant, the rare earth composite catalyst prepared in the embodiment is used for catalytically degrading the methyl orange, and the activity of the methyl orange is tested.
Taking 100ml of 60mg/l methyl orange solution, placing at 25 ℃, irradiating for 10min under the microwave power of 400W under the condition that the temperature is 25 ℃ 2 O 2 The amount used was 1ml, and the amount of catalyst added was 0.1g. Taking out after the irradiation is carried out for a set time, cooling and fixing the volume, measuring the absorbance of the solution at 490nm by using an ultraviolet-visible spectrophotometer, and calculating the removal rate of the methyl orange according to the absorbance.
The catalytic decomposition efficiency of the methyl orange is calculated by measuring the content of the methyl orange in the reaction solution before and after the reaction, and the calculation method of the degradation efficiency comprises the following steps:
η=（A0-A）/Ａ0×100%
wherein: a0 is the initial absorbance of methyl orange;
a is the absorbance after the reaction.
In the above examples, the catalytic degradation efficiency of methyl orange is shown in the following table:
| product(s) | Example 1 | Example 2 |
| The degradation rate% | 96 | 94 |
Therefore, the rare earth composite catalyst prepared by the embodiment of the invention has higher catalytic degradation rate.
In summary, according to the preparation method of the rare earth composite catalyst for degrading organic pollutants provided by the embodiment of the present invention, the rare earth metal salt and the transition metal salt are dissolved, a water bath is controlled at a certain temperature to obtain a mixed solution, a composite precipitant is added into the mixed solution, the pH range is controlled, and the steps of aging, drying, roasting, etc. are sequentially performed to obtain the rare earth composite catalyst. The catalytic characteristics of the rare earth element and the transition metal element are combined, so that the operation cost is reduced and the catalytic activity is improved.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The preparation method of the rare earth composite catalyst for degrading organic pollutants is characterized by comprising the following steps:
s10: dissolving rare earth metal salt and transition metal salt in a certain metering ratio in distilled water with a certain volume, and controlling the water bath at a certain temperature to obtain a mixed solution;
s20: dropwise adding a certain proportion of composite precipitator into the mixed solution under the condition of continuous stirring, and controlling the pH value of the mixed solution to a certain range;
s30: aging for a certain time, performing solid-liquid separation, washing the precipitate with distilled water for several times, and drying at a certain temperature to constant weight;
s40: roasting for a certain time at a certain temperature to obtain the rare earth composite catalyst.
2. The method of preparing a rare earth composite catalyst for degrading organic pollutants according to claim 1, wherein the rare earth metal salt is one of cerium nitrate, zirconium sulfate and lanthanum chloride, and the transition metal salt is one of iron nitrate, copper nitrate, nickel nitrate, zinc sulfate, titanium sulfate and manganese sulfate.
3. The method for preparing the rare earth composite catalyst for degrading the organic pollutants as claimed in claim 1 or 2, wherein the rare earth metal salt and the transition metal salt are mixed to form a composite metal salt, and the content of the rare earth metal salt is 0.1 to 5 percent of the content of the composite metal salt.
4. The method for preparing a rare earth composite catalyst for degrading organic pollutants according to claim 1, wherein the volume of the distilled water is 100ml, and the temperature of the water bath is controlled to be 20-60 ℃.
5. The method for preparing a rare earth composite catalyst for degrading organic pollutants according to claim 1, wherein the composite precipitant comprises one of ammonia water, sodium carbonate, sodium hydroxide, ammonium carbonate and ammonium bicarbonate, and an additive is one of polyethylene glycol 400, hexamethylenetetramine, urea and sodium citrate.
6. The method for preparing a rare earth composite catalyst for degrading organic pollutants according to claim 5, wherein the additive accounts for 1 to 10 percent of the content of the composite precipitator.
7. The method of preparing a rare earth composite catalyst for degrading organic pollutants according to claim 1, wherein the pH of the mixed solution is controlled to be 6.5 to 9.5, and the aging time is 2 to 8 hours.
8. The method of claim 1, wherein the drying temperature in the step S30 is 80-120 ℃.
9. The method of claim 1, wherein the calcination temperature in step S40 is 250-450 ℃ and the calcination time is 2-6h.
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