CN111905702A - Preparation method of porous particle filter material loaded with nano zero-valent iron for adsorbing and removing heavy metals in water - Google Patents
Preparation method of porous particle filter material loaded with nano zero-valent iron for adsorbing and removing heavy metals in water Download PDFInfo
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- CN111905702A CN111905702A CN201910401357.3A CN201910401357A CN111905702A CN 111905702 A CN111905702 A CN 111905702A CN 201910401357 A CN201910401357 A CN 201910401357A CN 111905702 A CN111905702 A CN 111905702A
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- 239000000463 material Substances 0.000 title claims abstract description 112
- 239000002245 particle Substances 0.000 title claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 60
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 50
- 238000005245 sintering Methods 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000011148 porous material Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 19
- 239000004113 Sepiolite Substances 0.000 claims description 18
- 229910052624 sepiolite Inorganic materials 0.000 claims description 18
- 235000019355 sepiolite Nutrition 0.000 claims description 18
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000005995 Aluminium silicate Substances 0.000 claims description 12
- 229910021536 Zeolite Inorganic materials 0.000 claims description 12
- 235000012211 aluminium silicate Nutrition 0.000 claims description 12
- 239000000440 bentonite Substances 0.000 claims description 12
- 229910000278 bentonite Inorganic materials 0.000 claims description 12
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 12
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 12
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 12
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 12
- 239000010457 zeolite Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 230000004048 modification Effects 0.000 claims description 10
- 238000012986 modification Methods 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 6
- 239000004005 microsphere Substances 0.000 claims description 6
- 238000006479 redox reaction Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000001694 spray drying Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000003463 adsorbent Substances 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 4
- -1 iron ions Chemical class 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 229910010277 boron hydride Inorganic materials 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 24
- 239000002351 wastewater Substances 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 9
- 238000001035 drying Methods 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000011133 lead Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 238000009851 ferrous metallurgy Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Substances [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
Images
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3028—Granulating, agglomerating or aggregating
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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
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3042—Use of binding agents; addition of materials ameliorating the mechanical properties of the produced sorbent
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
- B01J20/3064—Addition of pore forming agents, e.g. pore inducing or porogenic agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
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- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a preparation method of a porous granular filter material loaded with nano zero-valent iron for adsorbing and removing heavy metals in water, which comprises the following steps of 1) preparing a porous granular filter material precursor with porosity of 65-90% by sintering, and 2) generating and attaching nano zero-valent iron particles on the surface and internal pore points of the porous granular filter material precursor by chemical reaction, thereby completing the preparation of the porous granular filter material loaded with the nano zero-valent iron. 1. The preparation process is simple, the required conditions are mild, and the method has a mass production prospect. 2. The raw materials are low in price, easy to purchase in large quantities and low in preparation cost. 3. The porous granular filter material loaded with the nano zero-valent iron has high-efficiency adsorption capacity on heavy metal elements in heavy metal wastewater, and can form good economic and social benefits in the environmental field as a special water treatment agent for the heavy metal wastewater.
Description
Technical Field
The invention belongs to the technical field of heavy metal wastewater treatment, and particularly relates to a preparation method of a porous particle filter material loaded with nano zero-valent iron for adsorbing and removing heavy metals in water.
Background
With the rapid development of industrial economy, a large amount of industrial wastewater containing heavy metals is generated, and most of the heavy metal wastewater comes from the industries such as electroplating, ferrous metallurgy, mines, petrochemical industry and the like, and has great harm to the environment and human health. Therefore, the harmless treatment of heavy metal wastewater is a difficult problem to be solved at present, wherein the heavy metal wastewater pollution caused by the electroplating industry, the ferrous metallurgy industry and the petrochemical industry is particularly prominent.
The traditional method of using organic resin ion exchange to remove heavy metals from heavy metal wastewater is one of relatively simple and effective means. The practical application is greatly limited due to the defects of poor heat resistance, low saturated adsorption capacity and the like of the organic resin. The chemical precipitation method is to put a certain amount of chemical flocculant, such as potassium aluminum sulfate, polyaluminium chloride, ferric chloride and the like, into the wastewater, and sometimes, coagulant aids, such as active silica, clay, polyelectrolyte and the like, are also needed to be added, and the chemical precipitation method has the advantages that: simple method, low cost, wide element removing types, and mature technology and equipment. The disadvantages are that: heavy metal elements in the sediment are easy to leach out, and meanwhile, the generated sludge needs to be concentrated, dehydrated, solidified and the like, otherwise, secondary pollution is easily caused. The membrane treatment is used as a mature heavy metal wastewater treatment method, has higher requirements on the quality of raw water, has higher difficulty in one-step standard discharge of heavy metal wastewater with more complex treatment components, and has complex equipment and process and higher investment cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a porous particle filter material loaded with nano zero-valent iron for adsorbing and removing heavy metals in water, which has the advantages of simple preparation process, mild required conditions and mass production prospect.
The invention is realized by the following technical scheme:
a preparation method of a porous particle filter material loaded with nano zero-valent iron for adsorbing and removing heavy metals in water comprises the following steps,
1) preparing a porous granular filter material precursor with the porosity of 65-90 percent by a sintering mode,
2) nanometer zero-valent iron particles are generated and attached to the surface and the internal pore points of the porous granular filter material precursor through chemical reaction, so that the preparation of the nanometer zero-valent iron-loaded porous granular filter material is completed.
In the technical scheme, the particle filter material precursor comprises an adsorbent, a sintering aid, a binder and a pore-forming agent according to the mass ratio of 80-120: 4-10: 10-12: 9-13.
In the technical scheme, the adsorbent is formed by mixing active alumina and any one of zeolite powder, sepiolite and diatomite according to the mass ratio of 1 (6-8), wherein when the porous granular filter material precursor is prepared, any one of the zeolite powder, the sepiolite and the diatomite is subjected to acid modification before use.
In the technical scheme, the acid modification is carried out by soaking and modifying with 3-4 mol/L hydrochloric acid.
In the technical scheme, the sintering aid is common kaolin.
In the technical scheme, the pore-forming agent is any one of carbon powder, alumina hollow spheres and hollow glass microspheres, and the particle size of the pore-forming agent is 5-10 micrometers.
In the technical scheme, the binder is formed by mixing bentonite and hydroxymethyl cellulose according to the mass ratio of (5-10) to 1.
In the technical scheme, the grain size of the porous particle filter material loaded with the nano zero-valent iron is 2-3 mm.
In the technical scheme, the granular filter material consists of the raw materials in parts by weight,
10-14 parts of activated alumina;
70-100 parts of any one of zeolite powder, sepiolite and diatomite;
4-10 parts of common kaolin;
8-10 parts of bentonite;
1-2 parts of hydroxymethyl cellulose;
9-13 parts of any one of carbon powder, alumina hollow spheres and hollow glass microspheres.
In the technical scheme, the method comprises the following steps,
1) selecting any one of zeolite powder, sepiolite and diatomite for acid modification, adding 3-4 mol/L hydrochloric acid aqueous solution, stirring and reacting for 1-2 h, then washing with deionized water until effluent liquid is neutral, and completing modification after vacuum drying;
2) mixing the prepared modified zeolite powder, sepiolite or diatomite, activated alumina, common kaolin, bentonite, hydroxymethyl cellulose and carbon powder together according to a formula proportion, adding deionized water, uniformly mixing, wherein the deionized water accounts for 15% -20% of the whole mass, performing spray drying on the mixed material, preparing small balls with the particle size of 2-3 mm, performing high-temperature sintering on the prepared small balls at 950-1260 ℃, and performing heat preservation for 3-4 hours to obtain a porous granular filter material precursor;
3) slowly injecting Fe into the prepared porous particle filter material precursor3+The water solution with the concentration of 0.6-1 mol/L is used until the porous granular filter material precursor is completely soaked in the water solution, and after soaking for 30min, the porous granular filter material precursor is taken out and placed in an oven to be dried for later use at the temperature of 100-120 ℃;
4) slowly injecting BH into the prepared porous particle filter material precursor4-The water solution with the concentration of 0.8-1.2 mol/L is used until the porous granular filter material precursor is completely soaked in the water solution, oxidation-reduction reaction is carried out, the porous granular filter material precursor is taken out after being soaked for 20min, and vacuum drying is carried out;
5) and (3) carrying out anaerobic sintering on the porous particle filter material precursor prepared in the step (4) under the protection of nitrogen or other inert gases, wherein the sintering temperature is 500-600 ℃, and preserving heat for 2 hours to obtain the nano zero-valent iron-loaded porous particle filter material.
In the above technical scheme, the aqueous solution containing iron ions in step (3) is an aqueous solution of ferric chloride or ferric sulfate.
In the above technical scheme, the aqueous solution containing borohydride ions in the step (4) is sodium borohydride or potassium borohydride aqueous solution.
The invention has the advantages and beneficial effects that:
the particle size of the obtained filter material is 2-3 mm, the specific surface area of the filter material particles is large, the adsorption capacity is large, nano zero-valent iron particles generated and attached to the surfaces and the internal pore points of the filter material particles have good dispersibility and extremely high reaction activity, and the filter material has excellent reduction fixation and adsorption removal effects on heavy metal elements such as nickel, chromium, lead and the like in heavy metal wastewater, and more experimental results show that the filter material also has good adsorption effects on radionuclides such as strontium, cesium and the like.
The filter material particles synthesized by the invention also have the following advantages: 1. the preparation process is simple, the required conditions are mild, and the method has a mass production prospect. 2. The raw materials are low in price, easy to purchase in large quantities and low in preparation cost. 3. The porous granular filter material loaded with the nano zero-valent iron has high-efficiency adsorption capacity on heavy metal elements in heavy metal wastewater, and can form good economic and social benefits in the environmental field as a special water treatment agent for the heavy metal wastewater.
Drawings
FIG. 1 is a scanning electron microscope photograph of a porous particle filter material loaded with nanoscale zero-valent iron prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope photograph of the porous particle filter material loaded with nanoscale zero-valent iron prepared in example 2 of the present invention;
fig. 3 shows the surface structure of the filter material loaded with nano zero-valent iron porous particles prepared in example 3 of the present invention under an electron microscope with a magnification of 3000 times.
For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention is further described below with reference to specific examples.
Example 1
The first step is as follows: weighing 10 parts of activated alumina, 70 parts of zeolite powder, 4 parts of common kaolin, 10 parts of bentonite, 1 part of hydroxymethyl cellulose and 10 parts of carbon powder.
The second step is that: slowly injecting 3mol/L hydrochloric acid into the zeolite powder until the zeolite powder is completely immersed, stirring and reacting for 1h, then washing the mixture by deionized water until the effluent liquid is neutral, and drying the mixture in vacuum to obtain the modified zeolite powder.
The third step: adding deionized water accounting for 15 percent of the whole mass into the activated alumina, the modified zeolite powder, the common kaolin, the bentonite, the hydroxymethyl cellulose and the carbon powder, and uniformly mixing. And (3) carrying out spray drying on the mixed material to prepare small balls with the particle size of 2-3 mm. And sintering the prepared small balls at a high temperature of 950 ℃, and preserving heat for 3 hours to obtain the porous granular filter material precursor.
The fourth step: slowly injecting 0.6mol/L FeCl into the porous particle filter material precursor3And (3) completely soaking the aqueous solution to the porous granular filter material precursor in the aqueous solution for 30min, taking out the porous granular filter material precursor, and drying the porous granular filter material precursor in an oven at 100 ℃ for later use.
The fifth step: and (3) slowly injecting a sodium borohydride aqueous solution with the concentration of 1mol/L into the porous particle filter material precursor prepared in the fourth step until the porous particle filter material precursor is completely soaked in the aqueous solution, and carrying out oxidation-reduction reaction. Soaking for 20min, taking out, and vacuum drying.
And a sixth step: and (3) carrying out anaerobic sintering on the porous particle filter material precursor prepared in the fifth step under the protection of nitrogen or other inert gases, wherein the sintering temperature is 500 ℃, and keeping the temperature for 2 hours to obtain the nano zero-valent iron-loaded porous particle filter material.
Example 2
The first step is as follows: weighing 12 parts of active alumina, 85 parts of sepiolite powder, 7 parts of common kaolin, 10 parts of bentonite, 1.5 parts of hydroxymethyl cellulose and 9 parts of alumina hollow spheres by weight.
The second step is that: slowly injecting 4mol/L hydrochloric acid into the sepiolite powder until the sepiolite powder is completely immersed, stirring and reacting for 2 hours, then washing the sepiolite powder by deionized water until effluent liquid is neutral, and drying the sepiolite powder in vacuum to obtain the modified sepiolite powder.
The third step: adding deionized water accounting for 15 percent of the whole mass into the activated alumina, the modified sepiolite powder, the common kaolin, the bentonite, the hydroxymethyl cellulose and the alumina hollow spheres, and uniformly mixing the materials together. And (3) carrying out spray drying on the mixed material to prepare small balls with the particle size of 2-3 mm. And sintering the prepared pellets at a high temperature of 1000 ℃, and preserving heat for 3 hours to obtain the porous granular filter material precursor.
The fourth step: slowly injecting 0.4mol/L Fe into the porous particle filter material precursor2(SO4)3And (3) completely soaking the aqueous solution to the porous granular filter material precursor in the aqueous solution for 30min, taking out the porous granular filter material precursor, and drying the porous granular filter material precursor in an oven at 100 ℃ for later use.
The fifth step: and slowly injecting a sodium borohydride aqueous solution with the concentration of 1.2mol/L into the porous granular filter material precursor prepared in the fourth step until the porous granular filter material precursor is completely soaked in the aqueous solution, and carrying out oxidation-reduction reaction. Soaking for 20min, taking out, and vacuum drying.
And a sixth step: and (3) carrying out anaerobic sintering on the porous particle filter material precursor prepared in the fifth step under the protection of nitrogen or other inert gases, wherein the sintering temperature is 500 ℃, and keeping the temperature for 2 hours to obtain the nano zero-valent iron-loaded porous particle filter material.
Example 3
The first step is as follows: weighing 14 parts of activated alumina, 100 parts of diatomite, 10 parts of common kaolin, 10 parts of bentonite, 2 parts of hydroxymethyl cellulose and 13 parts of hollow glass microspheres in parts by weight.
The second step is that: slowly injecting 3mol/L hydrochloric acid into the diatomite until the diatomite is completely immersed, stirring and reacting for 2 hours, then washing the diatomite with deionized water until the effluent liquid is neutral, and drying the diatomite in vacuum to obtain the modified diatomite.
The third step: deionized water accounting for 20 percent of the whole mass is added into the activated alumina, the modified diatomite, the common kaolin, the bentonite, the hydroxymethyl cellulose and the hollow glass microspheres and mixed uniformly. And (3) carrying out spray drying on the mixed material to prepare small balls with the particle size of 2-3 mm. And sintering the prepared pellets at 1250 ℃ for 3h to obtain the porous granular filter material precursor.
The fourth step: slowly injecting 1mol/L FeCl into the porous particle filter material precursor3And (3) completely soaking the aqueous solution to the porous granular filter material precursor in the aqueous solution for 30min, taking out the porous granular filter material precursor, and drying the porous granular filter material precursor in a drying oven at 120 ℃ for later use.
The fifth step: slowly injecting 1.2mol/L potassium borohydride water solution into the porous particle filter material precursor prepared in the fourth step until the porous particle filter material precursor is completely soaked in the water solution, and carrying out oxidation-reduction reaction. Soaking for 20min, taking out, and vacuum drying.
And a sixth step: and (3) carrying out anaerobic sintering on the porous particle filter material precursor prepared in the fifth step under the protection of nitrogen or other inert gases, wherein the sintering temperature is 600 ℃, and keeping the temperature for 2 hours to obtain the porous particle filter material loaded with the nano zero-valent iron.
Effect example 1
The performance tests of the porous filter materials loaded with nanoscale zero-valent iron prepared in example 1, example 2 and example 3 are performed, and the test results are shown in table 1.
TABLE 1
Effect example 2
Pb using the porous particulate filter loaded with nano-zero-valent iron prepared in example 12+Static adsorption experiment, 1g of granular filter material and 10mg/L Pb were added to a beaker2+The solution (100 ml) was statically adsorbed at room temperature for 0.5 h. Taking a proper amount of the solution, centrifuging for 5 minutes at 3000r/min, taking the residual Pb in 1ml of test solution of the supernatant2+Concentration, detected residual Pb2+The concentration is 1.27mg/L, and the removal rate reaches 87.3 percent.
At the same time, for an initial concentration of 20mg/L Pb2+Solution, 50mg/L Pb2+The solution is statically adsorbed for 0.5h by using the nano zero-valent iron-loaded porous particle filter material prepared in example 1, and then Pb is obtained2+The removal rates are 82.2 percent and 74.3 percent respectively, and Pb is obtained after static adsorption for 3.5 hours2+The removal rates were 86% and 77.8%, respectively.
Effect example 3
Ni Using the porous particulate filter loaded with nano-zero-valent iron prepared in example 12+Dynamic adsorption experiment, washing the porous particle filter material loaded with nano zero-valent iron with deionized water, loading into an adsorption column, and circulating 10mg/L NiCl with a circulating pump2The solution is injected into an adsorption column, dynamic adsorption filtration is carried out by adopting a mode of lower water inlet and upper water outlet, and a water outlet is sampled and detected for Ni every 30s2+And (4) concentration. Tests show that the filter material loaded with the nano zero-valent iron porous particles is used for carrying out dynamic adsorption experiment on 10mg/L NiCl2Ni in solution2+The removal efficiency was over 96%, and some of the test results are shown in table 2. Meanwhile, the nano-zero-valent iron-loaded porous particle filter material prepared in example 1 is matched with 1mg/L NiCl2Ni in solution2+The dynamic adsorption removal efficiency is more than 98%.
TABLE 2
| Effluent sample | Water sample 1 | Water sample 2 | Water sample 3 | Water sample 4 |
| Ni2+Concentration (mg/L) | 0.23 | 0.3 | 0.34 | 0.31 |
| Removal efficiency (%) | 97.7 | 97 | 96.6 | 96.9 |
Effect example 4
Chromium dynamic adsorption experiments were performed using the loaded nano zero-valent iron porous particulate filter material prepared in example 3, configured with 10mg/L K using analytically pure potassium dichromate2CrO4The solution simulates chromium-containing wastewater. Washing the porous particle filter material loaded with the nano zero-valent iron with deionized water, then loading the washed porous particle filter material into an adsorption column, and using a circulating pump to pump 10mg/L K2CrO4The solution is injected into an adsorption column, dynamic adsorption filtration is carried out by adopting a mode of lower water inlet and upper water outlet, and the CrO is sampled and detected at the water outlet every 30s4 2-And (4) concentration. Tests show that the nano zero-valent iron loaded porous particle filter material can carry out the dynamic adsorption experiment on 10mg/L K2CrO4CrO in solution4 2-The removal efficiency was over 90%, and some of the test results are shown in table 4.
TABLE 3
| Effluent sample | Water sample 1 | Water sample 2 | Water sample 3 | Water sample 4 |
| CrO4 2-Concentration (mg/L) | 0.61 | 0.5 | 0.58 | 0.7 |
| Removal efficiency (%) | 93.9 | 95 | 94.2 | 93 |
According to the loaded nano zero-valent iron porous granular filter material for adsorbing and removing heavy metals in water, calcium salt, organic matters and other impurities are dissolved out after the zeolite powder, the sepiolite powder or the diatomite is subjected to acid modification, so that holes and pore canals are dredged and effective space is widened. In particular, the added activated alumina has the characteristics of larger specific surface area, high dispersity and porosity, and can increase the adsorption active center and the pores of the filter material and improve the adsorption capacity and the overall activity of the filter material.
The nano zero-valent iron in the porous particle filter material loaded with the nano zero-valent iron has high reaction activity, is easy to perform oxidation-reduction reaction with hexavalent chromium plasma in heavy metal wastewater, and can ensure that the removal rate of the heavy metal in the wastewater reaches more than 90% through chemical reduction, action and physical adsorption fixation without dissolving out secondary pollutants; the increase of structures can be reduced in the heavy metal ion adsorption process. Meanwhile, the filter material has the advantages of uniform particle appearance, controllable size, good mechanical strength and convenient use, and can be filled in containers such as adsorption columns, exchange towers and the like.
The preparation method provided by the invention has the advantages of low price of raw materials, mild preparation conditions, simple required equipment and mass production prospect, and is suitable for large-scale application in the field of heavy metal wastewater treatment.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (12)
1. A preparation method of a porous particle filter material loaded with nano zero-valent iron for adsorbing and removing heavy metals in water is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
1) preparing a porous granular filter material precursor with the porosity of 65-90 percent by a sintering mode,
2) nanometer zero-valent iron particles are generated and attached to the surface and the internal pore points of the porous granular filter material precursor through chemical reaction, so that the preparation of the nanometer zero-valent iron-loaded porous granular filter material is completed.
2. The preparation method of the porous particle filter material loaded with the nano zero-valent iron for adsorbing and removing the heavy metals in the water according to claim 1, is characterized in that: the particle filter material precursor comprises an adsorbent, a sintering aid, a binder and a pore-forming agent according to the mass ratio of 80-120: 4-10: 10-12: 9-13.
3. The preparation method of the porous particle filter material loaded with the nano zero-valent iron for adsorbing and removing the heavy metals in the water according to claim 2, is characterized in that: the adsorbent is formed by mixing active alumina and any one of zeolite powder, sepiolite and diatomite according to the mass ratio of 1 to (6-8), wherein when the porous granular filter material precursor is prepared, any one of the zeolite powder, the sepiolite and the diatomite is subjected to acid modification before use.
4. The preparation method of the porous particle filter material loaded with the nano zero-valent iron for adsorbing and removing the heavy metals in the water according to claim 3, which is characterized by comprising the following steps: the acid modification is carried out by soaking and modifying with 3-4 mol/L hydrochloric acid.
5. The preparation method of the porous particle filter material loaded with the nano zero-valent iron for adsorbing and removing the heavy metals in the water according to claim 2, is characterized in that: the sintering aid is common kaolin.
6. The preparation method of the porous particle filter material loaded with the nano zero-valent iron for adsorbing and removing the heavy metals in water according to claim 2, wherein the pore-forming agent is any one of carbon powder, alumina hollow spheres and hollow glass microspheres, and the particle size of the pore-forming agent is 5-10 microns.
7. The preparation method of the porous particle filter material loaded with the nano zero-valent iron for adsorbing and removing the heavy metals in the water according to claim 2, is characterized in that: the binder is prepared by mixing bentonite and hydroxymethyl cellulose according to the mass ratio of (5-10) to 1.
8. The preparation method of the porous particle filter material loaded with the nano zero-valent iron for adsorbing and removing the heavy metals in the water according to claim 1, is characterized in that: the particle size of the porous particle filter material loaded with the nano zero-valent iron is 2-3 mm.
9. The preparation method of the porous particle filter material loaded with the nano zero-valent iron for adsorbing and removing the heavy metals in the water according to claim 1, is characterized in that: the granular filter material consists of the raw materials in parts by weight,
10-14 parts of activated alumina;
70-100 parts of any one of zeolite powder, sepiolite and diatomite;
4-10 parts of common kaolin;
8-10 parts of bentonite;
1-2 parts of hydroxymethyl cellulose;
9-13 parts of any one of carbon powder, alumina hollow spheres and hollow glass microspheres.
10. The preparation method of the porous particle filter material loaded with the nano zero-valent iron for adsorbing and removing the heavy metals in the water according to claim 9, is characterized in that: comprises the following steps of (a) carrying out,
1) selecting any one of zeolite powder, sepiolite and diatomite for acid modification, adding 3-4 mol/L hydrochloric acid aqueous solution, stirring and reacting for 1-2 h, then washing with deionized water until effluent liquid is neutral, and completing modification after vacuum drying;
2) mixing the prepared modified zeolite powder, sepiolite or diatomite, activated alumina, common kaolin, bentonite, hydroxymethyl cellulose and carbon powder together according to a formula proportion, adding deionized water, uniformly mixing, wherein the deionized water accounts for 15% -20% of the whole mass, performing spray drying on the mixed material, preparing small balls with the particle size of 2-3 mm, performing high-temperature sintering on the prepared small balls at 950-1260 ℃, and performing heat preservation for 3-4 hours to obtain a porous granular filter material precursor;
3) slowly injecting Fe into the prepared porous particle filter material precursor3+The water solution with the concentration of 0.6-1 mol/L is used until the porous granular filter material precursor is completely soaked in the water solution, and after soaking for 30min, the porous granular filter material precursor is taken out and placed in an oven to be dried for later use at the temperature of 100-120 ℃;
4) slowly injecting BH into the prepared porous particle filter material precursor4-The water solution with the concentration of 0.8-1.2 mol/L is used until the porous granular filter material precursor is completely soaked in the water solution, oxidation-reduction reaction is carried out, the porous granular filter material precursor is taken out after being soaked for 20min, and vacuum drying is carried out;
5) and (3) carrying out anaerobic sintering on the porous particle filter material precursor prepared in the step (4) under the protection of nitrogen or other inert gases, wherein the sintering temperature is 500-600 ℃, and preserving heat for 2 hours to obtain the nano zero-valent iron-loaded porous particle filter material.
11. The preparation method of the porous particle filter material loaded with the nano zero-valent iron for adsorbing and removing the heavy metals in the water according to claim 10, is characterized in that: the aqueous solution containing iron ions in the step (3) is ferric chloride or ferric sulfate aqueous solution.
12. The preparation method of the porous particle filter material loaded with the nano zero-valent iron for adsorbing and removing the heavy metals in the water according to claim 10, is characterized in that: the aqueous solution containing the boron hydride ions in the step (4) is sodium borohydride or potassium borohydride aqueous solution.
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