CN112892473B - Preparation method of heavy metal removing material - Google Patents
Preparation method of heavy metal removing material Download PDFInfo
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- CN112892473B CN112892473B CN202110052220.9A CN202110052220A CN112892473B CN 112892473 B CN112892473 B CN 112892473B CN 202110052220 A CN202110052220 A CN 202110052220A CN 112892473 B CN112892473 B CN 112892473B
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- attapulgite
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- graphene oxide
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- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229960000892 attapulgite Drugs 0.000 claims abstract description 77
- 229910052625 palygorskite Inorganic materials 0.000 claims abstract description 77
- 238000003756 stirring Methods 0.000 claims abstract description 68
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 41
- 239000000047 product Substances 0.000 claims abstract description 39
- 238000001035 drying Methods 0.000 claims abstract description 36
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 30
- UIIMBOGNXHQVGW-UHFFFAOYSA-M NaHCO3 Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 29
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 15
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 15
- WIHMGGWNMISDNJ-UHFFFAOYSA-N 1,1-dichloropropane Chemical compound CCC(Cl)Cl WIHMGGWNMISDNJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 238000007873 sieving Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 150000007524 organic acids Chemical class 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- JFXDYPLHFRYDJD-UHFFFAOYSA-M sodium;6,7-dihydroxynaphthalene-2-sulfonate Chemical compound [Na+].C1=C(S([O-])(=O)=O)C=C2C=C(O)C(O)=CC2=C1 JFXDYPLHFRYDJD-UHFFFAOYSA-M 0.000 claims description 37
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 34
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- AEMRFAOFKBGASW-UHFFFAOYSA-N glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 8
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 12
- JFXDYPLHFRYDJD-UHFFFAOYSA-N sodium;6,7-dihydroxynaphthalene-2-sulfonic acid Chemical compound [Na+].C1=C(S(O)(=O)=O)C=C2C=C(O)C(O)=CC2=C1 JFXDYPLHFRYDJD-UHFFFAOYSA-N 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 239000008367 deionised water Substances 0.000 description 10
- 238000007792 addition Methods 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- AJVRSHNXSHMMCH-UHFFFAOYSA-K 2-hydroxypropane-1,2,3-tricarboxylate;iron(3+);hydrate Chemical compound O.[Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O AJVRSHNXSHMMCH-UHFFFAOYSA-K 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000006004 Quartz sand Substances 0.000 description 2
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 2
- 239000004113 Sepiolite Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- TUKQLEWOUPCTOS-UHFFFAOYSA-N dimagnesium;dioxido(oxo)silane;hydroxy-oxido-oxosilane;hydrate Chemical compound O.[Mg+2].[Mg+2].O[Si]([O-])=O.O[Si]([O-])=O.[O-][Si]([O-])=O TUKQLEWOUPCTOS-UHFFFAOYSA-N 0.000 description 2
- KARVSHNNUWMXFO-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane;hydrate Chemical compound O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O KARVSHNNUWMXFO-UHFFFAOYSA-N 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 230000002708 enhancing Effects 0.000 description 2
- 229960002413 ferric citrate Drugs 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000001965 increased Effects 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052901 montmorillonite Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- 230000001737 promoting Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052624 sepiolite Inorganic materials 0.000 description 2
- 235000019355 sepiolite Nutrition 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- -1 Chromium (III) Arsenic Chemical compound 0.000 description 1
- 235000019749 Dry matter Nutrition 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Ni2+ Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000001070 adhesive Effects 0.000 description 1
- 230000000274 adsorptive Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052803 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N silicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000004083 survival Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N tin hydride Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium(0) Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc 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
- B01J20/12—Naturally occurring clays or bleaching earth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01J20/2803—Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products
-
- 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
- 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 heavy metal removing material, which comprises the following steps: crushing raw attapulgite ore, sieving with a 80-mesh sieve to obtain attapulgite powder, placing the attapulgite powder in 40-60 wt% of organic acid solution, stirring and reacting at 60-80 ℃ for 20-40 min, slowly adding sodium bicarbonate during stirring, centrifugally filtering a product after reaction is finished, and drying a precipitate at 60-80 ℃ to obtain modified attapulgite; dissolving multilayer graphene oxide in acetone, then dropwise adding dichloropropane, performing microwave action for 30-60 min, and then drying at 60-100 ℃ for 60-80 min to obtain the multilayer graphene oxide subjected to layer expansion; and mixing and uniformly stirring the two products, then adding the two products into a 2, 3-dihydroxynaphthalene-6-sodium sulfonate solution, mixing and uniformly stirring, slowly dropwise adding DMF (dimethyl formamide) in the stirring process, carrying out ultrasonic treatment for 30min after dropwise adding is finished, then carrying out high-temperature treatment, and finally washing and drying to obtain the heavy metal removal material. The material obtained by the method has obvious effect of removing heavy metals.
Description
Technical Field
The invention belongs to the technical field of heavy metal removal, and particularly relates to a preparation method of a heavy metal removal material.
Background
At present, the industries of metal manufacturing, electronics, electroplating, chemistry, steel and nonferrous metal smelting and the like discharge a large amount of waste water containing heavy metal ions such as cadmium, chromium, lead, nickel, copper, zinc, cobalt, tin, vanadium, molybdenum, iron, manganese and the like in the production process, so that the water body is seriously polluted, and the survival of animals and plants is seriously influenced. Therefore, the removal of heavy metal contaminants is currently a very necessary step.
At present, the treatment method of heavy metal pollution of water mainly comprises the following steps: chemical precipitation, electrochemical methods, ion exchange, ultrafiltration, adsorption, membrane treatment techniques, and the like. For example, chinese patent application No. CN201710868060.9 discloses a method for preparing a heavy metal ion remover, which uses waste hardened cement concrete as a raw material, and obtains the heavy metal ion remover through primary crushing and pre-sintering, crushing and separating, ball milling activation, and powder selecting separation. For another example, application No. CN201910781658.3 discloses an adsorbent for removing heavy metals and its application, wherein the raw materials of the adsorbent include: dithio-carboxylated polyacrylamide, yeast surfactant and ferric citrate; the mass ratio of the dithio-carboxylated polyacrylamide, the yeast surfactant and the ferric citrate in the adsorbent is 100: 1.5-2.0: 5-10 in terms of dry matter. All the heavy metal removers remove heavy metal ions through adsorption, but the actual adsorption effect needs to be improved.
The attapulgite is a layer chain inorganic non-metallic mineral which takes water-containing magnesium-rich silicate as a main part, and has a plurality of special physicochemical and technological properties due to the unique crystal structure, and the main physicochemical properties and the technological properties are as follows: cation exchangeability, water absorption, adsorption decoloration, large specific surface area, colloid value and expansion capacity. In the natural attapulgite, the content of attapulgite is 70-80%, the content of montmorillonite and sepiolite is 10-15%, the content of quartz sand is 4-8%, and the content of calcite and dolomite is 1-5%. The presence of such impurities as montmorillonite, sepiolite and quartz sand inevitably impairs the original adsorptive, colloidal and adhesive properties of the attapulgite. The attapulgite has good adsorbability due to the large specific surface and the electrical property of the surface, but the rod crystals in the attapulgite crude ore usually exist in the form of rod crystal bundles and aggregates, which inevitably affect the specific surface area, further affect the adsorption performance and limit the application range of the attapulgite.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a heavy metal removal material aiming at the problem of poor effect of the existing heavy metal removal material. The heavy metal removing material obtained by the method can effectively remove the content of heavy metals in sewage.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme.
The invention provides a preparation method of a heavy metal removal material, which comprises the following steps:
crushing raw attapulgite ore, sieving with a 80-mesh sieve to obtain attapulgite powder, placing the attapulgite powder in 40-60 wt% of organic acid solution, stirring and reacting at 60-80 ℃ for 20-40 min, slowly adding sodium bicarbonate during stirring, centrifugally filtering a product after reaction is finished, and drying a precipitate at 60-80 ℃ to obtain modified attapulgite;
dissolving multilayer graphene oxide in acetone, then dropwise adding dichloropropane, performing microwave for 30-60 min under the action of a microwave field, and then drying at 60-100 ℃ for 60-80 min to obtain the multilayer graphene oxide subjected to layer expansion;
and mixing and uniformly stirring the obtained multilayer graphene oxide subjected to layer expansion with the obtained modified attapulgite, adding the mixture into a 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution, mixing and stirring, slowly dropwise adding DMF (dimethyl formamide) in the stirring process, carrying out ultrasonic treatment on the mixture for 30min after dropwise adding, carrying out high-temperature treatment, washing and drying the treated product, and thus obtaining the heavy metal removal material.
In the preparation method, the organic acid includes oxalic acid, acetic acid, glycolic acid, and citric acid.
In the preparation method, the ratio of the organic acid to the attapulgite powder is (5-10) mL: 1g of the total weight of the composition.
In the preparation method, the mass ratio of the sodium bicarbonate to the attapulgite powder is (0.04-0.06): 1.
the preparation method described above, wherein the centrifugation conditions are: the rotating speed is 600-800 r/min, and the time is 10-30 min.
The preparation method comprises the following steps of: dissolving 2, 3-dihydroxy naphthalene-6-sodium sulfonate in sodium hydroxide solution to obtain 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution.
The preparation method, wherein the ratio of the sodium 2, 3-dihydroxynaphthalene-6-sulfonate to the sodium hydroxide solution is 1 g: (100-300) mL.
In the preparation method, the high-temperature treatment conditions are as follows: the temperature is 600-800 ℃, and the time is 2-4 h. .
By the technical scheme, the invention at least has the following advantages: the invention takes the attapulgite as a main active substance, and improves the adsorption of heavy metal ions in the sewage by enhancing the adsorption effect of the attapulgite, thereby achieving the effect of removing. Firstly, the invention can remove the impurity substances contained in the attapulgite crude ore by the acidification of the organic acid, and the excessive H can be neutralized by adding the sodium bicarbonate + Compared with conventional acids, the organic acid used has higher safety than hydrochloric acid, nitric acid or sulfuric acid, and the organic acid has weaker acidity, so that the original adsorption performance of the attapulgite can be maintained. Secondly, placing the multilayer graphene oxide in acetone solution of dichloropropane, promoting the layer expansion reaction of the multilayer graphene oxide through the action of a microwave field, increasing the surface area of the graphene oxide, and then under the action of 2, 3-dihydroxy naphthalene-6-sodium sulfonate, enabling the modified attapulgite particles to be attached to the surface of the multilayer graphene oxide, and promoting the attachment of more attapulgite particles through microwave layer expansion to improve the adsorption performance of the material; in the process, the 2, 3-dihydroxy naphthalene-6-sodium sulfonate plays a role in adhesion, and the surface structure of the multilayer graphene oxide is changed, so that the van der Waals force of the combination between the attapulgite particles and the surface of the graphene oxide is increased, and the stability of the whole material is enhanced. Finally, passing through a high temperatureTherefore, the original structure can be kept, and the stability is further improved. The preparation method is simple and suitable for industrial production.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing a 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution: dissolving 1g of 2, 3-dihydroxy naphthalene-6-sodium sulfonate in 200mL of sodium hydroxide solution, and uniformly stirring.
The preparation method comprises the steps of crushing raw attapulgite ore, sieving with a 80-mesh sieve to obtain attapulgite powder, placing 100g of the attapulgite powder in 800mL of 50 wt% acetic acid solution, and stirring and reacting at 70 ℃ for 30min, wherein sodium bicarbonate is slowly added in the stirring process, and the total addition amount is 5 g. And after the reaction is finished, centrifuging the product at 700r/min for 20min, filtering, and drying the precipitated product at 70 ℃ to obtain the modified attapulgite. Dissolving 100g of multilayer graphene oxide in 100mL of acetone, then dropwise adding 2mL of dichloropropane, carrying out microwave treatment for 50min under the action of a microwave field, and then drying at 80 ℃ for 70min to obtain the expanded multilayer graphene oxide. And mixing and uniformly stirring the obtained multilayer graphene oxide subjected to layer expansion with the obtained modified attapulgite, then adding the mixture into 150mL of 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution for mixing and stirring, wherein 1mL of DMF is slowly dripped in the stirring process, after the dripping is finished, ultrasonically treating the mixture for 30min, treating the mixture at a high temperature of 700 ℃ for 3h, washing the treated product with deionized water, and then placing the washed product in an oven at a temperature of 60 ℃ for drying overnight to obtain the heavy metal removal material.
Example 2
Preparing a 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution: dissolving 1g of 2, 3-dihydroxy naphthalene-6-sodium sulfonate in 200mL of sodium hydroxide solution, and uniformly stirring.
The preparation method comprises the steps of crushing raw attapulgite, sieving with a 80-mesh sieve to obtain attapulgite powder, placing 100g of the attapulgite powder in 500mL of 50 wt% glycolic acid solution, and stirring and reacting at 70 ℃ for 30min, wherein sodium bicarbonate is slowly added in the stirring process, and the total addition amount is 6 g. And after the reaction is finished, centrifuging the product at 800r/min for 20min, filtering, and drying the precipitated product at 70 ℃ to obtain the modified attapulgite. Dissolving 100g of multilayer graphene oxide in 150mL of acetone, then dropwise adding 1mL of dichloropropane, carrying out microwave treatment for 50min under the action of a microwave field, and then drying at 80 ℃ for 70min to obtain the expanded multilayer graphene oxide. And mixing and uniformly stirring the obtained multilayer graphene oxide subjected to layer expansion with the obtained modified attapulgite, then adding the mixture into 100mL of 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution for mixing and stirring, wherein 1mL of DMF is slowly dripped in the stirring process, after the dripping is finished, ultrasonically treating the mixture for 30min, treating the mixture at a high temperature of 700 ℃ for 3h, washing the treated product with deionized water, and then placing the washed product in an oven at a temperature of 60 ℃ for drying overnight to obtain the heavy metal removal material.
Example 3
Preparing a 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution: 2g of 2, 3-dihydroxy naphthalene-6-sodium sulfonate is dissolved in 200mL of sodium hydroxide solution and stirred uniformly.
The preparation method comprises the steps of crushing raw attapulgite ore, sieving with a 80-mesh sieve to obtain attapulgite powder, placing 100g of the attapulgite powder in 800mL of 60 wt% citric acid solution, and stirring and reacting at 60 ℃ for 40min, wherein sodium bicarbonate is slowly added in the stirring process, and the total addition amount is 6 g. And after the reaction is finished, centrifuging the product at 800r/min for 10min, filtering, and drying the precipitated product at 70 ℃ to obtain the modified attapulgite. Dissolving 100g of multilayer graphene oxide in 100mL of acetone, then dropwise adding 1mL of dichloropropane, carrying out microwave for 30min under the action of a microwave field, and then drying for 60min at 100 ℃ to obtain the expanded multilayer graphene oxide. And mixing and uniformly stirring the obtained multilayer graphene oxide subjected to layer expansion with the obtained modified attapulgite, then adding the mixture into 150mL of 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution for mixing and stirring, wherein 1mL of DMF is slowly dripped in the stirring process, after the dripping is finished, ultrasonically treating the mixture for 30min, treating the mixture at the high temperature of 800 ℃ for 3h, washing the treated product with deionized water, and then placing the washed product in a 60 ℃ oven for drying overnight to obtain the heavy metal removal material.
Example 4
Preparing a 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution: dissolving 1g of 2, 3-dihydroxy naphthalene-6-sodium sulfonate in 300mL of sodium hydroxide solution, and uniformly stirring.
The preparation method comprises the steps of crushing raw attapulgite ore, sieving with a 80-mesh sieve to obtain attapulgite powder, placing 100g of the attapulgite powder in 500mL of 40 wt% oxalic acid solution, and stirring and reacting at 60 ℃ for 20min, wherein sodium bicarbonate is slowly added in the stirring process, and the total addition amount is 5 g. And after the reaction is finished, centrifuging the product at 600r/min for 30min, filtering, and drying the precipitate at 60 ℃ to obtain the modified attapulgite. Dissolving 100g of multilayer graphene oxide in 100mL of acetone, then dropwise adding 3mL of dichloropropane, carrying out microwave under the action of a microwave field for 40min, and then drying at 60 ℃ for 80min to obtain the expanded multilayer graphene oxide. And mixing and uniformly stirring the obtained multilayer graphene oxide subjected to layer expansion with the obtained modified attapulgite, then adding the mixture into 200mL of 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution for mixing and stirring, wherein 1mL of DMF is slowly dripped in the stirring process, after the dripping is finished, ultrasonically treating the mixture for 30min, treating the mixture at the high temperature of 600 ℃ for 4h, washing the treated product with deionized water, and then placing the washed product in an oven at the temperature of 60 ℃ for drying overnight to obtain the heavy metal removal material.
Example 5
Preparing a 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution: dissolving 1g of 2, 3-dihydroxy naphthalene-6-sodium sulfonate in 200mL of sodium hydroxide solution, and uniformly stirring.
The preparation method comprises the steps of crushing raw attapulgite ore, sieving with a 80-mesh sieve to obtain attapulgite powder, placing 100g of the attapulgite powder in 1000mL of 50 wt% citric acid solution, and stirring and reacting at 80 ℃ for 20min, wherein sodium bicarbonate is slowly added in the stirring process, and the total addition amount is 5 g. And after the reaction is finished, centrifuging the product at 700r/min for 30min, filtering, and drying the precipitate at 60 ℃ to obtain the modified attapulgite. Dissolving 100g of multilayer graphene oxide in 100mL of acetone, then dropwise adding 2mL of dichloropropane, carrying out microwave for 50min under the action of a microwave field, and then drying for 80min at 70 ℃ to obtain the expanded multilayer graphene oxide. And mixing and uniformly stirring the obtained multilayer graphene oxide subjected to layer expansion with the obtained modified attapulgite, then adding the mixture into 150mL of 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution for mixing and stirring, wherein 1mL of DMF is slowly dripped in the stirring process, after the dripping is finished, ultrasonically treating the mixture for 30min, treating the mixture at a high temperature of 700 ℃ for 4h, washing the treated product with deionized water, and then placing the washed product in an oven at a temperature of 60 ℃ for drying overnight to obtain the heavy metal removal material.
Example 6
Preparing a 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution: dissolving 1.5g of 2, 3-dihydroxy naphthalene-6-sodium sulfonate in 200mL of sodium hydroxide solution, and uniformly stirring.
The preparation method comprises the steps of crushing raw attapulgite ore, sieving with a 80-mesh sieve to obtain attapulgite powder, placing 100g of the attapulgite powder in 600mL of 50 wt% acetic acid solution, and stirring and reacting at 80 ℃ for 30min, wherein sodium bicarbonate is slowly added in the stirring process, and the total addition amount is 4 g. And after the reaction is finished, centrifuging the product at 600r/min for 40min, filtering, and drying the precipitate at 60 ℃ to obtain the modified attapulgite. Dissolving 100g of multilayer graphene oxide in 100mL of acetone, then dropwise adding 3mL of dichloropropane, carrying out microwave for 60min under the action of a microwave field, and then drying for 80min at 90 ℃ to obtain the expanded multilayer graphene oxide. And mixing and uniformly stirring the obtained multilayer graphene oxide subjected to layer expansion with the obtained modified attapulgite, then adding the mixture into 150mL of 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution for mixing and stirring, wherein 1mL of DMF is slowly dripped in the stirring process, after the dripping is finished, ultrasonically treating the mixture for 30min, treating the mixture at a high temperature of 700 ℃ for 3h, washing the treated product with deionized water, and then placing the washed product in an oven at a temperature of 60 ℃ for drying overnight to obtain the heavy metal removal material.
Example 7
Preparing a 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution: dissolving 1.5g of 2, 3-dihydroxy naphthalene-6-sodium sulfonate in 200mL of sodium hydroxide solution, and uniformly stirring.
The preparation method comprises the steps of crushing raw attapulgite ore, sieving with a 80-mesh sieve to obtain attapulgite powder, placing 100g of the attapulgite powder in 700mL of 60 wt% glycolic acid solution, and stirring and reacting at 70 ℃ for 30min, wherein sodium bicarbonate is slowly added in the stirring process, and the total addition amount is 6 g. And after the reaction is finished, centrifuging the product at 600r/min for 40min, filtering, and drying the precipitated product at 70 ℃ to obtain the modified attapulgite. Dissolving 100g of multilayer graphene oxide in 100mL of acetone, then dropwise adding 2mL of dichloropropane, carrying out microwave under the action of a microwave field for 40min, and then drying at 80 ℃ for 70min to obtain the expanded multilayer graphene oxide. And mixing and uniformly stirring the obtained multilayer graphene oxide subjected to layer expansion with the obtained modified attapulgite, then adding the mixture into 200mL of 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution for mixing and stirring, wherein 1mL of DMF is slowly dripped in the stirring process, after the dripping is finished, ultrasonically treating the mixture for 30min, treating the mixture at a high temperature of 700 ℃ for 4h, washing the treated product with deionized water, and then placing the washed product in an oven at a temperature of 60 ℃ for drying overnight to obtain the heavy metal removal material.
Example 8
Preparing a 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution: dissolving 1.5g of 2, 3-dihydroxy naphthalene-6-sodium sulfonate in 200mL of sodium hydroxide solution, and uniformly stirring.
The preparation method comprises the steps of crushing raw attapulgite ore, sieving with a 80-mesh sieve to obtain attapulgite powder, placing 100g of the attapulgite powder in 900mL of 55 wt% oxalic acid solution, and stirring and reacting at 70 ℃ for 40min, wherein sodium bicarbonate is slowly added in the stirring process, and the total addition amount is 5 g. And after the reaction is finished, centrifuging the product at 800r/min for 40min, filtering, and drying the precipitate at 60 ℃ to obtain the modified attapulgite. Dissolving 100g of multilayer graphene oxide in 100mL of acetone, then dropwise adding 1mL of dichloropropane, carrying out microwave treatment for 50min under the action of a microwave field, and then drying at 90 ℃ for 60min to obtain the expanded multilayer graphene oxide. And mixing and uniformly stirring the obtained multilayer graphene oxide subjected to layer expansion with the obtained modified attapulgite, then adding the mixture into 200mL of 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution for mixing and stirring, wherein 1mL of DMF is slowly dripped in the stirring process, after the dripping is finished, ultrasonically treating the mixture for 30min, treating the mixture at the high temperature of 800 ℃ for 4h, washing the treated product with deionized water, and then placing the washed product in an oven at the temperature of 60 ℃ for drying overnight to obtain the heavy metal removal material.
Comparative example 1
The preparation method comprises the steps of crushing raw attapulgite ore, sieving with a 80-mesh sieve to obtain attapulgite powder, placing 100g of the attapulgite powder in 800mL of 50 wt% acetic acid solution, and stirring and reacting at 70 ℃ for 30min, wherein sodium bicarbonate is slowly added in the stirring process, and the total addition amount is 5 g. And after the reaction is finished, centrifuging the product at 700r/min for 20min, filtering, and drying the precipitated product at 70 ℃ to obtain the modified attapulgite. Dissolving 100g of multilayer graphene oxide in 100mL of water, performing microwave treatment for 50min under the action of a microwave field, drying at 80 ℃ for 70min, mixing and uniformly stirring the obtained product and the obtained modified attapulgite, adding the mixture into 150mL of deionized water, mixing and stirring, slowly dropwise adding 1mL of DMF in the stirring process, performing ultrasonic treatment on the mixture for 30min after dropwise adding is completed, performing high-temperature treatment on the mixture at 700 ℃ for 3h, washing the treated product with deionized water, and drying in an oven at 60 ℃ overnight to obtain the heavy metal removal material.
Test example 1 evaluation of heavy Metal removing Effect of heavy Metal removing Material on removing heavy Metal ions from Sewage
The method comprises the steps of taking 1000mL of simulated electroplating wastewater, wherein the contents of cadmium, chromium, arsenic, lead and nickel are respectively 20mg/L, adding the heavy metal removal materials of the embodiments 1-8 and the heavy metal removal material of the comparative example 1, respectively 5mg, stirring for 5 minutes, standing for 15 minutes, taking supernate, and detecting the content of the heavy metal by using an atomic absorption spectrophotometer, wherein the specific results are shown in the following table 1, wherein the concentration unit of each substance is mg/L.
TABLE 1 concentration of each metal ion
| Numbering | Cadmium (Cd) | Chromium (III) | Arsenic (As) | Lead (II) | Nickel (II) |
| Example 1 | 0.08 | 0.06 | 0.05 | 0.05 | 0.03 |
| Example 2 | 0.10 | 0.08 | 0.08 | 0.13 | 0.09 |
| Example 3 | 0.09 | 0.24 | 0.06 | 0.18 | 0.17 |
| Example 4 | 0.13 | 0.15 | 0.11 | 0.09 | 0.12 |
| Example 5 | 0.04 | 0.21 | 0.15 | 0.07 | 0.11 |
| Example 6 | 0.16 | 0.12 | 0.06 | 0.22 | 0.14 |
| Example 7 | 0.12 | 0.13 | 0.07 | 0.17 | 0.10 |
| Example 8 | 0.11 | 0.21 | 0.16 | 0.14 | 0.18 |
| Comparative example 1 | 21.65 | 19.21 | 16.82 | 20.44 | 19.66 |
As can be seen from the results in Table 1, the heavy metal removing material of the present invention can effectively remove heavy metal ions in wastewater with a remarkable effect. Compared with comparative example 1, the multilayer graphene oxide in the environment of acetone and dichloropropane can promote the progress of the layer expanding effect of the graphene oxide, and the layer expanding effect is improved. The removal rate of the whole material to heavy metals can be promoted by adding the 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution, and the effect is obvious. Therefore, the 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution can enhance the performance of the whole material and improve the adsorption effect on heavy metal ions.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A method of preparing a heavy metal removal material, the method comprising the steps of:
crushing raw attapulgite ore, sieving with a 80-mesh sieve to obtain attapulgite powder, placing the attapulgite powder in 40-60 wt% of organic acid solution, stirring and reacting at 60-80 ℃ for 20-40 min, slowly adding sodium bicarbonate during stirring, centrifugally filtering a product after reaction is finished, and drying a precipitate at 60-80 ℃ to obtain modified attapulgite;
dissolving multilayer graphene oxide in acetone, then dropwise adding dichloropropane, performing microwave for 30-60 min under the action of a microwave field, and then drying at 60-100 ℃ for 60-80 min to obtain the multilayer graphene oxide subjected to layer expansion;
and mixing and uniformly stirring the obtained multilayer graphene oxide subjected to layer expansion with the obtained modified attapulgite, adding the mixture into a 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution, mixing and stirring, slowly dropwise adding DMF (dimethyl formamide) in the stirring process, carrying out ultrasonic treatment on the mixture for 30min after dropwise adding, carrying out high-temperature treatment, washing and drying the treated product, and thus obtaining the heavy metal removal material.
2. The method of claim 1, wherein the organic acid comprises oxalic acid, acetic acid, glycolic acid, citric acid.
3. The preparation method according to claim 1, wherein the ratio of the organic acid solution to the attapulgite powder is (5-10) mL: 1g of the total weight of the composition.
4. The preparation method according to claim 1, wherein the mass ratio of the sodium bicarbonate to the attapulgite powder is (0.04-0.06): 1.
5. the method of claim 1, wherein the centrifugation conditions are: the rotating speed is 600-800 r/min, and the time is 10-30 min.
6. The method of claim 1, wherein the sodium 2, 3-dihydroxynaphthalene-6-sulfonate solution is prepared by the following method: dissolving 2, 3-dihydroxy naphthalene-6-sodium sulfonate in sodium hydroxide solution to obtain 2, 3-dihydroxy naphthalene-6-sodium sulfonate solution.
7. The method according to claim 6, wherein the ratio of sodium 2, 3-dihydroxynaphthalene-6-sulfonate to sodium hydroxide solution is 1 g: (100-300) mL.
8. The method according to claim 1, wherein the high-temperature treatment conditions are: the temperature is 600-800 ℃, and the time is 2-4 h.
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