CN116328714A - Silicon-phosphorus modified alumina and application thereof to adsorption and regeneration of anionic dye - Google Patents
Silicon-phosphorus modified alumina and application thereof to adsorption and regeneration of anionic dye Download PDFInfo
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- CN116328714A CN116328714A CN202310541924.1A CN202310541924A CN116328714A CN 116328714 A CN116328714 A CN 116328714A CN 202310541924 A CN202310541924 A CN 202310541924A CN 116328714 A CN116328714 A CN 116328714A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 43
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 230000008929 regeneration Effects 0.000 title claims abstract description 25
- 238000011069 regeneration method Methods 0.000 title claims abstract description 25
- 125000000129 anionic group Chemical group 0.000 title claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 16
- 239000011148 porous material Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- -1 silicon-phosphorus modified boehmite Chemical class 0.000 claims abstract description 10
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 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 claims abstract description 6
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 6
- 239000010452 phosphate Substances 0.000 claims abstract description 6
- 239000011734 sodium Substances 0.000 claims abstract description 6
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000003463 adsorbent Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 238000003795 desorption Methods 0.000 claims description 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 claims 1
- 239000000975 dye Substances 0.000 abstract description 15
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 abstract description 12
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 abstract description 9
- 239000003054 catalyst Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 239000010842 industrial wastewater Substances 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 239000005416 organic matter Substances 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 239000010815 organic waste Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001694 spray drying Methods 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28076—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being more than 1.0 ml/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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Abstract
The invention discloses silicon-phosphorus modified alumina and application thereof to adsorption and regeneration of anionic dye. The method comprises the steps of dripping water glass and a compound containing phosphate radicals into a mixed solution of an aluminum sulfate solution and a sodium metaaluminate solution, and crystallizing to obtain slurry; filtering, washing and drying the slurry to obtain silicon-phosphorus modified boehmite; roasting the silicon-phosphorus modified boehmite at 600-1000 ℃ for 1-4h to obtain the silicon-phosphorus modified alumina. The prepared silicon-phosphorus modified alumina has large specific surface area and pore volume and has excellent adsorption effect on anionic dyes, especially Congo red and methyl blue. In addition, by utilizing the high thermal stability, the adsorption capacity of the high-temperature regeneration catalyst for 6 times is 96% of the primary adsorption capacity of Congo red and methyl blue. The adsorption and regeneration performances of the catalyst are superior to those of adsorption materials reported in literature, and the industrial wastewater treatment cost is further reduced.
Description
Technical Field
The invention belongs to the technical field of modified alumina, and particularly relates to silicon-phosphorus modified alumina and application thereof to adsorption and regeneration of anionic dye.
Background
Organic waste materials in waste water of pharmaceutical industry and dye industry can severely pollute the environment, and the organic waste materials generally have the characteristics of high toxicity, easy carcinogenesis and difficult degradation, so the method has important significance for the treatment and research of the pollutants, such as environmental safety, people health and the like.
At present, in the treatment of organic matter-containing wastewater in the pharmaceutical industry, an important method is spray drying and then high-temperature incineration, but the problems of complex operation, high equipment requirement and high energy consumption exist; if the organic matter is adsorbed by the adsorbent in the waste water containing the organic matter, and then the adsorbent adsorbing the organic matter is roasted, the method is more economical, the operation is simple, the adsorbent can be recycled, and the key of industrial application of the method is that the adsorbent has excellent thermal stability in the high-temperature regeneration process. The active alumina has larger specific surface area and pore volume, the isoelectric point is generally more than 7, and more of the active alumina is used as an adsorption material of industrial anionic dye in recent years, but the specific surface area and pore volume of the active alumina can be greatly reduced due to self sintering and crystal form change under high-temperature roasting, which is unfavorable for repeated use. The thermal stability of the alumina can be improved by modifying the alumina, so that the alumina adsorbent has certain regeneration performance.
Disclosure of Invention
The invention aims to solve the problem that the adsorption quantity of an alumina adsorbent in the prior art is reduced more during re-adsorption after high-temperature regeneration, and provides a silicon-phosphorus modified alumina adsorbent with high thermal stability, which is applied to the adsorption of anionic dyes in water and repeated circularity after regeneration. The adsorbent has strong thermal stability and good regeneration performance, can still maintain extremely strong adsorption effect after multiple regenerations, and greatly reduces the treatment cost of industrial wastewater.
The preparation method of the silicon-phosphorus modified alumina comprises the following steps: dripping water glass and a phosphate radical-containing compound into a mixed solution of an aluminum sulfate solution and a sodium metaaluminate solution, and crystallizing to obtain slurry; filtering, washing and drying the slurry to obtain silicon-phosphorus modified boehmite; roasting the silicon-phosphorus modified boehmite at 600-1000 ℃ for 1-4h to obtain the silicon-phosphorus modified alumina.
The roasting temperature is 400-600 ℃, and the roasting time is 2-3h.
The phosphate radical-containing compound is one or more of disodium hydrogen phosphate, sodium dihydrogen phosphate, dipotassium hydrogen phosphate and potassium dihydrogen phosphate.
The concentration of the aluminum sulfate solution is 0.1-0.7mol/kg.
The molar ratio of the phosphate-containing compound to the sodium metaaluminate to the aluminum sulfate to the aluminum is 0.01-0.21:0.02-0.71:1, preferably 0.02-0.15:0.03-0.41:1, calculated by silicon element and calculated by phosphorus element.
The specific surface area of the silicon-phosphorus modified boehmite is 500-800m2/g,21-700m2/g, and the pore volume is 0.2-4cm3/g, preferably 3-4cm3/g.
The silicon-phosphorus modified alumina prepared by the method is used as an anionic dye adsorbent in water.
The use method of the silicon-phosphorus modified alumina as an anion dye adsorbent in water comprises the following steps: dispersing silicon-phosphorus modified alumina in an aqueous solution containing anionic dye, stirring for 1-20h, and filtering to remove the anionic dye in the water by adsorption; filtering after the adsorption is finished, drying, and roasting at 400-1000 ℃ for 1-4 hours to finish the desorption regeneration of the adsorbent.
The addition amount of the silicon phosphorus modified alumina in the aqueous solution containing the anionic dye is 0.1-2.0g/L.
The concentration of the anionic dye in the aqueous solution containing the anionic dye is 50-800mg/L, and the pH value of the solution is 2.0-13.0.
The silicon-phosphorus modified alumina prepared by using the cheap and easily available raw materials has large specific surface area and pore volume, and has excellent adsorption effect on anionic dyes, especially Congo red and methyl blue, wherein the adsorption capacity on Congo red can reach 1051.8mg/g, and the adsorption capacity on methyl blue can reach 1312.1mg/g. In addition, by utilizing the high thermal stability, the adsorption capacity of the high-temperature regeneration catalyst for 6 times is 96% of the primary adsorption capacity of Congo red and methyl blue. The adsorption and regeneration performances of the catalyst are superior to those of adsorption materials reported in literature, and the industrial wastewater treatment cost is further reduced.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
Example 1
(1) Adding water glass and disodium hydrogen phosphate into a mixed solution of an aluminum sulfate solution and a sodium metaaluminate solution in a dropwise manner (the Si/Al molar ratio is 0.074, the P/Al molar ratio is 0.087 and the concentration of the aluminum sulfate solution is 0.5 mol/kg), and crystallizing to obtain a slurry; filtering, washing and drying the slurry to obtain silicon-phosphorus modified boehmite; the silicon-phosphorus modified boehmite is roasted for 4 hours at the temperature of 600 ℃ to obtain silicon-phosphorus modified alumina with the specific surface area of 515.2m < 2 >/g and the pore volume of 1.48cm < 3 >/g.
(2) Dispersing 0.2g of silicon phosphorus modified alumina obtained in the step (1) in a Congo red solution with the concentration of 200mg/L and the pH of 7.7, stirring for 10 hours at room temperature, and filtering to finish the adsorption. The adsorption capacity is 906.8mg/L.
(3) The filtered silicon-phosphorus modified alumina is dried, and after roasting for 2 hours at 600 ℃, the regeneration is completed once, the specific surface area is 462.8m2/g, and the pore volume is 1.47cm3/g. The regenerated silicon-phosphorus modified alumina is filtered out after Congo red is adsorbed by the same condition as (2), and the adsorption capacity is 903.8mg/L.
(4) And (3) drying the filtered silicon-phosphorus modified alumina, and roasting at 600 ℃ for 2 hours to complete the second regeneration, wherein the specific surface area is 437.0m2/g, and the pore volume is 1.45cm3/g. The silicon phosphorus-modified alumina regenerated twice was filtered out after adsorbing Congo red using the same conditions as in (2) in example 1, and the adsorption capacity was 905.3mg/L.
(5) The filtered silicon-phosphorus modified alumina is dried, baked for 2 hours at 600 ℃ and then regenerated for the third time, wherein the specific surface area is 428.4m2/g, and the pore volume is 1.42cm3/g. The silicon phosphorus-modified alumina was collected and regenerated three times, and was filtered out after adsorbing Congo red using the same conditions as in (2) in example 1, and its adsorption capacity was 899.4mg/L.
Example 2
(1) 0.2g of the silicon phosphorus modified alumina prepared in the step (1) of example 1 was dispersed in a methyl blue solution having a concentration of 200mg/L and a pH of 5.2, stirred at room temperature for 8 hours, and then filtered to complete adsorption. The adsorption capacity is 822.7mg/L.
(2) The filtered silicon-phosphorus modified alumina was dried, and after 2 hours of calcination at 600 ℃, the regeneration was completed once, with a specific surface area of 467.8m2/g and a pore volume of 1.42cm3/g. The regenerated silicon-phosphorus modified alumina is filtered out after methyl blue is adsorbed by the same condition as (1), and the adsorption capacity is 822.7mg/L.
(3) The filtered silicon-phosphorus modified alumina is dried and baked for 2 hours at 600 ℃ to complete the second regeneration, the specific surface area is 460.6m2/g, and the pore volume is 1.42cm3/g. The silicon-phosphorus modified alumina regenerated twice is taken, methyl blue is adsorbed by the same condition as in (1) and filtered out, and the adsorption capacity is 822.1mg/L.
(4) The filtered silicon-phosphorus modified alumina was dried, and after roasting at 600℃for 2 hours, the third regeneration was completed, with a specific surface area of 446.7m2/g and a pore volume of 1.41cm3/g. The silicon phosphorus modified alumina which is regenerated three times is taken, methyl blue is adsorbed by the same condition as the (1) and filtered out, and the adsorption capacity is 815.6mg/L.
Comparative example 1
The adsorption was performed according to the same conditions as in example 1, except that: alumina (specific surface area 180.4m2/g, pore volume 1.53cm 3/g) calcined from commercial SB powder was used as the adsorbent.
The adsorption capacity of the silicon carbide red is 341.7mg/L, the adsorption capacity of the silicon carbide red after regeneration is 284.0mg/L, and the adsorption capacity of the silicon carbide red after three times of regeneration is 121.3mg/L.
Comparative example 2
Adsorption was performed according to the same conditions as in example 2, except that: alumina calcined from commercial SB powder was used as the adsorbent.
The adsorption capacity of the catalyst for the methyl blue is 730.5mg/L, the adsorption capacity of the catalyst for the methyl blue after one regeneration is 546.1mg/L, and the adsorption capacity of the catalyst for the methyl blue after three regenerations is 468.1mg/L.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. The preparation method of the silicon-phosphorus modified alumina is characterized by comprising the following specific operations: dripping water glass and a phosphate radical-containing compound into a mixed solution of an aluminum sulfate solution and a sodium metaaluminate solution, and crystallizing to obtain slurry; filtering, washing and drying the slurry to obtain silicon-phosphorus modified boehmite; roasting the silicon-phosphorus modified boehmite at 600-1000 ℃ for 1-4h to obtain the silicon-phosphorus modified alumina.
2. The method according to claim 1, wherein the firing temperature is 400 to 600 ℃ and the firing time is 2 to 3 hours.
3. The method according to claim 1, wherein the phosphate group-containing compound is one or more of disodium hydrogen phosphate, sodium dihydrogen phosphate, dipotassium hydrogen phosphate and potassium dihydrogen phosphate.
4. The method according to claim 1, wherein the concentration of the aluminum sulfate solution is 0.1 to 0.7mol/kg.
5. The preparation method according to claim 1, wherein the molar ratio of phosphate-containing compound to sodium metaaluminate and aluminum sulfate to aluminum element is 0.01-0.21:0.02-0.71:1, preferably 0.02-0.15:0.03-0.41:1, calculated as silicon element and phosphorus element.
6. The preparation method according to claim 1, wherein the specific surface area of the silicon phosphorus modified boehmite is 500-800m2/g,21-700m2/g, and the pore volume is 0.2-4cm3/g, preferably 3-4cm3/g.
7. Use of the silicon phosphorus modified alumina prepared according to the method of any one of claims 1-6 as an anionic dye adsorbent in water.
8. The use of claim 7, wherein the silicon phosphorus modified alumina is used as an anionic dye adsorbent in water by: dispersing silicon-phosphorus modified alumina in an aqueous solution containing anionic dye, stirring for 1-20h, and filtering to remove the anionic dye in the water by adsorption; filtering after the adsorption is finished, drying, and roasting at 400-1000 ℃ for 1-4 hours to finish the desorption regeneration of the adsorbent.
9. The use according to claim 8, wherein the silicon phosphorus modified alumina is added to the aqueous solution containing the anionic dye in an amount of 0.1 to 2.0g/L.
10. The use according to claim 8, wherein the concentration of the anionic dye in the aqueous solution containing the anionic dye is 50-800mg/L and the pH of the solution is 2.0-13.0.
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