CN118059840B - Barium sulfate composite porous adsorption material and preparation method thereof - Google Patents
Barium sulfate composite porous adsorption material and preparation method thereof Download PDFInfo
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- CN118059840B CN118059840B CN202410350075.6A CN202410350075A CN118059840B CN 118059840 B CN118059840 B CN 118059840B CN 202410350075 A CN202410350075 A CN 202410350075A CN 118059840 B CN118059840 B CN 118059840B
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- propane sulfonate
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- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 title claims abstract description 131
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 46
- 239000000463 material Substances 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 150000001412 amines Chemical class 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 11
- UNXCZDNUXJJWHY-UHFFFAOYSA-M sodium;2-hydroxypropane-1-sulfonate Chemical compound [Na+].CC(O)CS([O-])(=O)=O UNXCZDNUXJJWHY-UHFFFAOYSA-M 0.000 claims abstract description 11
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000746 purification Methods 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 238000004065 wastewater treatment Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 27
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 21
- 229910001626 barium chloride Inorganic materials 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 13
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 9
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 9
- 235000011152 sodium sulphate Nutrition 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000001953 recrystallisation Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 2
- TZLNJNUWVOGZJU-UHFFFAOYSA-M sodium;3-chloro-2-hydroxypropane-1-sulfonate Chemical compound [Na+].ClCC(O)CS([O-])(=O)=O TZLNJNUWVOGZJU-UHFFFAOYSA-M 0.000 claims 1
- 229910021645 metal ion Inorganic materials 0.000 abstract description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 6
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 4
- 230000000536 complexating effect Effects 0.000 abstract description 3
- 230000003993 interaction Effects 0.000 abstract description 3
- 229910052708 sodium Inorganic materials 0.000 abstract description 3
- 239000011734 sodium Substances 0.000 abstract description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 2
- 125000004356 hydroxy functional group Chemical group O* 0.000 abstract description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910001987 mercury nitrate Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- DRXYRSRECMWYAV-UHFFFAOYSA-N nitrooxymercury Chemical compound [Hg+].[O-][N+]([O-])=O DRXYRSRECMWYAV-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J20/045—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 containing sulfur, e.g. sulfates, thiosulfates, gypsum
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- 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
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- B01J20/28011—Other properties, e.g. density, crush strength
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention relates to the technical field of barium sulfate, and discloses a barium sulfate composite porous adsorption material and a preparation method thereof, the invention utilizes diethanolamine and 3-chlorine-2-hydroxy sodium propane sulfonate to react to obtain diethanol (2-hydroxy sodium propane sulfonate) amine. The method comprises the steps of modifying diethanol (sodium 2-hydroxy propane sulfonate) amine into porous nano barium sulfate by utilizing interaction between sodium sulfonate and the surface of nano barium sulfate, introducing a large number of active hydroxy functional groups into the surface, and enabling hydroxy groups to have strong coordination complexing action with metal ions such as Cu 2+、Hg2+ and the like, so that the adsorption performance of the porous nano barium sulfate on the metal ions is improved. Has high adsorption rate to heavy metals such as Cu 2+、Hg2+. The practical application of the barium sulfate in the field of metal-containing wastewater treatment and purification is expanded.
Description
Technical Field
The invention relates to the technical field of barium sulfate, in particular to a barium sulfate composite porous adsorption material and a preparation method thereof.
Background
Electroplating wastewater and mining wastewater contain a large amount of toxic heavy metal ions such as copper, mercury, chromium and the like, and the treatment of the wastewater is urgent; common treatment methods mainly comprise an adsorption method, a precipitation method, a membrane separation method and the like, wherein the adsorption method is simple and convenient to operate and low in cost. And the adsorption materials are very rich in types, such as active porous carbon, porous titanium dioxide, porous molecular sieve and the like. The nano barium sulfate has higher specific surface area, is nontoxic and pollution-free, and has wide application prospect in the field of wastewater treatment and purification. The patent CN102266744B discloses preparation and application of an acidic medium black T-barium sulfate adsorption material, and discloses a preparation method which takes materials such as barium sulfate and the like as a framework and takes acidic medium black T as an inclusion material to form an adsorption material in a composite manner. However, the adsorbent has a small specific surface area and limited adsorption performance. The specific surface area of the barium sulfate material is increased, and the adsorption performance of heavy metal ions is improved.
Disclosure of Invention
The invention provides a barium sulfate composite porous adsorption material applied to metal-containing wastewater treatment and purification.
The technical scheme is as follows: the preparation method of the barium sulfate composite porous adsorption material comprises the following steps: adding porous nano barium sulfate into dimethyl sulfoxide, dispersing by ultrasonic, adding diethanol (sodium 2-hydroxy propane sulfonate) amine, reacting for 3-8h at 20-40 ℃, centrifuging, washing with water, and drying to obtain the barium sulfate composite porous adsorption material.
Wherein the mass ratio of the porous nano barium sulfate to the diethanol (sodium 2-hydroxy propane sulfonate) amine is 1g (0.1-2 g).
The preparation method of the porous nano barium sulfate comprises the following steps: adding polyvinyl alcohol into distilled water, heating, stirring and dissolving, then cooling to 50-60 ℃, adding barium chloride, and stirring for 4-8 hours to obtain a barium chloride solution; adding sodium sulfate into an ethanol water solution with the volume fraction of 60-75%, dropwise adding ammonia water to adjust the pH value to 8-9, then dropwise adding the solution into a barium chloride solution, stirring and reacting for 1-2h, centrifugally separating, washing with water and ethanol, drying, and then placing the product into a muffle furnace for calcining to obtain the porous nano barium sulfate.
Wherein the mass ratio of the polyvinyl alcohol to the barium chloride to the sodium sulfate is (0.3-0.8) 1:0.68.
The preparation method of the diethanol (2-hydroxy sodium propane sulfonate) amine comprises the following steps: adding diethanolamine and 3-chlorine-2-hydroxy sodium propane sulfonate into 5-8% sodium hydroxide aqueous solution, reacting for 4-10h at 35-60 ℃, cooling, dripping hydrochloric acid to adjust pH to 7-8, heating and evaporating for recrystallization to obtain diethanol (2-hydroxy sodium propane sulfonate) amine. The structural formula is as follows:
Wherein the mass ratio of the diethanolamine to the 3-chlorine-2-hydroxy sodium propane sulfonate is (0.55-0.63): 1.
Wherein, the barium sulfate composite porous adsorption material is applied to the treatment and purification of metal-containing wastewater.
The technical effects are as follows: according to the invention, polyvinyl alcohol is used as a template agent, a large amount of hydroxyl groups are contained, the polyvinyl alcohol and the Ba 2+ of barium chloride are subjected to complexation, ba 2+ is loaded into a polyvinyl alcohol molecular chain, then the polyvinyl alcohol is reacted with sodium sulfate, nano barium sulfate is generated in situ in the polyvinyl alcohol molecular chain, the polyvinyl alcohol template agent is removed through calcination, a large amount of pore channel structures are formed in the nano barium sulfate, and the porous nano barium sulfate is obtained, and has higher specific surface area and better adsorption performance.
The invention utilizes diethanolamine and 3-chlorine-2-hydroxy sodium propane sulfonate to react to obtain diethanol (2-hydroxy sodium propane sulfonate) amine. The method comprises the steps of modifying diethanol (sodium 2-hydroxy propane sulfonate) amine into porous nano barium sulfate by utilizing interaction between sodium sulfonate and the surface of nano barium sulfate, introducing a large number of active hydroxy functional groups into the surface, and enabling hydroxy groups to have strong coordination complexing action with metal ions such as Cu 2+、Hg2+ and the like, so that the adsorption performance of the porous nano barium sulfate on the metal ions is improved. And the porous nano barium sulfate is subjected to surface modification by diethanol (sodium 2-hydroxy propane sulfonate) amine, so that the porous nano barium sulfate has better dispersibility in water, is not easy to agglomerate, and further improves the adsorption performance. Has high adsorption rate to heavy metals such as Cu 2+、Hg2+. The practical application of the barium sulfate in the field of metal-containing wastewater treatment and purification is expanded.
Drawings
FIG. 1 is a scanning electron microscope image of porous nano barium sulfate.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) Adding 0.3g of polyvinyl alcohol into 120mL of distilled water, heating, stirring and dissolving, cooling to 60 ℃, adding 1g of barium chloride, and stirring for 4 to obtain a barium chloride solution; adding 0.68g of sodium sulfate into 120mL of 65% ethanol water solution, dropwise adding ammonia water to adjust the pH value to 9, then dropwise adding the solution into barium chloride solution, stirring and reacting for 2h, centrifugally separating, washing with water and ethanol, drying, and then placing the product into a muffle furnace for calcination to obtain the porous nano barium sulfate.
(2) 1.1G of diethanolamine and 2g of 3-chloro-2-hydroxy sodium propane sulfonate are added into 20mL of sodium hydroxide aqueous solution with mass fraction of 5% to react for 8 hours at 60 ℃, cooling is carried out, hydrochloric acid is added dropwise to adjust pH to 7, heating evaporation is carried out, and recrystallization is carried out, thus obtaining diethanol (2-hydroxy sodium propane sulfonate) amine. The reaction formula is as follows:
(3) 10g of porous nano barium sulfate is added into 150mL of dimethyl sulfoxide, ultrasonic dispersion is carried out, then 1g of diethanol (2-hydroxy sodium propane sulfonate) amine is added for reaction for 8 hours at the temperature of 30 ℃, centrifugal separation is carried out after the reaction, water washing and drying are carried out, and the barium sulfate composite porous adsorption material is obtained.
Example 2
(1) Adding 0.5g of polyvinyl alcohol into 120mL of distilled water, heating, stirring and dissolving, cooling to 50 ℃, adding 1g of barium chloride, and stirring for 6 hours to obtain a barium chloride solution; adding 0.68g of sodium sulfate into 120mL of ethanol water solution with the volume fraction of 75%, dropwise adding ammonia water to adjust the pH value to 9, then dropwise adding the solution into barium chloride solution, stirring and reacting for 2h, centrifugally separating, washing with water and ethanol, drying, and then placing the product into a muffle furnace for calcination to obtain the porous nano barium sulfate.
(2) 1.26G of diethanolamine and 2g of 3-chloro-2-hydroxy sodium propane sulfonate are added into 20mL of sodium hydroxide aqueous solution with mass fraction of 8% to react for 10 hours at 35 ℃, cooling is carried out, hydrochloric acid is added dropwise to adjust pH to 7, heating evaporation is carried out, and recrystallization is carried out, thus obtaining diethanol (2-hydroxy sodium propane sulfonate) amine.
(3) Adding 10g of porous nano barium sulfate into 200mL of dimethyl sulfoxide, dispersing by ultrasonic, adding 10g of diethanol (sodium 2-hydroxy propane sulfonate) amine, reacting for 8 hours at 20 ℃, centrifuging after the reaction, washing with water, and drying to obtain the barium sulfate composite porous adsorption material.
Example 3
(1) Adding 0.8g of polyvinyl alcohol into 120mL of distilled water, heating, stirring and dissolving, cooling to 60 ℃, adding 1g of barium chloride, and stirring for 4 hours to obtain a barium chloride solution; adding 0.68g of sodium sulfate into 120mL of ethanol water solution with the volume fraction of 75%, dropwise adding ammonia water to adjust the pH value to 9, then dropwise adding the solution into barium chloride solution, stirring and reacting for 1h, centrifugally separating, washing with water and ethanol, drying, and then placing the product into a muffle furnace for calcination to obtain the porous nano barium sulfate.
(2) 1.1G of diethanolamine and 2g of 3-chloro-2-hydroxy sodium propane sulfonate are added into 15mL of sodium hydroxide aqueous solution with mass fraction of 5% to react for 4 hours at 50 ℃, cooling is carried out, hydrochloric acid is added dropwise to adjust pH to 8, heating evaporation is carried out, and recrystallization is carried out, thus obtaining diethanol (2-hydroxy sodium propane sulfonate) amine.
(3) Adding 10g of porous nano barium sulfate into 300mL of dimethyl sulfoxide, dispersing by ultrasonic, adding 20g of diethanol (sodium 2-hydroxy propane sulfonate) amine, reacting for 3 hours at 40 ℃, centrifuging, washing with water and drying to obtain the barium sulfate composite porous adsorption material.
Comparative example 1 is porous nano barium sulfate. The preparation method is the same as in example 1.
Comparative example 2
(1) 1G of barium chloride is added into 120mL of distilled water, and the mixture is stirred for 4 to obtain a barium chloride solution; adding 0.68g of sodium sulfate into 120mL of ethanol water solution with the volume fraction of 65%, dropwise adding ammonia water to adjust the pH value to 9, then dropwise adding the solution into barium chloride solution, stirring and reacting for 2h, centrifugally separating, washing with water and ethanol, and drying to obtain the nano barium sulfate.
(2) 10G of nano barium sulfate is added into 150mL of dimethyl sulfoxide, ultrasonic dispersion is carried out, then 1g of diethanol (2-hydroxy sodium propane sulfonate) amine (the preparation method is the same as that of the example 1) is added, the reaction is carried out for 8 hours at the temperature of 30 ℃, centrifugal separation is carried out after the reaction, and the barium sulfate composite adsorption material is obtained after washing and drying.
1L of copper nitrate or mercury nitrate aqueous solution (the mass concentration of Cu 2+ or Hg 2+ is 100 mg/L) is prepared, 2g of barium sulfate composite porous adsorption material is added, adsorption is carried out at 25 ℃, the supernatant is taken every 0.5h, the concentration is measured by an atomic absorption photometry, and the adsorption rate Q is calculated. Q= (C 0-C)/C0×100％.C0 is the initial mass concentration of the solution, C is the mass concentration of the solution after adsorption.
TABLE 1 Cu 2+ adsorption Performance test
TABLE 2 Hg 2+ adsorption Performance test
The barium sulfate composite porous adsorption material prepared in the examples 1 to 3 contains a large number of porous structures, has higher specific surface area and better adsorption performance, and simultaneously utilizes the interaction between sodium sulfonate groups of diethanol (2-hydroxy sodium propane sulfonate) amine and the surface of nano barium sulfate, a large number of active hydroxyl functional groups are introduced into the surface, and the hydroxyl groups can have strong coordination complexing effect with metal ions such as Cu 2+、Hg2+, so that the adsorption performance of the porous nano barium sulfate on the metal ions is improved. And the porous nano barium sulfate is subjected to surface modification by diethanol (sodium 2-hydroxy propane sulfonate) amine, so that the porous nano barium sulfate has better dispersibility in water, is not easy to agglomerate, and further improves the adsorption performance. The adsorption rate of Cu 2+ in examples 1 to 3 was up to 93.1%, and the adsorption rate of Hg 2+ was up to 82.3%.
Comparative example 1 is porous nano barium sulfate, which is not subjected to surface modification by diethanol (sodium 2-hydroxy propane sulfonate) amine, does not introduce active hydroxyl functional groups on the surface, is easy to agglomerate in water, and has poor adsorption performance on metal ions such as Cu 2+、Hg2+.
The nano barium sulfate prepared in comparative example 2 does not contain a porous structure, has a low specific surface area, and has adsorption performance lower than that of examples 1 to 3.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (7)
1. The preparation method of the barium sulfate composite porous adsorption material is characterized by comprising the following steps of: adding porous nano barium sulfate into dimethyl sulfoxide, dispersing by ultrasonic, adding diethanol (sodium 2-hydroxy propane sulfonate) amine, centrifuging after reaction, washing and drying to obtain a barium sulfate composite porous adsorption material;
the mass ratio of the porous nano barium sulfate to the diethanol (2-hydroxy sodium propane sulfonate) amine is 1g (0.1-2 g);
the preparation method of the porous nano barium sulfate comprises the following steps: adding polyvinyl alcohol into distilled water, heating, stirring and dissolving, then cooling to 50-60 ℃, adding barium chloride, and stirring for 4-8 hours to obtain a barium chloride solution; adding sodium sulfate into an ethanol water solution, dropwise adding ammonia water to adjust the pH to 8-9, then dropwise adding the solution into a barium chloride solution, stirring and reacting for 1-2h, centrifugally separating, washing, drying, and then placing the product into a muffle furnace for calcining to obtain porous nano barium sulfate; the mass ratio of the polyvinyl alcohol to the barium chloride to the sodium sulfate is (0.3-0.8) 1:0.68.
2. The method for producing a barium sulfate composite porous adsorbing material according to claim 1, wherein in the method for producing a barium sulfate composite porous adsorbing material, the reaction is carried out at a temperature of 20 to 40 ℃ for 3 to 8 hours.
3. The method for preparing a barium sulfate composite porous adsorption material according to claim 1, wherein the volume fraction of the ethanol aqueous solution is 60-75%.
4. The method for preparing the barium sulfate composite porous adsorption material according to claim 1, wherein the method for preparing the diethanol (sodium 2-hydroxy propane sulfonate) amine is as follows: adding diethanolamine and 3-chlorine-2-hydroxy sodium propane sulfonate into sodium hydroxide aqueous solution, reacting for 4-10h at 35-60 ℃, cooling, dripping hydrochloric acid to adjust pH to 7-8, heating and evaporating for recrystallization, and obtaining diethanol (2-hydroxy sodium propane sulfonate) amine.
5. The method for preparing a barium sulfate composite porous adsorption material according to claim 4, wherein the mass fraction of the sodium hydroxide aqueous solution is 5-8%.
6. The method for preparing a barium sulfate composite porous adsorption material according to claim 4, wherein the mass ratio of diethanolamine to sodium 3-chloro-2-hydroxy propane sulfonate is (0.55-0.63): 1.
7. Use of the barium sulfate composite porous adsorption material obtained by the preparation method according to any one of claims 1 to 6 in metal-containing wastewater treatment and purification.
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