CN113275018A - Process method for preparing supported catalyst by recycling heavy metals in polluted water sample - Google Patents
Process method for preparing supported catalyst by recycling heavy metals in polluted water sample Download PDFInfo
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- CN113275018A CN113275018A CN202110621150.4A CN202110621150A CN113275018A CN 113275018 A CN113275018 A CN 113275018A CN 202110621150 A CN202110621150 A CN 202110621150A CN 113275018 A CN113275018 A CN 113275018A
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- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 58
- 239000003054 catalyst Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000004064 recycling Methods 0.000 title claims abstract description 12
- 230000008569 process Effects 0.000 title claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002244 precipitate Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000009388 chemical precipitation Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 239000001301 oxygen Substances 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 230000001376 precipitating effect Effects 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000007873 sieving Methods 0.000 claims abstract description 5
- 238000011068 loading method Methods 0.000 claims abstract description 4
- 239000000084 colloidal system Substances 0.000 claims abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 229910052878 cordierite Inorganic materials 0.000 claims description 5
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 150000002910 rare earth metals Chemical class 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 229910052723 transition metal Inorganic materials 0.000 claims description 4
- 150000003624 transition metals Chemical class 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 3
- 229910001593 boehmite Inorganic materials 0.000 claims description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 3
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- 239000013618 particulate matter Substances 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 23
- 239000002351 wastewater Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 231100000693 bioaccumulation Toxicity 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000002920 hazardous waste Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- 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
- 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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/86—Chromium
- B01J23/868—Chromium copper and chromium
-
- 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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention relates to the technical field of environmental protection, in particular to a process method for preparing a supported catalyst by recycling heavy metals in a polluted water sample. The method comprises the following steps of precipitating heavy metal ions in a polluted water sample by using a chemical precipitation method, and performing solid-liquid separation to obtain a solid heavy metal precipitate; carrying out pretreatment such as cleaning, crushing, grinding, sieving and the like on the solid heavy metal precipitate to obtain fine granular heavy metal-containing powder; preparing an aluminum sol colloidal solution; adding the fine powder containing the heavy metal prepared in the step 2) into the aluminum sol colloidal solution, and uniformly stirring to obtain a uniformly dispersed aluminum sol colloidal solution containing the heavy metal; and loading the colloid on an integral carrier, and roasting in an oxygen-containing atmosphere to obtain the supported catalyst.
Description
The technical field is as follows:
the invention relates to the technical field of environmental protection, in particular to a process method for preparing a supported catalyst by recycling heavy metals in a polluted water sample.
Background art:
in natural environment, heavy metal elements in different forms have nondegradable property and bioaccumulation property, and even if the heavy metal content of a polluted water sample discharged by an industrial enterprise is very small, the polluted water sample can be transmitted through the bioaccumulation property and a food chain, so that an ecological system and human health are influenced. The chemical precipitation method is one of the main methods for treating heavy metal pollution, however, the generated heavy metal sludge is often required to be treated as dangerous waste, and the operation cost of enterprises is increased.
The catalyst can reduce the activation energy of the reaction, and is widely applied in the field of environmental protection. The catalyst has a great deal of application in the fields of power plant flue gas denitration, automobile exhaust three-way catalysts, catalytic combustion degradation of volatile organic compounds and the like; in the field of wastewater treatment, ozone catalytic oxidation in water can accelerate the generation of hydroxyl radicals with strong oxidizing property due to the addition of a catalyst, thereby promoting the degradation rate of organic matters in water, and the method is an advanced oxidation technology with a prospect.
Common active components of the catalyst include noble metals, transition metal oxides and rare earth metal oxides, such as platinum, palladium, iron, nickel, copper, manganese, zinc, zirconium, cerium, and the like. Most of the elements are just the main components of the heavy metal polluted water sample of the industrial enterprise. Therefore, the heavy metal components in the wastewater can be recycled by technical means to prepare the industrial catalyst. Not only solves the problem of heavy metal water body pollution, but also saves the treatment cost of hazardous waste for enterprises, and produces the catalyst to generate economic benefit. For a polluted water sample containing multi-component heavy metal elements, the precipitate formed by the precipitation method also contains a plurality of components, which is not beneficial to the subsequent purification of the complex composite oxide and reduces the value of the complex composite oxide in the traditional recycling.
The invention content is as follows:
the invention aims at the problems and provides a process method for preparing a supported catalyst by recycling heavy metals in a polluted water sample, which recycles heavy metal elements in water pollution and is used for producing an industrial catalyst.
In order to achieve the purpose, the invention adopts the following technical scheme that the method comprises the following process steps,
1. precipitating heavy metal ions in a polluted water sample by using a chemical precipitation method, and performing solid-liquid separation to obtain a solid heavy metal precipitate;
2. carrying out pretreatment such as cleaning, crushing, grinding, sieving and the like on the solid heavy metal precipitate to obtain fine granular heavy metal-containing powder;
3. uniformly dispersing pseudo-thin alumina into water, and continuously adding acid liquor until the liquid is changed into sol solution from suspension to obtain alumina sol colloidal solution;
4. adding the fine powder containing the heavy metal prepared in the step 2) into the aluminum sol colloidal solution, and uniformly stirring to obtain a uniformly dispersed aluminum sol colloidal solution containing the heavy metal, wherein the heavy metal powder accounts for 5-40% of the total mass;
5. and loading the colloid on an integral carrier, and roasting in an oxygen-containing atmosphere to obtain the supported catalyst.
The precipitating agent used in the chemical precipitation method in the step 1 is sodium bicarbonate, sodium carbonate, sodium hydroxide or hydrogen sulfide, and the molar ratio of the precipitating agent to heavy metal ions in water is 1-3: 1, pH > 7.2.
The particle size of the heavy metal precipitate after pretreatment in the step 2 is less than 0.1-0.5 mm, and the fine heavy metal precipitate after pretreatment can be subjected to acid corrosion, so that the specific surface area of the particles is increased.
In the step 3, the weight ratio of the boehmite to the water is 1: 5-15, wherein the acid is concentrated nitric acid with the concentration of 68 wt%.
The alumina sol colloidal solution prepared in the step 3 can be modified by more than one component of transition metal and rare earth metal, wherein the transition metal is iron, cobalt, nickel, manganese, zinc or copper, and the rare earth metal is cerium or lanthanum.
In the step 5, loading the aluminum sol containing the catalyst active component on a catalyst carrier by adopting an impregnation method or a pulling method, and oxidizing and decomposing the heavy metal precipitate, the modified component and the aluminum sol into the active component in an oxygen-containing atmosphere; the catalyst carrier can be in a honeycomb shape, a granular shape or a strip shape, and the component can be cordierite, alumina or molecular sieve.
The prepared supported catalyst can also be added with noble metal active components to improve the activity of the catalyst.
The invention has the beneficial effects that:
the method recycles heavy metal elements in water body pollution to produce the industrial catalyst, solves the problem of water body heavy metal pollution, saves the treatment cost of hazardous waste of heavy metal sludge, produces the industrial catalyst, generates economic benefit, and has obvious environmental benefit and economic benefit
The specific implementation mode is as follows:
the following examples are given to further illustrate the preparation of the catalyst, but the present invention is not limited to these examples.
Example 1
The electroplating wastewater discharged from a certain electroplating plant contains heavy metal ions such as nickel, chromium, copper and zinc, wherein the total nickel content is 200-300 mg/L, the total chromium content is 150-200 mg/L, the total copper content is 200-300 mg/L, and the total zinc content is 50-100 mg/L. Adding 0.3 wt% of sodium hydroxide into water by adopting a chemical precipitation method to form hydroxide precipitate insoluble in water, and performing solid-liquid separation on the precipitate by adopting inclined plate precipitation and plate-frame filter pressing to obtain multi-component hydroxide precipitate;
cleaning the precipitate, grinding, and sieving with 200 mesh sieve to obtain fine powder with heavy metal content less than 75 um;
according to the water: the boehmite is 10: 1, dropwise adding 68 wt% concentrated nitric acid solution while magnetically stirring until an aluminum sol colloidal solution is formed, wherein the pH value of the solution is between 2 and 5;
putting the obtained powder into the prepared aluminum sol colloidal solution, wherein the mass ratio of the powder to the prepared aluminum sol colloidal solution is 1: 5, uniformly stirring to obtain a uniformly dispersed multi-component heavy metal-containing aluminum sol solution;
taking granular activated alumina with the particle size of 3-8mm as a catalyst carrier, putting the granular activated alumina into the prepared aluminum sol colloidal solution, soaking for 20min, and taking out to obtain a catalyst carrier which takes the granular alumina as a carrier and is loaded with aluminum sol and heavy metal-containing component powder on the surface of the carrier;
placing the obtained alumina in a muffle furnace, drying at 100 ℃ for 2h in air atmosphere, and roasting at 550 ℃ for 4h to obtain the alumina serving as a first carrier, an activated alumina coating oxidized by alumina sol serving as a second carrier, wherein Cr is embedded in the second carrier2O3-NiO-CuO-ZnO composite oxide supported industrial catalyst.
Example 2
The difference from example 1 is that after the preparation of the alumina sol colloidal solution, La (NO) was put into the colloidal solution3)3·6H2The mass ratio of the O modified element to the alumina sol colloidal solution is 0.5%, and the O modified element is used for modifying the second carrier to adjust the distribution ratio of active components of the catalyst, so that the catalytic activity of the catalyst is improved.
Example 3
Two water samples of Ni-containing polluted wastewater and sulfate radical-containing high-concentration organic wastewater are discharged by a certain production enterprise, wherein the sulfate radical-containing high-concentration organic wastewater is reduced into H by adopting an anaerobic biological method2And S, converting the organic matters into methane. Generated H-containing2Introducing the S gas part to Ni-containing polluted wastewater for chemical precipitation reaction,
the reaction formula is as follows: a.H2S＝HS-+H+；b.HS-+Ni2+＝NiS+H+Generating NiS sediment, and performing solid-liquid separation to obtain NiS sediment;
cleaning the NiS precipitate, grinding, and sieving with a 100-mesh sieve to obtain fine powder containing heavy metal components smaller than 150 um;
weighing pseudo-boehmite, putting the pseudo-boehmite into an aqueous solution to obtain a 10 wt% solution, and dropwise adding a 68 wt% nitric acid solution while magnetically stirring until an aluminum sol colloidal solution is formed, wherein the pH value of the solution is between 2 and 3. Adding 2 wt% MnO to the aluminum sol solution2Modifying;
putting the obtained powder into the prepared modified aluminum sol colloidal solution, and uniformly stirring to obtain a uniformly dispersed NiS-containing heavy metal aluminum sol solution;
taking honeycomb cordierite as a catalyst carrier, putting the catalyst carrier into the prepared aluminum sol colloidal solution, soaking for 20min, taking out, and blowing cordierite channels with air to obtain the catalyst carrier with the cordierite as the carrier, wherein the surface of the carrier is loaded with aluminum sol and heavy metal-containing component powder;
and (2) placing the obtained alumina in a muffle furnace, drying the alumina at 80 ℃ for 2h in the air atmosphere, and roasting the alumina for 2h at 500 ℃ to obtain the supported industrial catalyst which takes the alumina as a first carrier, takes an active alumina coating oxidized by alumina sol as a second carrier, and is embedded with a Ni-Mn-Ce active component on the second carrier.
Claims (6)
1. A process for preparing a supported catalyst by recycling heavy metals in a polluted water sample is characterized by comprising the following steps,
(1) precipitating heavy metal ions in a polluted water sample by using a chemical precipitation method, and performing solid-liquid separation to obtain a solid heavy metal precipitate;
(2) carrying out pretreatment such as cleaning, crushing, grinding, sieving and the like on the solid heavy metal precipitate to obtain fine granular heavy metal-containing powder;
(3) uniformly dispersing pseudo-thin alumina into water, and continuously adding acid liquor until the liquid is changed into sol solution from suspension to obtain alumina sol colloidal solution;
(4) adding the fine powder containing the heavy metal prepared in the step 2) into the aluminum sol colloidal solution, and uniformly stirring to obtain a uniformly dispersed aluminum sol colloidal solution containing the heavy metal, wherein the heavy metal powder accounts for 5-40% of the total mass;
(5) and loading the colloid on an integral carrier, and roasting in an oxygen-containing atmosphere to obtain the supported catalyst.
2. The process method for preparing the supported catalyst by recycling the heavy metals in the polluted water sample according to claim 1, wherein the precipitant used in the chemical precipitation method in the step 1) is sodium bicarbonate, sodium carbonate, sodium hydroxide or hydrogen sulfide, and the molar ratio of the precipitant to the heavy metal ions in the water is 1-3: 1, pH > 7.2.
3. The process method for preparing the supported catalyst by recycling the heavy metals in the polluted water sample according to claim 1, wherein the particle size of the heavy metal precipitate after the pretreatment in the step 2) is less than 0.1-0.5 mm, and the fine heavy metal precipitate after the pretreatment can be subjected to acid corrosion to increase the specific surface area of the particulate matter.
4. The process method for preparing the supported catalyst by recycling the heavy metals in the polluted water sample according to claim 1, wherein the weight ratio of the boehmite to the water in the step 3) is 1: 5-15, wherein the acid is concentrated nitric acid with the concentration of 68 wt%.
5. The process method for preparing the supported catalyst by recycling the heavy metals in the polluted water sample according to claim 1, wherein the alumina sol colloidal solution prepared in the step 3) can be modified by more than one of transition metals and rare earth metals, wherein the transition metals are iron, cobalt, nickel, manganese, zinc or copper, and the rare earth metals are cerium or lanthanum.
6. The process method for preparing the supported catalyst by recycling the heavy metal in the polluted water sample according to claim 1, wherein in the step 5), the alumina sol containing the active component of the catalyst is loaded on the catalyst carrier by adopting an impregnation method or a pulling method, and the heavy metal precipitate, the modified component and the alumina sol are oxidized and decomposed into the active component in an oxygen-containing atmosphere; the catalyst carrier can be in a honeycomb shape, a granular shape or a strip shape, and the component can be cordierite, alumina or molecular sieve.
Priority Applications (1)
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