CN113617329A - Mesoporous Fe3O4One-step preparation of composite adsorbent and application thereof in treating As (III) -containing aqueous solution - Google Patents
Mesoporous Fe3O4One-step preparation of composite adsorbent and application thereof in treating As (III) -containing aqueous solution Download PDFInfo
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 49
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 26
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 17
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims abstract description 17
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000002505 iron Chemical class 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 239000012716 precipitator Substances 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 6
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- PTLRDCMBXHILCL-UHFFFAOYSA-M sodium arsenite Chemical compound [Na+].[O-][As]=O PTLRDCMBXHILCL-UHFFFAOYSA-M 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- 239000012298 atmosphere Substances 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 238000012216 screening Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 35
- 238000000034 method Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract 1
- 238000006386 neutralization reaction Methods 0.000 abstract 1
- 229910052785 arsenic Inorganic materials 0.000 description 15
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 15
- 239000000463 material Substances 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- -1 clays Chemical compound 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 208000023504 respiratory system disease Diseases 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/06—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
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—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 surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
-
- 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
-
- 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
- C02F2101/103—Arsenic compounds
Abstract
The invention discloses one-step mesoporous Fe3O4The preparation method of the composite adsorbent comprises the steps of taking ferric trichloride hexahydrate and ferrous sulfate heptahydrate as raw materials, fully dissolving the raw materials in an iron salt solution prepared in a deionized water solution, then uniformly mixing an iron salt mixed solution and a mesoporous hollow sphere template agent, adding sufficient sodium hydroxide as a precipitator and a template remover, and adding a proper amount of sodium hydroxide to precipitate Fe on the surface of the mesoporous hollow sphere3O4Simultaneously removing the hollow ball template, washing the product with a large amount of deionized water untilAfter neutralization, mesoporous Fe is obtained3O4The whole process is carried out under nitrogen atmosphere to prevent ferrous raw material from being oxidized. The invention also provides the application of the adsorbent in a high-concentration As (III) -containing aqueous solution of 100 mg/L. The invention has the advantages of simple preparation operation, low cost and high adsorption capacity, and is mesoporous Fe3O4Provides a new method for simple preparation, and provides an idea for preparing the high-efficiency As (III) adsorbent.
Description
Technical Field
The invention relates to the field of sewage treatment, in particular to mesoporous Fe3O4A preparation method of the composite adsorbent and application thereof in treating an As (III) -containing aqueous solution.
Background
Arsenic (As), commonly known As arsenic, is a highly toxic carcinogenic element widely present in the environment. Arsenic is exposed to soil or air environments through the mining and smelting of arsenic-bearing ores, and then leaches out of contaminated soil and air with rainfall and flows into surface and ground water, resulting in severe water pollution. In natural water, most of the arsenic is present in an inorganic state, i.e., As (v) and As (iii). As (III) is more toxic than As (V) and is likely to cause serious human cancer, cardiovascular and respiratory diseases. As (III) has weaker affinity to the center of the adsorbent and stronger solubility and fluidity, so that the removal difficulty is higher.
In the treatment of arsenic pollution, chemical precipitation, microbial reduction, membrane separation, phytoremediation, oxidation, flocculation, cementation, adsorption and the like have been used for treating As (iii) in sewage. Among them, the adsorption method is widely used because of its low cost, high efficiency and simple operation. Accordingly, a number of adsorbent materials have been proposed for the treatment of water contaminated with arsenic, including clays, zeolites, cellulose, alginates, chitosan, biochar, and iron oxide.
Among the materials, Fe3O4The material has high adsorption capacity to As (III), and is widely accepted in As (III) repair because of the large amount of As (III) existing on the earth. But due to Fe3O4The particles are small, the specific surface area is large, and self-agglomeration easily occurs, so that the adsorption efficiency is reduced. The traditional solution is to mix Fe3O4Loaded on the surface of the carrier, limits self agglomeration and enhances the arsenic adsorption capacity of the carrier. However, the support does not generally have arsenic adsorption properties, which reduces the adsorption properties of the material. In addition, mesoporous ferroferric oxide is prepared by taking KIT-6 and other mesoporous silica as hard template agents, and after the mesoporous ferroferric oxide is prepared, the template is removed, so that the problem that the template carrier does not absorb arsenic pollutants is solvedThe disadvantage of the attachment. However, the complicated procedure and strict experimental requirements limit its wide application. Therefore, the mesoporous ferroferric oxide is prepared by a simpler operation requirement and a rapid preparation method, and the mesoporous ferroferric oxide can be effectively applied to the actual trivalent arsenic treatment process.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides mesoporous Fe3O4Preparation method of composite adsorbent and application thereof in treating As (III) -containing aqueous solution, and mesoporous Fe thereof3O4The composite adsorbent is simple to operate, environment-friendly, high in adsorption efficiency and low in process requirement, and is applied to separating As (III) in aqueous solution.
The invention is realized by the following technical scheme:
mesoporous Fe3O4Composite adsorbent of Fe3O4And SiO2The composition comprises the following raw materials in a raw material content ratio of Fe, Si and O of 37.85:3.84: 58.36.
Mesoporous Fe3O4The preparation method of the composite adsorbent comprises the steps of taking ferric trichloride hexahydrate and ferrous sulfate heptahydrate as raw materials, taking the mesoporous hollow sphere as a template agent, adding a certain amount of sodium hydroxide solution as a precipitator and a template remover, and adding a proper amount of sodium hydroxide to the surface of the mesoporous hollow sphere to precipitate Fe3O4Simultaneously removing the hollow sphere template to obtain mesoporous Fe3O4The composite adsorbent is prepared by the following specific steps:
(1) 33.3mg of ferric chloride hexahydrate and 16.7mg of ferrous sulfate heptahydrate were accurately weighed and dissolved in 50mL of deionized water, respectively, that is, the iron salt ratio was 2: 1, uniformly mixing the two solutions in a three-necked bottle in a nitrogen atmosphere to prevent ferrous salt from being oxidized to prepare a ferric salt solution;
(2) accurately weighing 50.0mg of mesoporous hollow sphere template agent, dispersing in the three-necked bottle in the step (1), continuously stirring in a nitrogen atmosphere until the mesoporous hollow sphere template agent is uniformly mixed, and fully dispersing ferric salt on the surface and in the pore diameter of the mesoporous hollow sphere to obtain a mixed solution;
(3) quickly adding 100mL of 2mol/L sodium hydroxide solution precipitator and template remover into the mixed solution prepared in the step (2), and stirring for 1 hour at room temperature in a nitrogen atmosphere to uniformly mix the sodium hydroxide solution and ferric salt and perform primary precipitation;
(4) heating the solution prepared in the step (3) to 70 ℃, and continuously stirring for 4 hours in a nitrogen atmosphere to ensure that iron salt is fully precipitated and simultaneously remove the mesoporous hollow sphere template agent;
(5) washing with a large amount of deionized water to neutrality, removing redundant sodium hydroxide, and vacuum drying at 60 deg.C to obtain mesoporous Fe3O4A composite adsorbent.
As a preferred embodiment of the invention, the weight ratio of the ferric trichloride hexahydrate to the ferrous sulfate heptahydrate is 2-1.5: 1.
as a preferred embodiment of the present invention, the weight ratio of the ferric trichloride hexahydrate to the ferrous sulfate heptahydrate is 2: 1.
as a preferred embodiment of the present invention, the weight ratio of the mesoporous hollow spheres to the iron salt solution is 3: 1 to 27.
As a preferred embodiment of the present invention, the weight ratio of the mesoporous hollow sphere to the iron salt solution is 1: 1.
as a preferred embodiment of the present invention, the concentration of the sodium hydroxide solution is 1 to 3mol/L, preferably 2 mol/L.
Mesoporous Fe3O4The application of the composite adsorbent in treating As (III) -containing aqueous solution.
As a preferred embodiment of the present invention, the As (III) aqueous solution is an aqueous sodium arsenite solution.
As a preferred embodiment of the present invention, 5mg of mesoporous Fe is added to 25mL of 100mg/L As (III) aqueous solution3O4The composite adsorbent is fully vibrated and adsorbed for 24 hours under the conditions of 230rpm, pH8 and 37 ℃.
Compared with the prior art, the invention has the following beneficial effects:
(1) the mesoporous Fe obtained by the invention3O4The composite adsorbent has high adsorption capacity of more than 189.5mg/g for As (III) in water.
(2) The mesoporous Fe of the invention3O4The composite adsorbent is prepared by a one-step method, is simple and quick to operate and can be produced in a large scale.
Detailed Description
The following examples illustrate the invention in detail: the present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following embodiments.
The adsorbent for removing arsenic from water is prepared by the following method, ferric trichloride hexahydrate and ferrous sulfate heptahydrate are used as raw materials, a mesoporous hollow sphere is used as a template agent, a certain amount of sodium hydroxide solution is added to be used as a precipitator and the template remover, and the product is washed to be neutral by a large amount of deionized water to obtain the adsorbent.
The mesoporous Fe of the invention3O4The preparation method of the composite adsorbent comprises the following specific steps,
(1) accurately weighing 16.7-299.7mg of ferric trichloride hexahydrate and 16.7-299.7mg of ferrous sulfate heptahydrate, respectively dissolving in 50mL of deionized water, and then uniformly mixing the two solutions in a three-necked bottle under the nitrogen atmosphere;
(2) accurately weighing 50.0-150mg of hollow spheres, dispersing the hollow spheres in the three-necked bottle, and continuously stirring the mixture in a nitrogen atmosphere until the mixture is uniformly mixed;
(3) quickly adding 100mL of 1-3mol/L sodium hydroxide solution into the mixed solution, and stirring for 1 hour at room temperature under the nitrogen atmosphere;
(4) heating the solution to 70 ℃, and continuously stirring for 4 hours under the nitrogen atmosphere;
(5) washing with a large amount of deionized water to neutrality, and vacuum drying at 60 deg.C to obtain mesoporous Fe3O4A composite adsorbent.
The method for removing arsenic in water comprises the steps of firstly preparing 100mg/L of arsenic concentration in water to be measured, adjusting the pH value to be 8, and adding 5.0mg of mesoporous Fe3O4And (5) compounding the adsorbent, and adsorbing for 24 hours.
Mesoporous Fe3O4Application of composite adsorbent in treating As (III) -containing aqueous solution. The As (III) aqueous solution is sodium arsenite aqueous solution. Adding 5mg of mesoporous Fe into 100mg/L of As (III) aqueous solution3O4The composite adsorbent is fully vibrated and adsorbed for 24 hours under the conditions of 230rpm, pH8 and 37 ℃.
Example 1:
(1) 33.3mg of ferric chloride hexahydrate and 16.7mg of ferrous sulfate heptahydrate were accurately weighed and dissolved in 50mL of deionized water, respectively, that is, the iron salt ratio was 2: 1, then uniformly mixing the two solutions in a three-necked bottle in a nitrogen atmosphere;
(2) accurately weighing 50.0mg of hollow spheres, dispersing the hollow spheres in the three-necked bottle, and continuously stirring the mixture in a nitrogen atmosphere until the mixture is uniformly mixed;
(3) quickly adding 100mL of 2mol/L sodium hydroxide solution into the mixed solution, and stirring for 1 hour at room temperature under the nitrogen atmosphere;
(4) heating the solution to 70 ℃, and continuously stirring for 4 hours under the nitrogen atmosphere;
(5) washing with a large amount of deionized water to neutrality, and vacuum drying at 60 deg.C to obtain mesoporous Fe3O4A composite adsorbent.
And (3) adsorption result:
weighing 5.0mg of mesoporous Fe3O4The composite adsorbent is placed in a conical flask containing 25mL of 100mg/L As (III) solution, the mixture is shaken for 24 hours under the conditions of 37 ℃, 230rpm and pH8, and then the mixture is filtered by a 0.22um needle filter and then the concentration of residual arsenic in the supernatant is detected by ICP-MS, so that the mesoporous Fe is calculated3O4Adsorption capacity of the composite adsorbent to As (III) in aqueous solution. As (III) has an adsorption capacity of 189.5 mg/g.
Example 2:
mesoporous Fe according to the example3O4The preparation method of the composite adsorbent is different from that of the example 1 in that: (1) 30.0mg of ferric chloride hexahydrate and 20.0mg of ferrous sulfate heptahydrate, namely the iron salt ratio is 1.5: 1. the rest steps are the same.
And (3) adsorption result: the adsorption conditions in this example were the same as those in example 1. As (III) has an adsorption capacity of 128.2 mg/g.
Example 3:
mesoporous Fe according to the example3O4The preparation method of the composite adsorbent is different from that of the example 1 in that: (2) 150.0mg of mesoporous hollow spheres are added, namely the mass ratio of the mesoporous hollow spheres to the total ferric salt is 3: 1. the rest steps are the same.
And (3) adsorption result: the adsorption conditions in this example were the same as those in example 1. As (III) has an adsorption capacity of 120.8 mg/g.
Example 4:
mesoporous Fe according to the example3O4The preparation method of the composite adsorbent is different from that of the example 1 in that: (1) 99.9mg of ferric trichloride hexahydrate and 50.1mg of ferrous sulfate heptahydrate are added, namely the mass ratio of the hollow spheres to the total ferric salt is 1: 3. the rest steps are the same.
And (3) adsorption result: the adsorption conditions in this example were the same as those in example 1. As (III) has an adsorption capacity of 165.3 mg/g.
Example 5:
mesoporous Fe according to the example3O4The preparation method of the composite adsorbent is different from that of the example 1 in that: (1) 199.8mg of ferric trichloride hexahydrate and 100.2mg of ferrous sulfate heptahydrate are added, namely the mass ratio of the mesoporous hollow spheres to the total ferric salt is 1: 6. the rest steps are the same.
And (3) adsorption result: the adsorption conditions in this example were the same as those in example 1. As (III) has an adsorption capacity of 157.1 mg/g.
Example 6:
mesoporous Fe according to the example3O4The preparation method of the composite adsorbent is different from that of the example 1 in that: (1) 299.7mg of ferric chloride hexahydrate and 150.3mg of ferrous sulfate heptahydrate are added, namely the mass ratio of the mesoporous hollow spheres to the total ferric salt is 1: 9. the rest steps are the same.
And (3) adsorption result: the adsorption conditions in this example were the same as those in example 1. As (III) has an adsorption capacity of 154.8 mg/g.
Example 7:
mesoporous Fe according to the example3O4The preparation method of the composite adsorbent is different from that of the example 1 in that: (3) middle addingAdding 1mol/L sodium hydroxide solution. The rest steps are the same.
And (3) adsorption result: the adsorption conditions in this example were the same as those in example 1. As (III) has an adsorption capacity of 111.2 mg/g.
Example 8:
mesoporous Fe according to the example3O4The preparation method of the composite adsorbent is different from that of the example 1 in that: (3) to which a 3mol/L sodium hydroxide solution was added. The rest steps are the same.
And (3) adsorption result: the adsorption conditions in this example were the same as those in example 1. As (III) has an adsorption capacity of 180.8 mg/g.
Table 1 is a table comparing the adsorption capacities of the above embodiments for As (III)
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. Mesoporous Fe3O4A composite adsorbent, characterized in that it is composed of Fe3O4And SiO2The composition comprises the following raw materials in a raw material content ratio of Fe, Si and O of 37.85:3.84: 58.36.
2. Mesoporous Fe3O4The preparation method of the composite adsorbent is characterized in that ferric trichloride hexahydrate and ferrous sulfate heptahydrate are used as raw materials, the mesoporous hollow sphere is used as a template agent, a certain amount of sodium hydroxide solution is added to be used as a precipitator and a template remover, and a product is subjected to a large amount of deionized waterAfter being washed to be neutral, the mesoporous Fe3O4Compounding to obtain the adsorbent, and specifically preparing the adsorbent by the following steps:
(1) 33.3mg of ferric chloride hexahydrate and 16.7mg of ferrous sulfate heptahydrate were accurately weighed and dissolved in 50mL of deionized water, respectively, that is, the iron salt ratio was 2: 1, uniformly mixing the two solutions in a three-necked bottle in a nitrogen atmosphere to prevent ferrous salt from being oxidized to prepare a ferric salt solution;
(2) accurately weighing 50.0mg of mesoporous hollow sphere template agent, dispersing in the three-necked bottle in the step (1), continuously stirring in a nitrogen atmosphere until the mesoporous hollow sphere template agent is uniformly mixed, and uniformly distributing iron salt on the surface and in the holes of the mesoporous hollow sphere to obtain a mixed solution;
(3) quickly adding 100mL of 2mol/L sodium hydroxide solution serving as a precipitator and a template remover into the mixed solution prepared in the step (2), and stirring for 1 hour at room temperature under the atmosphere of nitrogen to uniformly mix the sodium hydroxide solution and ferric salt and perform primary precipitation;
(4) heating the solution prepared in the step (3) to 70 ℃, and continuing stirring for 4 hours in a nitrogen atmosphere to fully precipitate iron salt and remove the template;
(5) washing with a large amount of deionized water to neutrality, washing off excessive sodium hydroxide, and vacuum drying at 60 deg.C to obtain mesoporous Fe3O4A composite adsorbent.
3. Mesoporous Fe according to claim 23O4The preparation method of the composite adsorbent is characterized in that the weight ratio of ferric trichloride hexahydrate to ferrous sulfate heptahydrate is (2-1.5): 1, screening out the optimal weight ratio of ferric trichloride hexahydrate to ferrous sulfate heptahydrate.
4. Mesoporous Fe according to claim 33O4The preparation method of the composite adsorbent is characterized in that the weight ratio of the ferric trichloride hexahydrate to the ferrous sulfate heptahydrate is 2: 1.
5. mesoporous Fe according to claim 23O4A preparation method of a composite adsorbent, which comprises the following steps,the mesoporous hollow sphere is characterized in that the weight ratio of the mesoporous hollow sphere to the ferric salt solution is 3: 1-27, so as to screen out the weight ratio of the optimal hollow sphere to the total iron salt.
6. Mesoporous Fe according to claim 23O4The preparation method of the composite adsorbent is characterized in that the weight ratio of the mesoporous hollow spheres to the ferric salt solution is 1: 1.
7. mesoporous Fe according to claim 23O4The preparation method of the composite adsorbent is characterized in that the concentration of the sodium hydroxide solution is 1-3mol/L, preferably 2mol/L, so as to screen out the optimal concentrations of a sodium hydroxide precipitator and a template remover.
8. Mesoporous Fe according to claim 23O4The application of the composite adsorbent in treating As (III) -containing aqueous solution.
9. Mesoporous Fe according to claim 83O4The application of the composite adsorbent in treating the aqueous solution with high As (III) concentration and 100mg/L content is characterized in that the aqueous solution of As (III) is a sodium arsenite aqueous solution.
10. Mesoporous Fe according to claim 83O4The application of the composite adsorbent in treating As (III) -containing aqueous solution is characterized in that 5mg of mesoporous Fe is added into 100mg/L of As (III) aqueous solution3O4The composite adsorbent is fully vibrated and adsorbed for 24 hours under the conditions of 230rpm, pH8 and 37 ℃.
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| CN103464065A (en) * | 2013-09-22 | 2013-12-25 | 北京化工大学 | Magnetic nanosphere with mesoporous shell and quick preparation method thereof |
| CN109794216A (en) * | 2019-02-27 | 2019-05-24 | 福建工程学院 | A kind of preparation of nano adsorption material and its application in repairing heavy metal in soil pollution |
| CN111495315A (en) * | 2020-04-23 | 2020-08-07 | 齐鲁工业大学 | Pb in water body2+Application and preparation method of adsorbing material |
| CN113023818A (en) * | 2021-03-12 | 2021-06-25 | 沂水鸿羽环境科技中心 | Water purification material |
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|---|---|---|---|---|
| CN103464065A (en) * | 2013-09-22 | 2013-12-25 | 北京化工大学 | Magnetic nanosphere with mesoporous shell and quick preparation method thereof |
| CN109794216A (en) * | 2019-02-27 | 2019-05-24 | 福建工程学院 | A kind of preparation of nano adsorption material and its application in repairing heavy metal in soil pollution |
| CN111495315A (en) * | 2020-04-23 | 2020-08-07 | 齐鲁工业大学 | Pb in water body2+Application and preparation method of adsorbing material |
| CN113023818A (en) * | 2021-03-12 | 2021-06-25 | 沂水鸿羽环境科技中心 | Water purification material |
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Application publication date: 20211109 |