CN113398896B - Preparation method of sodium polyacrylate dispersed ferrous sulfide intercalation layered double hydroxide - Google Patents
Preparation method of sodium polyacrylate dispersed ferrous sulfide intercalation layered double hydroxide Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title claims abstract description 83
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 title claims abstract description 46
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000009830 intercalation Methods 0.000 title abstract description 10
- 230000002687 intercalation Effects 0.000 title abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 145
- 239000011259 mixed solution Substances 0.000 claims abstract description 38
- 238000001179 sorption measurement Methods 0.000 claims abstract description 38
- 238000005406 washing Methods 0.000 claims abstract description 22
- 150000001768 cations Chemical class 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 239000011734 sodium Substances 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- 239000002244 precipitate Substances 0.000 claims abstract description 16
- 150000001450 anions Chemical class 0.000 claims abstract description 14
- 238000007872 degassing Methods 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 20
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000011777 magnesium Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 5
- 239000010865 sewage Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 230000005284 excitation Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 230000001737 promoting effect Effects 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 9
- 230000009467 reduction Effects 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 231100000783 metal toxicity Toxicity 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical group O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 12
- 229910017604 nitric acid Inorganic materials 0.000 description 12
- 230000002195 synergetic effect Effects 0.000 description 9
- 230000001360 synchronised effect Effects 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 238000011010 flushing procedure Methods 0.000 description 4
- 230000004075 alteration Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- -1 hydrogen sulfide free radical Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
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- 231100000053 low toxicity Toxicity 0.000 description 1
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- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
-
- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- 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
- B01J20/28014—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
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
-
- 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
-
- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
-
- 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
-
- 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
A preparation method of sodium polyacrylate dispersed ferrous sulfide intercalated layered double hydroxide comprises the following steps: s1, preparing a sodium polyacrylate aqueous solution to obtain a solution A; s2, preparing a layered double hydroxide aqueous solution to obtain a solution B; s3, adding the solution B into the solution A to obtain a mixed solution C; s4, preparing FeSO 4 .7H 2 O or FeCl 3 Degassing the aqueous solution to obtain a solution D; s5, preparing Na 2 S and/or NaBH 4 Degassing the aqueous solution to obtain a solution E; s6, dropwise adding the solution D into the solution C, and stirring to obtain a mixed solution F; s7, dropwise adding the solution E into the solution F to finally generate black precipitate, and washing and drying to obtain the productThe sodium polyacrylate disperses the nano ferrous sulfide intercalation layered double hydroxide. Ferrous sulfide dispersed in sodium polyacrylate solution is intercalated into the layered amphiphilic hydroxide to prevent ferrous sulfide agglomeration, so that the ferrous sulfide can synergistically and efficiently adsorb metal anions and cations, promote heavy metal adsorption and reduction, and reduce heavy metal toxicity.
Description
Technical Field
The invention relates to a sewage treatment technology, in particular to a preparation method of sodium polyacrylate dispersed ferrous sulfide intercalated layered double hydroxide.
Background
Accompanying with industrial production and human activities, a large amount of heavy metals flow into water bodies to cause water environment damage, for example, the heavy metals and the contents thereof in sewage of a certain Zn electroplating wastewater factory are As (III) (89.5 mg/L), as (V) (60.8 mg/L), cr (25.3 mg/L), cd (52.4 mg/L), cu (5.9 mg/L), zn (274.1 mg/L), mn (26.8 mg/L) and Fe (33.1 mg/L), etc. Therefore, the research and development of the composite material for realizing synchronous and efficient removal of the mixed heavy metals are concerned widely.
The layered double hydroxide is an inorganic material with high efficiency, low cost, low price, easy obtaining and simple synthesis process, has certain adsorption capacity on heavy metals and certain catalytic performance on organic matters, and can be used as a substrate material to realize the immobilization of nano materials. But the industrial application of the metal ion adsorbent is limited due to the problems of low adsorption efficiency, slow adsorption rate, difficulty in realizing synchronous adsorption of metal anions and cations and the like.
At present, the preparation of the sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide composite material and the research on the synergistic adsorption removal of Cr (VI), as (III), as (V), cd (II), ni (II) and Cu (II) ions by the sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide composite material are not found.
It is to be noted that the information disclosed in the above background section is only for understanding the background of the present application and thus may include information that does not constitute prior art known to a person of ordinary skill in the art.
Disclosure of Invention
The invention provides a preparation method of sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide aiming at the problems of poor synergistic adsorption effect of metal anions and cations, easy agglomeration of a nano composite material and the like, and the obtained material realizes the synergistic efficient adsorption of the metal anions and cations.
In order to realize the purpose, the invention adopts the following technical scheme:
a preparation method of sodium polyacrylate dispersed ferrous sulfide intercalated layered double hydroxide comprises the following steps:
s1, preparing a sodium polyacrylate aqueous solution to obtain a solution A;
s2, preparing a layered double hydroxide aqueous solution to obtain a solution B;
s3, adding the solution B into the solution A to obtain a mixed solution C;
s4, preparing FeSO 4 .7H 2 O or FeCl 3 Degassing the aqueous solution to obtain a solution D;
s5, preparing Na 2 S and/or NaBH 4 Degassing the aqueous solution to obtain a solution E;
s6, dropwise adding the solution D into the solution C, and stirring to obtain a mixed solution F;
and S7, dropwise adding the solution E into the solution F to finally generate black precipitate, and washing and drying to obtain the sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide.
Further:
the layered double hydroxide is nitric acid type layered double hydroxide.
The method specifically comprises the following steps:
s1, adding 0.06g of sodium polyacrylate into 240mL of distilled water, and stirring to obtain a solution A;
s2, adding 0.4g of nitric acid type layered double hydroxide into 10mL of distilled water, and performing ultrasonic treatment for 30min to obtain a solution B;
s3, adding the solution B into the solution A to obtain a mixed solution C, and sequentially stirring and ultrasonically treating for 30min under the protection of nitrogen;
s4, taking a proper amount of FeCl 3 Dissolving in 30-40mL of degassed water to obtain a solution D;
s5, taking a proper amount of Na 2 S or taking appropriate amount of Na 2 S and NaBH 4 Dissolving in 20-30mL of degassed water to obtain a solution E;
s6, dropwise adding the solution D into the solution C under the protection of nitrogen, and magnetically stirring for 2 hours to obtain a mixed solution F;
and S7, dropwise adding the solution E into the solution F under the protection of nitrogen to finally generate black precipitates, and washing and drying to obtain the sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide.
In step S7, the black precipitate is separated from deionized water 1: rinsing 1, centrifuging at 9000rpm for 3min by a centrifuge, repeating for three times, drying at-48 deg.C for 12h by a freeze dryer, and grinding in a nitrogen box for collection.
The step S2 specifically includes:
preparing a divalent and trivalent metal cation mixed solution to obtain a solution A1; naOH and Na are prepared 2 CO 3 Mixing the solution to obtain a solution B1; preparing a mixed solution C1 of the solution B1 and the solution A1; heating and aging the mixed solution C1 to obtain carbonic acid type layered double hydroxide; washing the layered double hydroxide with ethanol and degassed water, centrifuging, repeating for several times, and drying to constant weight; heating constant weight carbonic acid type layered double hydroxide for reaction, and after the temperature is reduced, transferring to vacuum cooling; ball milling and sieving to obtain the nitric acid type layered double hydroxide.
The divalent and trivalent metal cations are selected from: mg (magnesium) 2+ And Al 3+ ；Mg 2+ And Fe 3+ 。
The step S2 specifically includes: preparing A1 mol/L mixed solution of divalent and trivalent metal cations to obtain a solution A1; preparing 1.5mol/L NaOH and 1mol/L Na 2 CO 3 Mixing the solution to obtain a solution B1; dropwise adding the solution A1 and the solution B1 together into distilled water with the pH value of about 10, and stirring to obtain a solution C1; aging the obtained solution C1 in an oven at 70 ℃ for 24 hours to obtain carbonic acid type layered double hydroxide; mixing ethanol and degassed water 1:1, washing, centrifuging at 9000rpm for 3min by a centrifuge, repeating for several times, drying at 70 deg.C until the conductivity of the final washing solution is less than 1000 us/cm; reacting constant-weight carbonic acid type layered double hydroxide in a muffle furnace at 600 ℃ for 2hWhen the temperature is reduced to 200 ℃, transferring the mixture into a vacuum drying oven for cooling; ball milling is carried out for 15min at the rotating speed of 220rpm, the recovered powder is sieved by a 60-mesh sieve, and finally the nitric acid type layered double hydroxide is obtained.
Sodium polyacrylate dispersed ferrous sulfide intercalated layered double hydroxide is prepared by the preparation method.
The sodium polyacrylate dispersed ferrous sulfide intercalated layered double hydroxide prepared by the preparation method is applied to the sewage treatment to realize the promotion of the synergistic adsorption of metal anions and cations.
In the application, the adsorption of any one or a plurality of Cr (VI), as (V), as (III), cd (II) and Cu (II) is promoted.
The invention has the following beneficial effects:
according to the invention, ferrous sulfide dispersed in a sodium polyacrylate solution is intercalated in the layered amphiphilic hydroxide to prevent the ferrous sulfide from agglomerating, so that the synergistic and efficient adsorption of metal anions and cations can be realized, and meanwhile, the precipitation of arsenic can be promoted under the irradiation of ultraviolet light, the adsorption and reduction effects of heavy metals are promoted, and the toxicity of the heavy metals is reduced.
The ferrous sulfide has stronger reduction performance, and can reduce heavy metal anions with high valence and high toxicity into cations with low valence and low toxicity, so as to be adsorbed by layered double hydroxide. Simultaneously, ferrous sulfide can release hydrogen sulfide free radical to form sulfide (CdS, as) with metal ions 2 S 3 Etc.) to realize the synchronous removal of metal cations and anions. However, the phenomenon of nanoparticle agglomeration can be caused by simply intercalating ferrous sulfide into the layered double hydroxide, and the sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide composite material prepared by the invention improves the adsorption and catalysis performance of the composite material and realizes the synergistic promotion of the synchronous adsorption of metal cations and anions.
Drawings
FIG. 1 is the dynamic curve of adsorbing Cr (VI) by intercalated layered double hydroxide of sodium polyacrylate dispersed nano ferrous sulfide prepared in example 3 of the present invention.
FIG. 2 is an SEM image of sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide prepared in example 3 of the present invention.
FIG. 3 is a kinetic curve of the synergistic adsorption of Cr (VI) by Cd (II) intercalated layered double hydroxide dispersed in sodium polyacrylate prepared in example 3 of the present invention.
FIG. 4 is a kinetic curve of the synergistic adsorption of Cr (VI) by Cu (II) intercalated layered double hydroxide with sodium polyacrylate dispersed nano ferrous sulfide prepared in example 3 of the present invention.
FIG. 5 is a kinetic curve of ultraviolet-promoted As (III) with sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide prepared in example 3 of the present invention.
Fig. 6 is a schematic view of ultraviolet light-promoted adsorption precipitation of As (III) and As (V) by the sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide prepared in embodiment 3 of the present invention.
Detailed description of the preferred embodiments
The following describes embodiments of the present invention in detail. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
The embodiment of the invention provides a preparation method of sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide, which comprises the following preparation processes:
firstly, the following steps: layered double hydroxide
Selecting 1mol/L divalent and trivalent metal cation to form mixed solution A1 (Mg can be selected) 2+ And Al 3+ ，Mg 2+ And Fe 3+ Etc.) and 1.5mol/L NaOH and 1mol/L Na 2 CO 3 The resulting mixed solution B1 was added dropwise to distilled water having a pH of about 10, and the mixture was stirred sufficiently to obtain a solution C1 (containing a white precipitate therein). And aging the obtained solution C1 in an oven at 70 ℃ for 24 hours to obtain the carbonic acid type layered double hydroxide. Ethanol and degassed water 1:1 flushing (degassing water is deionized water and nitrogen gas are aerated for 30min, carbon dioxide in the water body is removed), centrifuging, finally, the conductivity of the washing liquid is less than 1000us/cm, and drying in an oven at 70 ℃ to constant weight. Transferring constant heavy carbonate intercalation layered double hydroxide into a ceramic crucible, and reacting in a muffle furnace at 600 DEG CAnd (4) taking 2 hours, and timely transferring the crucible into a vacuum drying oven until the crucible is completely cooled when the temperature of the muffle furnace is reduced to 200 ℃. Grinding, crushing and sieving by a 60-mesh sieve to finally obtain nitric acid type lamellar double hydroxide;
II, secondly: sodium polyacrylate dispersed nano ferrous sulfide intercalation layered double hydroxide
Adding 0.06g of sodium polyacrylate into 240mL of distilled water, and fully stirring to obtain a solution A; adding 0.4g of nitric acid type layered double hydroxide into 10mL of distilled water, and carrying out ultrasonic treatment for 30min to obtain a solution B; adding the solution B into the solution A to obtain a mixed solution C, and sequentially stirring and ultrasonically treating for 30min under the protection of nitrogen; taking appropriate amount of FeSO 4 .7H 2 O or FeCl 3 Dissolving in 40mL of degassed water to obtain a solution D; taking a proper amount of Na 2 S and NaBH 4 Dissolving in 20mL of degassed water to obtain a solution E; dropwise adding the solution D into the solution C under the protection of nitrogen, and magnetically stirring for 2 hours to obtain a light green mixed solution F; and (3) dropwise adding the solution E into the solution F under the protection of nitrogen to finally generate black precipitate, washing with ethanol and deionized water, centrifuging, freeze-drying, and grinding and collecting in a nitrogen box to obtain the sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide.
The obtained composite material sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide can be applied to promoting the synchronous adsorption of Cr (VI), as (V), as (III), cd (II) and Cu (II).
Example 1:
0.75mol/LMg 2+ and 0.25mol/LAl 3+ The component A is mixed solution of 1.5mol/L NaOH and 1mol/L Na 2 CO 3 The mixed solution B is dropwise added into distilled water with the pH value of about 10, and the mixture is fully stirred for 2 hours to obtain solution C (containing white precipitate). And aging the obtained solution C in an oven at 70 ℃ for 24 hours to obtain the carbonic acid type layered double hydroxide. Ethanol and degassed water 1: washing 1, centrifuging at 9000rpm for 3min, repeating for several times, and drying in 70 deg.C oven to constant weight, wherein the conductivity of the final washing solution is less than 1000 us/cm. Transferring constant weight carbonic acid type layered double hydroxide into a ceramic crucible, reacting in a muffle furnace at 600 ℃ for 2h, and timely transferring the crucible into a vacuum drying oven when the temperature of the muffle furnace is reduced to 200 DEG CUntil it is completely cooled. Ball-milling for 15min at the rotation speed of 220rpm by a ball mill, recovering powder, and sieving by a 60-mesh sieve to finally obtain nitric acid type layered double hydroxides;
0.06g of sodium polyacrylate is added into 240mL of distilled water and fully stirred to obtain a solution A; adding 0.4g of nitric acid type layered double hydroxide into 10mL of distilled water, and carrying out ultrasonic treatment for 30min to obtain a solution B; adding the solution B into the solution A to obtain a mixed solution C, and sequentially stirring and ultrasonically treating for 30min under the protection of nitrogen; taking 1.4618gFeCl 3 Dissolving in 30mL of degassed water to obtain a solution D; taking 1.6224gNa 2 S and 1.8915gNaBH 4 Dissolving in 30mL of degassed water to obtain a solution E; dropwise adding the solution D into the solution C under the protection of nitrogen, and magnetically stirring for 2 hours to obtain a light green mixed solution F; and (3) dropwise adding the solution E into the solution F under the protection of nitrogen, finally generating a black precipitate, and mixing ethanol and deionized water 1:1 flushing, centrifuging at 9000rpm of a centrifugal machine for 3min, repeating for three times, drying for 12h by a freeze dryer at-48 ℃, grinding and collecting in a nitrogen box to obtain the sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide, and storing in a refrigerator at-5 ℃.
Example 2:
0.75mol/LMg 2+ and 0.25mol/LAl 3+ The component A is mixed solution of 1.5mol/L NaOH and 1mol/L Na 2 CO 3 The mixed solution B is dropwise added into distilled water with the pH value of about 10, and the mixture is fully stirred for 2 hours to obtain solution C (containing white precipitate). And aging the obtained solution C in an oven at 70 ℃ for 24 hours to obtain the carbonic acid type layered double hydroxide. Mixing ethanol and degassed water 1: washing with a washing machine 1, centrifuging at 9000rpm for 3min by a centrifuge, repeating for several times, wherein the conductivity of the last washing solution is less than 1000us/cm, and drying in an oven at 70 ℃ to constant weight. And transferring the constant-weight carbonic acid type layered double hydroxide into a ceramic crucible, reacting for 2 hours in a muffle furnace at the temperature of 600 ℃, and timely transferring the crucible into a vacuum drying oven until the crucible is completely cooled when the temperature of the muffle furnace is reduced to 200 ℃. Ball-milling for 15min at a rotating speed of 220rpm by a ball mill, recovering powder, and sieving by a 60-mesh sieve to finally obtain the nitric acid type layered double hydroxide;
0.06g of sodium polyacrylate is added into 240mL of distilled water and fully stirred to obtain a solution A; 0.4g nitric acid type lamellar crystals were added to 10mL of distilled waterCarrying out ultrasonic treatment on the double hydroxide for 30min to obtain a solution B; adding the solution B into the solution A to obtain a mixed solution C, and sequentially stirring and ultrasonically treating for 30min under the protection of nitrogen; 1.91264gFeSO 4 .7H 2 Dissolving O in 40mL of degassed water to obtain a solution D; 1.8432gNa was taken 2 S and 0.8g NaBH 4 Dissolving in 20mL of degassed water to obtain a solution E; dropwise adding the solution D into the solution C under the protection of nitrogen, and magnetically stirring for 2 hours to obtain a light green mixed solution F; and (3) dropwise adding the solution E into the solution F under the protection of nitrogen to finally generate a black precipitate, and mixing ethanol and deionized water 1:1 flushing, centrifuging at 9000rpm of a centrifugal machine for 3min, repeating for three times, drying at-48 deg.C for 12h with a freeze dryer, grinding in a nitrogen box, collecting to obtain sodium polyacrylate dispersed nanometer ferrous sulfide intercalation layered double hydroxide, and storing in a refrigerator at-5 deg.C.
Example 3:
0.75mol/LMg 2+ and 0.25mol/LAl 3+ The component A is mixed solution of 1.5mol/L NaOH and 1mol/L Na 2 CO 3 The mixed solution B is dropwise added into distilled water with the pH value of about 10, and the mixture is fully stirred for 2 hours to obtain solution C (containing white precipitate). And aging the obtained solution C in an oven at 70 ℃ for 24 hours to obtain the carbonic acid type layered double hydroxide. Ethanol and degassed water 1: washing 1, centrifuging at 9000rpm for 3min, repeating for several times, and drying in 70 deg.C oven to constant weight, wherein the conductivity of the final washing solution is less than 1000 us/cm. And transferring the constant-weight carbonic acid type layered double hydroxide into a ceramic crucible, reacting for 2 hours in a muffle furnace at the temperature of 600 ℃, and timely transferring the crucible into a vacuum drying oven until the crucible is completely cooled when the temperature of the muffle furnace is reduced to 200 ℃. Ball-milling for 15min at a rotating speed of 220rpm by a ball mill, recovering powder, and sieving by a 60-mesh sieve to finally obtain the nitric acid type layered double hydroxide;
0.06g of sodium polyacrylate is added into 240mL of distilled water and fully stirred to obtain a solution A; adding 0.4g of nitric acid type layered double hydroxide into 10mL of distilled water, and carrying out ultrasonic treatment for 30min to obtain a solution B; adding the solution B into the solution A to obtain a mixed solution C, and sequentially stirring and ultrasonically treating for 30min under the protection of nitrogen; 1.91264gFeSO 4 .7H 2 Dissolving O in 40mL of degassed water to obtain a solution D; 1.8432gNa was taken 2 S dissolved in 20mL of degassed waterTo obtain a solution E; dropwise adding the solution D into the solution C under the protection of nitrogen, and magnetically stirring for 2 hours to obtain a light green mixed solution F; and (3) dropwise adding the solution E into the solution F under the protection of nitrogen, finally generating a black precipitate, and mixing ethanol and deionized water 1:1 flushing, centrifuging at 9000rpm of a centrifugal machine for 3min, repeating for three times, drying at-48 ℃ for 12h by a freeze dryer, grinding and collecting in a nitrogen box to obtain the third sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide, and storing in a refrigerator at-5 ℃.
And (4) performance testing:
the composite material prepared in example 3 was subjected to Cr (VI) adsorption performance measurement, and the adsorption performance was measured by adding 15mg of the prepared composite material to 30mL of 10mg/L Cr (VI) solution. From fig. 1, it can be found that the reduction and adsorption performance of the ferrous sulfide to Cr (VI) can be improved by the intercalation of the ferrous sulfide into the layered double hydroxide, and the reduction and adsorption performance of the composite material to Cr (VI) can be further improved by the dispersion of the ferrous sulfide by PAA.
SEM powder characterization is carried out on the composite material prepared in the example 3, as shown in figure 2, the layered double hydroxide is of a sheet structure, the ferrous sulfide is also of a flower sheet structure, and the ferrous sulfide is successfully intercalated into the layered double hydroxide through intercalation to form fine flower sheets, so that the specific surface area is favorably improved, and the adsorption performance of the composite material is enhanced.
FIG. 3 is a kinetic curve of the prepared composite material on Cr (VI) adsorption in the presence of Cd (II), wherein the reaction conditions are as follows: 15mg of adsorbent, 30mL, a mixed solution of 20mg/L Cr (VI) and 50mg/L Cd (II). As can be seen from FIG. 3, compared with a single Cr (VI) solution, the addition of Cd (II) can promote the adsorption removal of Cr (VI), which indicates that the composite material has the metal anions and cations to synergistically promote the adsorption performance and can realize the synchronous adsorption of anions and cations in sewage.
FIG. 4 is a graph showing the kinetics of adsorption of Cr (VI) by the prepared composite material in the presence of Cu (II), wherein the reaction conditions are as follows: 15mg of adsorbent, 30mL, a mixed solution of 20mg/L of Cr (VI) and 50mg/L of Cu (II). From fig. 3, it can be seen that the addition of Cu (II) can promote the adsorption removal of Cr (VI) compared to a single Cr (VI) solution, indicating that the composite material has metal cations and anions to synergistically promote the adsorption performance. Compared with ferrous sulfide, the synergistic adsorption performance of the composite material is obviously improved by the intercalation layered amphiphilic hydroxide.
FIG. 5 is the As (III) adsorption kinetics curve of the prepared composite material under the irradiation of ultraviolet light, and the reaction conditions are As follows: 60mg of adsorbent, 150mL,20mg/LAs (III) solution. As can be seen from FIG. 5, the adsorption performance of the composite material to As (III) is obviously increased under the condition of ultraviolet light excitation, and it is possible that the ultraviolet light excitation promotes the composite material to release hydrogen sulfide free radicals to form As with As (III) 2 S 3 Precipitating to promote the adsorption removal of As (III).
FIG. 6 is a schematic diagram of the prepared composite material after adsorbing As (III) and As (V) under ultraviolet and dark conditions, the reaction conditions are As follows: 60mg of adsorbent, 150mL,20mg/LAs (III) or As (V) solution. It can be seen from FIG. 6 that the yellow As is significantly promoted by the ultraviolet light irradiation 2 S 3 The precipitation is generated, and the ultraviolet irradiation excitation can enhance the precipitation performance of the composite material.
The background of the present invention may contain background information related to the problem or environment of the present invention and does not necessarily describe the prior art. Accordingly, the inclusion in the background section is not an admission of prior art by the applicant.
The foregoing is a further detailed description of the invention in connection with specific/preferred embodiments thereof and it is not intended to limit the invention to the specific embodiments disclosed herein. It will be apparent to those skilled in the art that numerous alterations and modifications can be made to the described embodiments without departing from the inventive concepts herein, and such alterations and modifications are to be considered as within the scope of the invention. In the description herein, references to the description of the term "one embodiment," "some embodiments," "preferred embodiments," "an example," "a specific example," or "some examples" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Various embodiments or examples and features of various embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction. Although embodiments of the present invention and their advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the scope of the claims.
Claims (8)
1. The application of the sodium polyacrylate dispersed ferrous sulfide intercalated layered double hydroxide in adsorbing As (III) and As (V) and promoting the precipitation of As (III) and As (V) under the condition of ultraviolet light excitation is characterized in that the preparation method of the sodium polyacrylate dispersed ferrous sulfide intercalated layered double hydroxide comprises the following steps:
s1, preparing a sodium polyacrylate aqueous solution to obtain a solution A;
s2, preparing a layered double hydroxide aqueous solution to obtain a solution B;
s3, adding the solution B into the solution A to obtain a mixed solution C;
s4, preparing FeSO 4 .7H 2 O or FeCl 3 Degassing the aqueous solution to obtain a solution D;
s5, preparing Na 2 S-degassed aqueous solution or Na 2 S and NaBH 4 Degassing the aqueous solution to obtain a solution E;
s6, dropwise adding the solution D into the solution C, and stirring to obtain a mixed solution F;
and S7, dropwise adding the solution E into the solution F to finally generate black precipitate, and washing and drying to obtain the sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide.
2. Use according to claim 1, wherein the layered double hydroxide is a carbonic acid-type layered double hydroxide.
3. The use according to claim 1, comprising in particular the steps of:
s1, adding 0.06g sodium polyacrylate into 240mL distilled water, and stirring to obtain a solution A;
s2, adding 0.4g of carbonic acid type layered double hydroxide into 10mL distilled water, and carrying out ultrasonic treatment for 30min to obtain a solution B;
s3, adding the solution B into the solution A to obtain a mixed solution C, and sequentially stirring and ultrasonically treating for 30min under the protection of nitrogen;
s4, taking a proper amount of FeCl 3 Dissolving in 30-40mL degassed water to obtain solution D;
s5, taking a proper amount of Na 2 S or taking proper amount of Na 2 S and NaBH 4 Dissolving in 20-30mL degassed water to obtain solution E;
s6, dropwise adding the solution D into the solution C under the protection of nitrogen, and magnetically stirring the solution D for 2h to obtain a mixed solution F;
and S7, dropwise adding the solution E into the solution F under the protection of nitrogen to finally generate black precipitates, and washing and drying to obtain the sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide.
4. The use of claim 3, wherein in step S7, the black precipitate is formed by mixing ethanol with deionized water at a ratio of 1: washing 1, centrifuging at 9000rpm for 3min, repeating for three times, drying at-48 deg.C for 12 hr with a freeze dryer, and grinding in nitrogen box.
5. The use according to any one of claims 1 to 4, wherein step S2 specifically comprises:
preparing a divalent and trivalent metal cation mixed solution to obtain a solution A1; naOH and Na are prepared 2 CO 3 Mixing the solution to obtain a solution B1; preparing a mixed solution C1 of the solution B1 and the solution A1; heating and aging the mixed solution C1 to obtain carbonic acid type layered double hydroxide; washing the layered double hydroxide with ethanol and degassed water, centrifuging, repeating for several times, and drying to constant weight; heating constant weight carbonic acid type layered double hydroxide for reaction, cooling in vacuum after temperature is reducedBut; ball milling and sieving to obtain the carbonic acid type layered double hydroxide.
6. The use according to claim 5, wherein the divalent and trivalent metal cations are selected from the group consisting of: mg (magnesium) 2+ And Al 3+ ；Mg 2+ And Fe 3+ 。
7. The application according to claim 5, wherein step S2 specifically comprises: preparing A1 mol/L mixed solution of divalent and trivalent metal cations to obtain a solution A1; preparing 1.5mol/L NaOH and 1mol/L Na 2 CO 3 Mixing the solution to obtain a solution B1; dropwise adding the solution A1 and the solution B1 together into distilled water with the pH value of 10, and stirring to obtain a solution C1; aging the obtained solution C1 in an oven at 70 ℃ for 24 hours to obtain carbonic acid type layered double hydroxide; mixing ethanol and degassed water 1: washing 1, centrifuging at 9000rpm for 3min by a centrifuge, repeating for several times, and drying at 70 deg.C to constant weight, wherein the conductivity of the final washing solution is less than 1000 us/cm; reacting constant weight carbonic acid type layered double hydroxide in a muffle furnace at 600 ℃ for 2h, and transferring the reaction product into a vacuum drying oven for cooling when the temperature is reduced to 200 ℃; ball milling at 220rpm for 15min, recovering powder, and sieving with 60 mesh sieve to obtain carbonic acid type layered double hydroxide.
8. The application of the sodium polyacrylate dispersed ferrous sulfide intercalated layered double hydroxide in the promotion of the cooperative adsorption of metal anions and cations in sewage treatment is characterized in that the promotion of the cooperative adsorption of the metal anions and cations is that Cd (II) promotes the adsorption removal of Cr (VI) or Cu (II) promotes the adsorption removal of Cr (VI), and the preparation method of the sodium polyacrylate dispersed ferrous sulfide intercalated layered double hydroxide comprises the following steps:
s1, preparing a sodium polyacrylate aqueous solution to obtain a solution A;
s2, preparing a layered double hydroxide aqueous solution to obtain a solution B;
s3, adding the solution B into the solution A to obtain a mixed solution C;
s4, preparing FeSO 4 .7H 2 O or FeCl 3 Degassing the aqueous solution to obtain a solution D;
s5, preparing Na 2 S-degassed aqueous solution or Na 2 S and NaBH 4 Degassing the aqueous solution to obtain a solution E;
s6, dropwise adding the solution D into the solution C, and stirring to obtain a mixed solution F;
and S7, dropwise adding the solution E into the solution F to finally generate a black precipitate, and washing and drying to obtain the sodium polyacrylate dispersed nano ferrous sulfide intercalated layered double hydroxide.
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