CN111617735A - Amine odor removal material - Google Patents
Amine odor removal material Download PDFInfo
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- CN111617735A CN111617735A CN202010460482.4A CN202010460482A CN111617735A CN 111617735 A CN111617735 A CN 111617735A CN 202010460482 A CN202010460482 A CN 202010460482A CN 111617735 A CN111617735 A CN 111617735A
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- salt solution
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- 239000000463 material Substances 0.000 title claims abstract description 107
- 150000001412 amines Chemical class 0.000 title claims abstract description 42
- 239000000243 solution Substances 0.000 claims abstract description 70
- 238000001035 drying Methods 0.000 claims abstract description 41
- 238000002791 soaking Methods 0.000 claims abstract description 25
- 238000001179 sorption measurement Methods 0.000 claims abstract description 24
- 239000012266 salt solution Substances 0.000 claims abstract description 23
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 230000003197 catalytic effect Effects 0.000 claims abstract description 7
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000004321 preservation Methods 0.000 claims abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 41
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 31
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 24
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 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 18
- 239000002781 deodorant agent Substances 0.000 claims description 18
- 235000019270 ammonium chloride Nutrition 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 12
- 230000001877 deodorizing effect Effects 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 229910021536 Zeolite Inorganic materials 0.000 claims description 10
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 10
- 239000010457 zeolite Substances 0.000 claims description 10
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 150000000703 Cerium Chemical class 0.000 claims description 8
- 239000012670 alkaline solution Substances 0.000 claims description 8
- 150000002696 manganese Chemical class 0.000 claims description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- 239000003463 adsorbent Substances 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 5
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 5
- 125000000524 functional group Chemical group 0.000 claims description 5
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 238000005470 impregnation Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000005909 Kieselgur Substances 0.000 claims description 3
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 3
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 3
- 229940071125 manganese acetate Drugs 0.000 claims description 3
- 239000011565 manganese chloride Substances 0.000 claims description 3
- 235000002867 manganese chloride Nutrition 0.000 claims description 3
- 229940099607 manganese chloride Drugs 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
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 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
- 238000007598 dipping method Methods 0.000 claims description 2
- 239000003929 acidic solution Substances 0.000 claims 1
- 238000011534 incubation Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 16
- 239000007789 gas Substances 0.000 abstract description 8
- 238000011068 loading method Methods 0.000 abstract description 6
- 238000004332 deodorization Methods 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 20
- 229910021529 ammonia Inorganic materials 0.000 description 15
- 238000010438 heat treatment Methods 0.000 description 13
- 238000005406 washing Methods 0.000 description 11
- 235000019645 odor Nutrition 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 241000282414 Homo sapiens Species 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- 229910002706 AlOOH Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- -1 ammonium ions Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000009615 deamination Effects 0.000 description 1
- 238000006481 deamination reaction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 210000002249 digestive system Anatomy 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 210000000750 endocrine system Anatomy 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 230000003211 malignant effect Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 150000003754 zirconium Chemical class 0.000 description 1
Classifications
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/165—Natural alumino-silicates, e.g. zeolites
-
- 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
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
-
- 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
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- B01J35/615—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/406—Ammonia
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention provides an amine deodorization material, and belongs to the field of deodorization materials. The preparation method comprises the following steps: (1) carrying out hydrothermal treatment on the adsorption material in the reactor by using an inorganic salt solution, and cleaning and drying to obtain a modified material carrier; (2) soaking the modified material carrier in an acid solution and then drying to obtain a soaked carrier; (3) preparing a catalytic activity precursor solution, soaking the soaked carrier into the catalytic activity precursor solution again in the same volume, performing heat preservation reaction, and then roasting to obtain the catalyst. The invention can effectively adjust the specific surface area, porosity and average pore diameter of the selected adsorbing material, can match the loading capacity in a grading way, has more excellent material loading effect, and then effectively removes various amine malodorous gases at the same time through the synergistic effect of catalysis and adsorption in the normal temperature environment.
Description
Technical Field
The invention relates to the field of deodorization materials, in particular to an amine deodorization material.
Background
With the development of economy and the improvement of living standard, people's environmental awareness is gradually increased, and malodorous pollution has received high attention globally as one of environmental public hazards. The odor pollution mainly comprises two types of odors generated in life and in industrial production. The sources of malodor in daily life are: odor emitted by indoor decoration materials comprises foul gas containing volatile organic compounds and the like, such as paint, binder and the like, which has great harm to human bodies; in addition, kitchens, living rooms, toilets, garbage dumps and pet rooms are all places where malodors often occur. The sources of malodor in industrial production mainly include: chemical plants, pesticide plants, coating plants, food fermentation plants, poultry plants, and the like. These malodorous gases mainly include volatile inorganic salts containing ammonium ions, such as ammonia, ammonium chloride, trimethylamine, etc., and organic pollutants containing amine functional groups.
Amine malodorous gases are typical malodorous substances, and have a great influence on human beings and the environment. Such substances can strongly stimulate the sensory organs of people, make people feel unpleasant and dislike, and cause psychological burden; meanwhile, the amine odor gas with a certain concentration can cause harm to the respiratory system, the circulatory system, the digestive system, the endocrine system and the like of the human body.
At present, the treatment scheme for amine odor type malignant gas in China and abroad mainly focuses on acid modified adsorption materials, for example, in a normal-temperature ammonia gas high-efficiency treatment material with a patent number of CN 105268399B, porous adsorption materials such as activated carbon, activated alumina and zeolite molecular sieves are mainly applied as carriers, aluminum salt and zirconium salt are used as mixed modifiers, and acid is used as a surface modifier for modification to prepare an ammonia gas removal material. But the pore size and porosity of the adsorbent material are not controlled in the modification process.
Patent No. CN 104368307A, name "preparation method of special active carbon for ammonia adsorption", patent No. CN 109455713A, name "preparation technology of industrial high-efficiency deamination active carbon", patent No. CN 107952413A, name "modified high-efficiency ammonia-proof active carbon and preparation method" all use active carbon as substrate, acid is ammonia gas removal material that modifier prepared, but the pore structure of substrate is not stipulated in the above-mentioned several technical schemes, and because the active carbon itself is more basic groups, will neutralize the basic groups in the active carbon first in the acid modification process, cause the partial pore collapse of active carbon.
In view of this, the present application is specifically made.
Disclosure of Invention
The invention aims to provide an amine odor removal material, which can effectively adjust the specific surface area, porosity and average pore diameter of a selected adsorption material, can be used for proportioning the loading capacity in a grading way, has more excellent loading effect, and can effectively remove various amine odor gases at the same time through the synergistic effect of catalysis and adsorption in a normal temperature environment.
In order to achieve the above purpose, the invention adopts the following technical scheme:
an amine deodorant material, which is prepared by a method comprising:
step 1:
and carrying out hydrothermal treatment on the adsorption material in the reactor by using an inorganic salt solution, and cleaning and drying to obtain the modified material carrier.
The adsorption material is a porous adsorption material without acidic functional groups.
Preferably, the adsorbent material is one or more of zeolite, porous resin, activated alumina, diatomaceous earth, or porous silica. The porous materials have uneven pore size distribution, smaller specific surface area and poor hydrophilic ability, so the porous materials need to be subjected to hole expansion, capacity increase and hydrophilic modification.
The inorganic salt solution is one or a mixed solution of more of ammonia water, ammonium chloride or ammonium dihydrogen phosphate solution with the mass concentration of 5-50%.
The hydrothermal treatment is that inorganic salt solution is atomized and then is introduced into the reactor at the speed of 5-10ml/min, the temperature rise speed is controlled to be 1-20 ℃/min, the treatment temperature is 120-.
Crystals with larger particle sizes can be generated during the hydrothermal treatment, so that larger interparticle pores are formed, the pore size of the carrier is increased, and the pore size is gradually increased along with the increase of the treatment temperature, but the strength of the carrier is reduced if the treatment temperature is too high. Taking activated alumina as an example, the activated alumina nanoparticles can be converted into regular AlOOH nanosheets by treatment at 200 ℃ for 2h, thereby increasing the specific surface area.
Thus, by the above treatment, the specific surface area of the adsorbent material is significantly increased, while the average pore size is significantly reduced.
Step 2:
and (3) soaking the modified material carrier in an acid solution, and then drying to obtain the soaked carrier.
The acid solution is one or more of phosphoric acid, acetic acid or formic acid with the mass concentration of 1-5%.
The dipping time is 30-180min, and the drying temperature is 90-150 ℃.
The purpose of this impregnation is to further remove the basic functional groups on the surface of the modified porous adsorbent. Meanwhile, the adsorption materials such as zeolite, porous resin, activated alumina, diatomaceous earth, or porous silica are all adsorption materials that do not contain an acidic functional group. Therefore, the ammonia water and ammonium salt are used for pore-expanding treatment in the step 1, and acid-base neutralization reaction cannot occur. In the acid solution impregnation process in the step 2, all weak acids are used, and mainly neutralization reaction is carried out before the generation of the medium-basic functional groups in the hole expanding process, the reaction mainly occurs on the surface, and the weak acid at the concentration is incapable of further corroding the substrate to cause the collapse of pores, so that the pore structure is effectively maintained.
And step 3:
preparing a catalytic activity precursor solution, soaking the soaked carrier into the catalytic activity precursor solution again in the same volume, performing heat preservation reaction, and then roasting to obtain the catalyst.
The catalytic activity precursor solution is a mixed solution of a cerium salt solution, a manganese salt solution and an alkaline solution.
The volume ratio of the cerium salt solution, the manganese salt solution and the alkaline solution is 0.2-4:0.1-5: 1-10.
The cerium salt solution is one or more of cerium nitrate, cerium sulfate or cerium chloride; the manganese salt solution is one or more of manganese acetate, manganese chloride, manganese sulfate or manganese nitrate; the alkaline solution is sodium hydroxide, potassium hydroxide or ammonia water solution.
Preferably, the molar concentration of the cerium salt solution is 0.1-1mol/L, the molar concentration of the manganese salt solution is 0.3-3mol/L, and the molar concentration of the alkaline solution is 2-10 mol/L.
The temperature of the heat preservation reaction is 60-100 ℃, and the time is 12-24 h; the roasting is carried out for 2-6h in a muffle furnace at the temperature of 300-500 ℃;
preferably, the calcined sample is washed by pure water for 2-3 times, soluble salt in pores is removed, and then the calcined sample is dried at the temperature of 80-120 ℃.
Preferably, during the equal volume impregnation, stirring is continued for 0.5-3 h.
Compared with the prior art, the invention has the beneficial effects that at least:
1) the amine deodorization material can effectively adjust the specific surface area, the porosity and the average pore diameter of the selected adsorbing material, can be used for proportioning the loading capacity in a grading way, and has more excellent loading effect.
2) The amine odor removing material can effectively remove various amine malodorous gases at the same time under the normal temperature environment through the synergistic effect of catalysis and adsorption.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to specific examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
An amine deodorant material, the preparation method comprises the following steps:
(1) selecting 1-3mm spherical zeolite as an adsorption material base material, carrying out hydrothermal treatment on the spherical zeolite in a reactor by using a 5% ammonia water solution, namely atomizing the ammonia water solution, introducing the atomized ammonia water solution into a furnace at a speed of 6ml/min, raising the temperature of the furnace body at a speed of 5 ℃/min, raising the temperature to 250 ℃, keeping the temperature for 2 hours, cooling the furnace, cleaning the furnace for 3 times by using clear water, and drying the furnace in a 100 ℃ oven to obtain the modified material carrier.
The specific surface area of the spherical zeolite before and after the test treatment is increased from 320 square meters per gram to 397 square meters per gram.
(2) And (2) soaking the modified material carrier in a phosphoric acid solution with the mass fraction of 2% for 60min, and then drying at 100 ℃ to obtain the soaked carrier.
(3) And (3) soaking the impregnated carrier into a mixed solution of 0.4mol/L cerium nitrate, 0.3mol/L manganese nitrate and 2mol/L sodium hydroxide solution in an equal volume, wherein the volume ratio of the mixed solution is 0.2:0.1: 1. Continuously stirring for 0.5h, reacting for 24h at 100 ℃, then transferring into a muffle furnace to calcine for 2h at 350 ℃, washing the calcined sample for 3 times by pure water, and drying at 100 ℃.
And (3) product testing: 100g of the above-mentioned amine deodorizing material is placed in a filter element, and the wind speed is 200m3H, initial ammonia concentration 2mg/m3The ammonia gas removal rate per unit time was 83%.
Example 2
An amine deodorant material, the preparation method comprises the following steps:
(1) selecting 1-3mm spherical porous resin as a base material of an adsorption material, carrying out hydrothermal treatment on the spherical porous resin in a reactor by using a 15% ammonium chloride solution, namely atomizing the ammonium chloride solution, introducing the atomized ammonium chloride solution into a furnace at a speed of 7ml/min, heating the furnace body at a speed of 5 ℃/min, heating to 300 ℃, keeping the temperature for 2 hours, cooling along with the furnace, cleaning for 3 times by using clear water, and drying in an oven at 100 ℃ to obtain the modified material carrier.
The specific surface area of the spherical porous resin before and after the test treatment is increased from 576 square meters per gram to 612 square meters per gram.
(2) And (2) soaking the modified material carrier in an acetic acid solution with the mass fraction of 2.5% for 90min, and then drying at 120 ℃ to obtain the soaked carrier.
(3) And (3) soaking the soaked carrier into a mixed solution of 1mol/L cerium nitrate, 0.8mol/L manganese nitrate and 2mol/L ammonia water solution in an equal volume, wherein the volume ratio of the mixed solution is 0.5:0.5: 1.2. Continuously stirring for 1h, reacting for 24h at 100 ℃, then transferring into a muffle furnace to calcine for 2h at 400 ℃, washing the calcined sample for 2 times by pure water, and drying at 120 ℃.
And (3) product testing: 100g of the above-mentioned amine deodorizing material is placed in a filter element, and the wind speed is 200m3H, initial ammonia concentration 2mg/m3The ammonia removal rate per unit time was 90%.
Example 3
An amine deodorant material, the preparation method comprises the following steps:
(1) selecting 1-3mm silicon spheres (porous silicon dioxide) as a base material of an adsorption material, carrying out hydrothermal treatment on the silicon spheres in a reactor by using 7% ammonium dihydrogen phosphate solution, namely atomizing the ammonium dihydrogen phosphate solution, introducing the atomized ammonium dihydrogen phosphate solution into a furnace at a speed of 5ml/min, heating the furnace body at a temperature of 5 ℃/min to 350 ℃, preserving heat for 4 hours, cooling the furnace, cleaning the furnace body for 3 times by using clear water, and drying the furnace body in a 100 ℃ drying oven to obtain the modified material carrier.
The specific surface area of the silicon balls before and after the test treatment is increased from 340 square meters per gram to 420 square meters per gram.
(2) And (2) soaking the modified material carrier in an acetic acid solution with the mass fraction of 1% for 30min, and then drying at 100 ℃ to obtain the soaked carrier.
(3) And (3) soaking the impregnated carrier into a mixed solution of 0.6mol/L cerium nitrate, 0.3mol/L manganese nitrate and 2.5mol/L sodium hydroxide solution in an equal volume ratio of 1.5:0.5: 1. Continuously stirring for 1h, reacting for 24h at 100 ℃, then transferring into a muffle furnace to calcine for 3h at 400 ℃, washing the calcined sample for 3 times by pure water, and drying at 100 ℃.
And (3) product testing: 100g of the above-mentioned amine deodorizing material is placed in a filter element, and the wind speed is 200m3H, initial ammonia concentration 2mg/m3The ammonia gas removal rate per unit time was 91%.
Example 4
An amine deodorant material, the preparation method comprises the following steps:
(1) selecting 1-3mm spherical activated alumina as a base material of an adsorption material, carrying out hydrothermal treatment on the activated alumina in a reactor by using a 5% ammonia water solution, namely atomizing the ammonia water solution, introducing the atomized ammonia water solution into a furnace at a speed of 6ml/min, heating the furnace body at a temperature rise speed of 5 ℃/min, raising the temperature to 150 ℃, keeping the temperature for 2 hours, cooling the furnace, cleaning the furnace body for 3 times by using clear water, and drying the furnace body in a 100 ℃ drying oven to obtain the modified material carrier.
The specific surface area of the activated alumina before and after the test treatment is increased from 204.6 square meters per gram to 320 square meters per gram.
(2) And (2) soaking the modified material carrier in a phosphoric acid solution with the mass fraction of 2% for 60min, and then drying at 100 ℃ to obtain the soaked carrier.
(3) And (3) soaking the impregnated carrier into a mixed solution of 0.4mol/L cerium nitrate, 0.3mol/L manganese nitrate and 2mol/L sodium hydroxide solution in an equal volume, wherein the volume ratio of the mixed solution is 0.2:0.1: 1. Continuously stirring for 0.5h, reacting for 24h at 100 ℃, then transferring into a muffle furnace to calcine for 2h at 350 ℃, washing the calcined sample for 3 times by pure water, and drying at 100 ℃ to obtain the catalyst.
And (3) product testing: 100g of the above-mentioned amine deodorizing material is placed in a filter element, and the wind speed is 200m3H, initial ammonia concentration 2mg/m3The ammonia gas removal rate per unit time was 88%.
Example 5
An amine deodorant material, the preparation method comprises the following steps:
(1) selecting 1-3mm diatom balls as a base material of an adsorption material, carrying out hydrothermal treatment on the diatom balls in a reactor by using a 10% ammonium chloride solution, namely atomizing the ammonium chloride solution, introducing the ammonium chloride solution into the furnace at a speed of 10ml/min, heating the furnace body at a speed of 5 ℃/min, heating to 500 ℃, keeping the temperature for 6 hours, cooling along with the furnace, cleaning for 3 times by using clear water, and drying in an oven at 100 ℃ to obtain the modified material carrier.
The specific surface area of the diatom balls before and after the test treatment is increased from 127.6 square meters per gram to 179 square meters per gram.
(2) And (2) soaking the modified material carrier in 1% formic acid solution for 60min, and then drying at 90 ℃ to obtain the soaked carrier.
(3) And (3) soaking the impregnated carrier into a mixed solution of 0.7mol/L cerium nitrate, 0.4mol/L manganese nitrate and 3mol/L sodium hydroxide solution in an equal volume, wherein the volume ratio of the mixed solution is 3:1.5: 4. Continuously stirring for 0.5h, reacting for 24h at 100 ℃, then transferring into a muffle furnace to calcine for 3h at 450 ℃, washing the calcined sample for 3 times by pure water, and drying at 100 ℃ to obtain the catalyst.
And (3) product testing: 100g of the above-mentioned amine deodorizing material is placed in a filter element, and the wind speed is 200m3H, initial ammonia concentration 2mg/m3The ammonia gas removal rate per unit time was 82%.
Example 6
An amine deodorant material, the preparation method comprises the following steps:
(1) selecting 1-3mm spherical activated alumina as a base material of an adsorption material, carrying out hydrothermal treatment on the spherical activated alumina in a reactor by using 50% ammonium chloride solution, namely atomizing the ammonium chloride solution, introducing the ammonium chloride solution into a furnace at a speed of 7ml/min, heating the furnace body at a speed of 20 ℃/min, heating to 200 ℃, keeping the temperature for 2 hours, cooling along with the furnace, washing for 3 times by using clear water, and drying in a 90 ℃ oven to obtain the modified material carrier.
The specific surface area of the spherical activated alumina before and after the test treatment is increased from 204.6 square meters per gram to 335 square meters per gram.
(2) And (2) soaking the modified material carrier in a mixed solution of 5% by mass of formic acid and acetic acid for 90min, and then drying at 120 ℃ to obtain the soaked carrier.
(3) And (3) soaking the impregnated carrier into a mixed solution of 0.1mol/L cerium sulfate, 0.8mol/L manganese sulfate and 10mol/L ammonia water solution in an equal volume ratio of 4:5: 10. Continuously stirring for 3h, reacting for 18h at 60 ℃, then transferring into a muffle furnace to calcine for 6h at 500 ℃, washing the calcined sample for 3 times by pure water, and drying at 100 ℃ to obtain the catalyst.
And (3) product testing: 100g of the above-mentioned deodorizing material is packed in a filter elementMedium wind speed 200m3H, initial ammonia concentration 2mg/m3The ammonia removal rate per unit time was 92%.
Example 7
An amine deodorant material, the preparation method comprises the following steps:
(1) selecting 1-3mm spherical activated alumina as a base material of an adsorption material, carrying out hydrothermal treatment on the spherical activated alumina in a reactor by using a 20% ammonia water solution, namely atomizing the ammonia water solution, introducing the atomized ammonia water solution into a furnace at a speed of 7ml/min, heating the furnace body at a temperature rise speed of 1 ℃/min, raising the temperature to 700 ℃, keeping the temperature for 0.5h, cooling the furnace, cleaning the furnace body for 3 times by using clear water, and drying the furnace body in a 120 ℃ oven to obtain the modified material carrier.
The specific surface area of the spherical activated alumina before and after the test treatment is increased from 204.6 square meters per gram to 309 square meters per gram.
(2) And (2) soaking the modified material carrier in an acetic acid solution with the mass fraction of 3% for 180min, and then drying at 150 ℃ to obtain the soaked carrier.
(3) And (3) soaking the soaked carrier into a mixed solution of 1mol/L cerium chloride, 3mol/L manganese chloride and 5mol/L ammonia water solution in an equal volume, wherein the volume ratio of the mixed solution is 0.5:3: 5. Continuously stirring for 1.5h, reacting for 12h at 80 ℃, then transferring into a muffle furnace to calcine for 3h at 300 ℃, washing the calcined sample for 3 times by pure water, and drying at 100 ℃ to obtain the catalyst.
And (3) product testing: 100g of the above-mentioned amine deodorizing material is placed in a filter element, and the wind speed is 200m3H, initial ammonia concentration 2mg/m3The ammonia gas removal rate per unit time was 81%.
Example 8
An amine deodorant material, the preparation method comprises the following steps:
(1) selecting 1-3mm spherical activated alumina as a base material of an adsorption material, carrying out hydrothermal treatment on the spherical activated alumina in a reactor by using a 20% ammonia water solution, namely atomizing the ammonia water solution, introducing the atomized ammonia water solution into a furnace at a speed of 7ml/min, heating the furnace body at a speed of 1 ℃/min, heating the furnace body to 400 ℃, keeping the temperature for 1h, cooling the furnace, cleaning the furnace body for 3 times by using clear water, and drying the furnace body in an oven at 100 ℃ to obtain the modified material carrier.
The specific surface area of the spherical activated alumina before and after the test treatment is increased from 204.6 square meters per gram to 316 square meters per gram.
(2) And (2) soaking the modified material carrier in an acetic acid solution with the mass fraction of 3% for 60min, and then drying at 150 ℃ to obtain the soaked carrier.
(3) And (3) soaking the soaked carrier into a mixed solution of 1mol/L cerium chloride, 1.5mol/L manganese acetate and 2mol/L potassium hydroxide solution in an equal volume, wherein the volume ratio of the mixed solution is 0.5:3: 1. Continuously stirring for 1.5h, reacting for 12h at 80 ℃, then transferring into a muffle furnace to calcine for 3h at 350 ℃, washing the calcined sample for 3 times by pure water, and drying at 100 ℃ to obtain the catalyst.
And (3) product testing: 100g of the above-mentioned amine deodorizing material is placed in a filter element, and the wind speed is 200m3H, initial ammonia concentration 2mg/m3The ammonia gas removal rate per unit time was 76%.
Comparative example 1
An amine deodorant material, the preparation method comprises the following steps:
(1) selecting 1-3mm spherical zeolite as an adsorption material base material, carrying out hydrothermal treatment on the spherical zeolite in a reactor by using a 3% ammonia water solution, namely atomizing the ammonia water solution, introducing the atomized ammonia water solution into a furnace at a speed of 1ml/min, raising the temperature of the furnace body at a speed of 5 ℃/min, raising the temperature to 100 ℃, keeping the temperature for 2 hours, cooling the furnace, cleaning the furnace for 3 times by using clear water, and drying the furnace in a 100 ℃ oven to obtain the modified material carrier.
The specific surface area of the spherical zeolite never increased significantly before and after the test treatment.
(2) And (2) soaking the modified material carrier in a phosphoric acid solution with the mass fraction of 0.5% for 30min, and then drying at 100 ℃ to obtain the soaked carrier.
(3) The impregnated carrier is immersed into a mixed solution of 0.05mol/L cerium nitrate, 0.1mol/L manganese nitrate and 1mol/L sodium hydroxide solution in equal volume, wherein the volume ratio of the mixed solution is 0.1:0.05: 1. Continuously stirring for 0.5h, reacting for 24h at 100 ℃, then transferring into a muffle furnace to calcine for 2h at 200 ℃, washing the calcined sample for 3 times by pure water, and drying at 100 ℃.
And (3) product testing: 100g of the above-mentioned amine deodorizing material is placed in a filter element, and the wind speed is 200m3H, initial ammonia concentration 2mg/m3The ammonia gas removal rate per unit time was 26.7%.
Comparative example 2
An amine deodorant material, the preparation method comprises the following steps:
(1) selecting 1-3mm spherical porous resin as a base material of an adsorption material, carrying out hydrothermal treatment on the porous resin in a reactor by using 70% ammonium chloride solution, namely atomizing the ammonium chloride solution, introducing the atomized ammonium chloride solution into a furnace at a speed of 3ml/min, heating the furnace body at a speed of 15 ℃/min, heating the furnace body to 900 ℃, keeping the temperature for 2 hours, cooling the furnace, cleaning the furnace body for 3 times by using clean water, and drying the furnace body in a 100 ℃ drying oven to obtain the modified material carrier.
The specific surface area of the porous resin before and after the test treatment is reduced from 576 square meters per gram to 420 square meters per gram.
(2) And (2) soaking the modified material carrier in an acetic acid solution with the mass fraction of 0.7% for 20min, and then drying at 120 ℃ to obtain the soaked carrier.
(3) Soaking the soaked carrier into a mixed solution of 2mol/L cerium nitrate, 0.2mol/L manganese nitrate and 0.5mol/L ammonia water solution in an equal volume ratio of 0.1: 0.5:3. Continuously stirring for 10min, reacting at 100 ℃ for 24h, calcining in a muffle furnace at 200 ℃ for 2h, washing the calcined sample for 3 times by pure water, and drying at 100 ℃.
And (3) product testing: 100g of the above-mentioned amine deodorizing material is placed in a filter element, and the wind speed is 200m3H, initial ammonia concentration 2mg/m3The ammonia removal rate per unit time was 35%.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Claims (10)
1. The preparation method of the amine odor removal material is characterized by comprising the following steps:
(1) carrying out hydrothermal treatment on the adsorption material in the reactor by using an inorganic salt solution, and cleaning and drying to obtain a modified material carrier;
(2) soaking the modified material carrier in an acid solution and then drying to obtain a soaked carrier;
(3) preparing a catalytic activity precursor solution, soaking the soaked carrier into the catalytic activity precursor solution again in the same volume, performing heat preservation reaction, and then roasting to obtain the catalyst.
2. The amine deodorant material according to claim 1, wherein the adsorbent in the step (1) is a porous adsorbent not containing an acidic functional group;
preferably, the adsorbent material is one or more of zeolite, porous resin, activated alumina, diatomaceous earth or porous silica.
3. The amine deodorant material according to claim 1 or 2, wherein the inorganic salt solution in the step (1) is one or a mixture of more of an aqueous ammonia solution, an ammonium chloride solution or an ammonium dihydrogen phosphate solution having a mass concentration of 5% to 50%.
4. The amine deodorizing material as defined in claim 3, wherein the hydrothermal treatment in step (1) is carried out by atomizing the inorganic salt solution, introducing into the reactor at a rate of 5-10ml/min, controlling the temperature rise rate at 1-20 ℃/min, the treatment temperature at 120-700 ℃, and the treatment time at 0.5-6h, and then cooling and cooling with a furnace.
5. The amine deodorant material according to claim 1, wherein the acidic solution in the step (2) is one or more of phosphoric acid, acetic acid and formic acid with a mass concentration of 1-5%.
6. The deodorizing material according to claim 1 or 5, wherein the dipping time in the step (2) is 30 to 180min and the drying temperature is 90 to 150 ℃.
7. The amine deodorant material according to claim 1, wherein in the step (3), the catalytically active precursor solution is a mixed solution of a cerium salt solution, a manganese salt solution and an alkaline solution.
8. The amine deodorant material according to claim 7, wherein the volume ratio of the cerium salt solution, the manganese salt solution and the alkaline solution is 0.2-4:0.1-5: 1-10.
9. The amine deodorant material according to claim 7 or 8, wherein the cerium salt solution is one or more of cerium nitrate, cerium sulfate or cerium chloride; the manganese salt solution is one or more of manganese acetate, manganese chloride, manganese sulfate or manganese nitrate; the alkaline solution is sodium hydroxide, potassium hydroxide or ammonia water solution;
preferably, the molar concentration of the cerium salt solution is 0.1-1mol/L, the molar concentration of the manganese salt solution is 0.3-3mol/L, and the molar concentration of the alkaline solution is 2-10 mol/L.
10. The amine deodorant material according to claim 1, wherein in the step (3), the temperature of the incubation reaction is 60-100 ℃ for 12-24 hours; the roasting is carried out for 2-6h in a muffle furnace at the temperature of 300-500 ℃;
preferably, the calcined sample is dried after being washed for 2-3 times by pure water;
preferably, during the equal volume impregnation, stirring is continued for 0.5-3 h.
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