CN112237899B - Lanthanum-magnesium modified sepiolite for dephosphorization of black and odorous water body - Google Patents
Lanthanum-magnesium modified sepiolite for dephosphorization of black and odorous water body Download PDFInfo
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- 239000004113 Sepiolite Substances 0.000 title claims abstract description 171
- 229910052624 sepiolite Inorganic materials 0.000 title claims abstract description 171
- 235000019355 sepiolite Nutrition 0.000 title claims abstract description 166
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 103
- RIAXXCZORHQTQD-UHFFFAOYSA-N lanthanum magnesium Chemical compound [Mg].[La] RIAXXCZORHQTQD-UHFFFAOYSA-N 0.000 title claims abstract description 95
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 61
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000011574 phosphorus Substances 0.000 claims abstract description 31
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 31
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 230000000694 effects Effects 0.000 claims description 19
- 229910052746 lanthanum Inorganic materials 0.000 claims description 16
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 16
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 15
- 239000011777 magnesium Substances 0.000 claims description 15
- 229910052749 magnesium Inorganic materials 0.000 claims description 15
- 239000011148 porous material Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 12
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 7
- 239000002352 surface water Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 3
- 239000011573 trace mineral Substances 0.000 claims description 3
- 235000013619 trace mineral Nutrition 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 55
- 229920006395 saturated elastomer Polymers 0.000 abstract description 8
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 150000002603 lanthanum Chemical class 0.000 abstract description 4
- 159000000003 magnesium salts Chemical class 0.000 abstract description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 13
- 241000195649 Chlorella <Chlorellales> Species 0.000 description 8
- 239000000706 filtrate Substances 0.000 description 8
- 239000003463 adsorbent Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 241000195493 Cryptophyta Species 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004876 x-ray fluorescence Methods 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000001963 growth medium Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000008520 organization Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005067 remediation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- JSPLKZUTYZBBKA-UHFFFAOYSA-N trioxidane Chemical class OOO JSPLKZUTYZBBKA-UHFFFAOYSA-N 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 229910002422 La(NO3)3·6H2O Inorganic materials 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 159000000014 iron salts Chemical class 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—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
-
- 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
- C02F2101/105—Phosphorus compounds
Abstract
The invention relates to lanthanum-magnesium modified sepiolite for dephosphorization of black and odorous water, which is prepared by modifying natural sepiolite with a lanthanum salt and magnesium salt mixed solution, wherein the adsorption of orthophosphate in 12 h reaches balance, the fitted saturated adsorption amount is up to 119mg/g, the pH (6-9) application range of the lanthanum-magnesium modified sepiolite is wider than that of the natural sepiolite before modification, the lanthanum-magnesium modified sepiolite has high selectivity to orthophosphate in the water, the adsorption treatment to phosphorus (0.5-2.0 mg/L) in urban black and odorous water is excellent, the ecological safety risk is low, and the application prospect is good.
Description
Technical Field
The invention relates to lanthanum-magnesium modified sepiolite for dephosphorization of black and odorous water bodies, and belongs to the field of sewage treatment.
Background
The water pollution control action plan issued and implemented in 2015 of China provides clear requirements for urban black and odorous water body treatment: by 2020, the black and odorous water bodies of the built-up areas of cities above the ground level are controlled within 10 percent; by 2030, the black and odorous water body of the built-up area of the national city is totally eliminated. Black and odorous water body treatment has become one of the most interesting environmental problems in ecological civilization construction and water pollution control in China. The content of total phosphorus in the water environment exceeds the quality standard (GB 3838-2002) of the surface water environment and III-type water quality index (> 0.2 mg/L) is one of main reasons for causing black and odorous water body. The phosphorus element cannot circulate in the natural world, so that aquatic plants such as algae grow excessively to reduce dissolved oxygen in water, and the water body is eutrophicated to finally cause black and odorous water body. Therefore, how to remove phosphorus in black and odorous water bodies by adopting an efficient and green method has become one of the key problems for solving the black and odorous water bodies at present.
Common sewage dephosphorization methods include chemical precipitation, biological, membrane separation and adsorption. For black and odorous water bodies, the total phosphorus concentration is generally 0.5-2.0 mg/L, compared with the high-concentration phosphorus in industrial wastewater, the effect of removing the low-concentration phosphorus (< 2 mg/L) by adopting a chemical precipitation method and a biological method is not ideal, and membrane loss is easy to occur in a membrane separation technology. Compared with the dephosphorization technology, the adsorption method has the advantages of simple operation, low cost, stable operation, no secondary pollution and the like. And the adsorbent with high efficiency, low consumption and environmental protection is selected, so that the removal of phosphorus in the black and odorous water body and the ecological function of the water body are facilitated.
Sepiolite is a fibrous porous magnesium silicate natural mineral, is composed of 2 layers of silicon oxygen tetrahedrons and 1 layer of magnesium oxygen octahedrons, is of a 2:1 chain layered crystal structure, has abundant reserves in China, has been ascertained to be 2600 ten thousand tons, and is in world No. 2. In order to develop sepiolite performance, the physical and chemical properties of the sepiolite can be changed by modification, so that the adsorption performance of the sepiolite is improved. At present, modification of natural sepiolite and application to wastewater dephosphorization treatment are reported, for example, a Chinese patent (CN 2013100705629) activates inert calcium in the natural sepiolite by a heating modification method to obtain a calcium-based sepiolite adsorbent with higher adsorption capacity for phosphorus; there are also modified sepiolite adsorbents prepared by acid activation, magnesium salts, iron salts, aluminum salts, lanthanum salts, and the like. However, the modified sepiolite prepared in the above way has the disadvantages of high cost, low adsorption capacity (less than 70 mg P/g.adsorbent), poor effect of removing low-concentration phosphorus, and the like. Therefore, the natural sepiolite needs to be effectively modified, the adsorption dephosphorization performance of the sepiolite is enhanced, and the characteristics and advantages of the sepiolite natural adsorbent are maintained.
In recent years, composite adsorbents based on two or more metal (hydroxy) oxides have received attention, which are capable of combining not only the advantages of a single metal (hydroxy) oxide, but also tend to exhibit a significant synergistic effect. The rare earth element lanthanum is paid attention to because of its natural affinity to phosphorus and good phosphorus removal effect. However, lanthanum salt particles are easy to agglomerate in water, the surface of the lanthanum salt particles is negatively charged, the dephosphorization utilization rate is low, and the cost is high. Magnesium salt materials are cheap and easy to obtain, the surface of the metal magnesium oxide is positively charged, and can be combined with phosphorus through electrostatic attraction and surface hydroxyl coordination, however, the effect of magnesium adsorption on low-concentration phosphorus is relatively weak. The natural sepiolite with larger specific surface area and porous structure is used as a carrier to prepare the lanthanum-magnesium modified sepiolite, so that positive charges on the surface of the sepiolite can be increased, aggregation of lanthanum-magnesium nanoparticles is reduced, dispersibility of lanthanum oxide and magnesium oxide on the surface of the sepiolite is enhanced, contact and adsorption of the lanthanum oxide and magnesium oxide on orthophosphate are enhanced, adsorption capacity and removal capacity of low-concentration phosphorus are improved, and phosphorus removal adsorption performance of the sepiolite is remarkably enhanced.
Disclosure of Invention
The invention aims to: in order to solve the problem of dephosphorization of black and odorous water, the modified sepiolite is provided for dephosphorization of lanthanum magnesium in black and odorous water.
The technical scheme of the invention is as follows:
1. a lanthanum magnesium modified sepiolite for dephosphorization of black and odorous water body is characterized in that:
(1) The lanthanum-magnesium modified sepiolite has a spherical granular structure and is prepared from SiO 2 、MgO、La 2 O 3 、CaO、Fe 2 O 3 、Al 2 O 3 And other trace elements, the mass contents of which are 37.5%, 40.5%, 7.33%, 10.4%, 1.2%, 2.1% and 0.97%, respectively, and the BET specific surface area is 81 m 2 Per gram, pore volume of 0.34. 0.34 cm 3 /g, pore size 27 nm;
(2) The lanthanum-magnesium modified sepiolite is used for dephosphorizing black and odorous water body and is characterized in that:
1) Putting lanthanum-magnesium modified sepiolite into a simulated black and odorous water body with the orthophosphate content of 2-300 mg/L and the pH value of 7.0+/-0.1, oscillating and dispersing 24-h at 25 ℃ and 200 rpm, and obtaining the fitting saturated adsorption quantity of the orthophosphate in the simulated black and odorous water body by fitting calculation of a Langmuir equation, wherein the fitting saturated adsorption quantity of the orthophosphate in the simulated black and odorous water body is 119-mg/g, and is 55 times higher than the fitting saturated adsorption quantity of the natural sepiolite on the orthophosphate;
2) Adding lanthanum-magnesium modified sepiolite into a simulated black and odorous water body with the orthophosphate content of 200 mg/L and the pH value of 7.0+/-0.1, oscillating and dispersing at 25 ℃ and 200 rpm, and quickly adsorbing orthophosphate in the simulated black and odorous water body in initial 10 h, wherein the adsorption quantity is increased rapidly to 98.43 mg/g, and the adsorption quantity is kept at 102 mg/g after 12 h, so that the adsorption reaches balance;
3) Putting lanthanum-magnesium modified sepiolite into simulated black and odorous water bodies with orthophosphate content of 200 mg/L and different pH values, and oscillating and dispersing at 25 ℃ and 200 rpm for 24 h, wherein the application range of the pH of orthophosphate in the simulated black and odorous water bodies is wider, and the adsorption capacity of lanthanum-magnesium modified sepiolite to orthophosphate is kept at 102 mg/g within the pH range of 6-9;
4) Adding lanthanum-magnesium modified sepiolite into Na with different mass concentrations (0, 50, 100 and 200 mg/L) 2 SO 4 、NaCl、NaNO 3 And NaHCO 3 In a simulated black and odorous water body with the orthophosphate content of 200 mg/L and the pH value of 7.0+/-0.1, and oscillating and dispersing 24 h at 25 ℃ and 200 rpm, the product has high selective adsorption of orthophosphate in the simulated black and odorous water body and common anion SO in the black and odorous water body 4 2- 、Cl - 、NO 3 - And HCO 3 - The influence on the removal of orthophosphate by the lanthanum-magnesium modified sepiolite is small, and the adsorption quantity of the lanthanum-magnesium modified sepiolite on the orthophosphate is kept at 102 mg/g;
5) Adding lanthanum-magnesium modified sepiolite with different mass concentrations (0, 0.01, 0.05, 0.1, 0.5, 1.0 and 5.0 g/L) into ultrapure water, shaking and dispersing at 25deg.C and 200 rpm for 24 h, filtering with 0.45 μm filter head to obtain lanthanum-magnesium modified sepiolite filtrate, inoculating biological chlorella to be tested into OECD (economic Cooperation and development organization) culture medium containing lanthanum-magnesium modified sepiolite filtrate with different mass concentrations, and initial algae cell density of 3.5X10 5 culturing the sample in a constant temperature illumination incubator at 25 ℃ for seven days of biomass of chlorella in the sample every 24 days h, wherein experimental results show that lanthanum-magnesium modified sepiolite filtrate has no inhibition effect on the growth of chlorella, and the lanthanum-magnesium modified sepiolite has low toxicity on the biological growth of water bodies and low ecological safety risk;
6) The lanthanum-magnesium modified sepiolite is put into an actual black and odorous water body 1 (the total phosphorus and orthophosphate concentration are respectively 0.68 mg/L and 0.59 mg/L, the pH value is 7.72) and an actual black and odorous water body 2 (the total phosphorus and orthophosphate concentration are respectively 1.36 mg/L and 1.22 mg/L, the pH value is 7.31), the adding amount is respectively 0.1 g/L and 0.3 g/L, the vibration dispersion is carried out for 24 h at 25 ℃ and 200 rpm, the total phosphorus and orthophosphate in the actual black and odorous water body 1 and the actual black and odorous water body 2 are not more than 0.1 mg/L after being treated by the lanthanum-magnesium modified sepiolite, the water quality standard of surface water II (GB 3838-2002) is achieved, and the treatment effect of the lanthanum-magnesium modified sepiolite is superior to that of lanthanum-loaded modified sepiolite (lanthanum-sepiolite mass ratio of 0.3:1.0) or magnesium-loaded modified sepiolite (magnesium-loaded sepiolite mass ratio of 1.3:0).
2. The lanthanum-magnesium modified sepiolite for dephosphorization of black and odorous water body as described in the claim 1 is prepared by the following method: lanthanum nitrate (La (NO) 3 ) 3 ·6H 2 O) and magnesium chloride (MgCl) 2 ·6H 2 O) mixing lanthanum and magnesium according to the mass ratio of 1:5, controlling the mass concentration of lanthanum nitrate to be 1-2 g/L, adding ultrapure water, stirring and dissolving to avoid the interference of other ions, and obtaining a mixed solution of lanthanum nitrate and magnesium chloride; adding natural sepiolite into the mixed solution of lanthanum nitrate and magnesium chloride according to the mass ratio of the natural sepiolite to lanthanum element 1:0.05 in the mixed solution of lanthanum nitrate and magnesium chloride, and mixing and stirring at 25 ℃ to dissolve the natural sepiolite to obtain an intermediate reaction solution; adjusting the pH value of the intermediate reaction solution to 11-11.5 by using 1-5 mol/L sodium hydroxide solution, stirring for 4-6 hours, carrying out suction filtration, drying a filter cake at 55-75 ℃ for 8-16 hours, grinding, and sieving with 0.15-mm aperture to obtain the lanthanum-magnesium modified sepiolite for dephosphorization of black and odorous water bodies;
the natural sepiolite is prepared by grinding, sieving with 0.15-mm aperture, and has specific surface area of 68 m 2 /g, pore volume of 0.15 cm 3 /g, natural sepiolite with a pore size of 19 nm.
The invention has the advantages compared with the prior art: provides the lanthanum-magnesium modified sepiolite which is high in efficiency, low in consumption, green and environment-friendly and is used for treating black and odorous water bodies. The specific surface area and adsorption sites of the natural sepiolite serving as an adsorption material are effectively improved through lanthanum-magnesium modification, the fitting saturation adsorption quantity of orthophosphate in the black and odorous water body is up to 119mg/g, the adsorption quantity is improved by 55 times compared with that of the natural sepiolite before modification, the adsorption quantity has an excellent removal effect on low-concentration phosphorus (< 2 mg/L) in the actual black and odorous water body, the application range of pH (6-9) is wider, and the ecological safety risk is low. The obtained lanthanum-magnesium modified sepiolite improves the material function of natural sepiolite and has good application prospect in the field of environmental protection.
Drawings
FIG. 1 is an isothermal adsorption curve of natural sepiolite and lanthanum-magnesium modified sepiolite adsorption orthophosphate of example 1, illustrating that the fitted saturated adsorption amount of lanthanum-magnesium modified sepiolite to orthophosphate in simulated black and odorous water body is 119mg/g after being fitted by Langmuir equation, which is 55 times higher than the fitted saturated adsorption amount of natural sepiolite to orthophosphate.
FIG. 2 is a graph of adsorption kinetics of lanthanum magnesium modified sepiolite to orthophosphate of example 2, illustrating that lanthanum magnesium modified sepiolite initially begins within 10 h and the adsorption rate of orthophosphate in simulated black and odorous water bodies is fast, the adsorption capacity increases rapidly to 98.43 mg/g, and the adsorption capacity remains at 102 mg/g after 12 h, the adsorption reaching equilibrium.
Fig. 3 shows the effect of the initial pH of the solution of example 3 on the adsorption of orthophosphate by lanthanum-magnesium modified sepiolite, which illustrates that the application range of the lanthanum-magnesium modified sepiolite to the pH of orthophosphate in a simulated black and odorous water body is wide, and the adsorption amount of the lanthanum-magnesium modified sepiolite to the orthophosphate is kept at 102 mg/g within the pH range of 6-9.
FIG. 4 is a graph showing the effect of coexisting ions of example 4 on adsorption of orthophosphate by lanthanum-magnesium modified sepiolite, illustrating that lanthanum-magnesium modified sepiolite has high selective adsorption of orthophosphate in simulated black and odorous water bodies, and that the anions SO are common in black and odorous water bodies 4 2- 、Cl - 、NO 3 - And HCO 3 - The influence on the removal of orthophosphate is small, and the adsorption quantity of lanthanum-magnesium modified sepiolite on orthophosphate is kept at 102 mg/g.
Fig. 5 is an effect of the lanthanum-magnesium-modified sepiolite filtrate of example 5 on the biomass of chlorella, which shows that the lanthanum-magnesium-modified sepiolite filtrate has no inhibition effect on the growth of chlorella, and the lanthanum-magnesium-modified sepiolite has low biological toxicity to water and low ecological safety risk.
Fig. 6 shows the effect of lanthanum magnesium modified sepiolite of example 6 on total phosphorus and orthophosphate removal in an actual black and odorous water body 1. FIG. 6 shows that when the addition amount of lanthanum-magnesium modified sepiolite is 0.1 g/L, the total phosphorus (0.68 mg/L) and orthophosphate (0.59 mg/L) in the actual black and odorous water body 1 (pH 7.72) are treated by the lanthanum-magnesium modified sepiolite, the concentrations are respectively 0.092 mg/L and 0.064 mg/L, the lanthanum-magnesium modified sepiolite achieves the surface water II-type water quality standard (GB 3838-2002), and the treatment effect of the lanthanum-magnesium modified sepiolite is better than that of lanthanum-loaded modified sepiolite (lanthanum-sepiolite mass ratio of 0.3:1.0) or magnesium-loaded modified sepiolite (magnesium-sepiolite mass ratio of 0.3:1.0) prepared by the same method.
Fig. 7 shows the effect of lanthanum magnesium modified sepiolite of example 7 on total phosphorus and orthophosphate removal in an actual black and odorous water body 2. FIG. 7 shows that when the addition amount of lanthanum-magnesium modified sepiolite is 0.3 g/L, the concentration of total phosphorus (1.36 mg/L) and orthophosphate (1.22 mg/L) in the actual black and odorous water body 2 (pH 7.31) after the lanthanum-magnesium modified sepiolite is treated is 0.088 mg/L and 0.082 mg/L respectively, the lanthanum-magnesium modified sepiolite achieves the quality standard of surface water II (GB 3838-2002), and the treatment effect of the lanthanum-magnesium modified sepiolite is better than that of lanthanum-loaded modified sepiolite (lanthanum-sepiolite mass ratio of 0.3:1.0) or magnesium-loaded modified sepiolite (magnesium-sepiolite mass ratio of 0.3:1.0) prepared by the same method.
Detailed Description
The technical scheme and the implementation mode of the invention are described below by examples, but the invention is not limited to the following examples.
Example 1
9 groups of orthophosphate simulated black and odorous water bodies with different concentrations are prepared, the concentrations are 2, 5, 10, 20, 40, 60, 100, 200 and 300 mg/L from small to large, and 2 mol/L HCl and 2 mol/L NaOH solution are used for regulating the pH value to 7.0+/-0.1.
Preparing lanthanum-magnesium modified sepiolite: lanthanum nitrate 1.56 g (La (NO 3 ) 3 · 6H 2 O) and 20.91 g magnesium chloride (MgCl) 2 · 6H 2 Adding 250 mL ultrapure water, stirring and dissolving to obtain a lanthanum nitrate and magnesium chloride mixed solution; adding 10 g natural sepiolite into a mixed solution of lanthanum nitrate and magnesium chloride, mixing and stirring at 25 ℃ for dissolution to obtain an intermediate reaction solution; adjusting pH of the intermediate reaction solution to 11 with 2 mol/L sodium hydroxide solution, stirring 5. 5 h, vacuum filtering, and oven drying the filter cake at 65deg.C 12. 12 hGrinding and sieving with 0.15-mm aperture to obtain lanthanum-magnesium modified sepiolite.
Natural sepiolite and prepared lanthanum magnesium modified sepiolite are weighed, respectively 0.5 g, and respectively put into 9 groups of simulated black and odorous water bodies of orthophosphate with different concentrations of 500 mL, and are oscillated at 25 ℃ and 200 rpm for 24 h. The experimental results are shown in FIG. 1, and the relevant parameters are shown in Table 1, using Langmuir and Freundlich fitting equations, respectively, to fit the experimental results. The fitting saturated adsorption quantity of lanthanum-magnesium modified sepiolite to orthophosphate in the simulated black and odorous water body is 119mg/g, which is improved by 55 times compared with the fitting saturated adsorption quantity of natural sepiolite to orthophosphate.
TABLE 1 isothermal adsorption curve fitting parameters for natural sepiolite and lanthanum magnesium modified sepiolite adsorption orthophosphates
Example 2
12 groups of orthophosphate with the concentration of 200 mg/L are prepared to simulate black and odorous water body, and 2 mol/L HCl and 2 mol/L NaOH solution are used for regulating the pH value to 7.0+/-0.1.
The lanthanum-magnesium modified sepiolite prepared in example 1 is weighed, each group is put into 0.5-g, and the mixture is respectively put into 500-mL simulated black and odorous water bodies containing 200-mg/L orthophosphate, and the mixture is oscillated for 0.5-48 h at 25 ℃ and 200 rpm. The experimental results are shown in fig. 2, the experimental results are fitted by adopting a quasi-first-order kinetic model and a quasi-second-order kinetic model respectively, and relevant parameters are shown in table 2. Experimental results show that the lanthanum-magnesium modified sepiolite has a fast adsorption rate of orthophosphate in the simulated black and odorous water body in initial 10 h, the adsorption quantity is increased rapidly to 98.43 mg/g, and the adsorption quantity is kept at 102 mg/g in 12 h, so that the adsorption reaches equilibrium.
TABLE 2 kinetic parameters of lanthanum magnesium modified sepiolite adsorption orthophosphate
Example 3
9 groups of orthophosphate simulated black and odorous water bodies with the concentration of 200 mg/L are prepared, and pH values of the orthophosphate simulated black and odorous water bodies are respectively adjusted to 3, 4, 5, 6, 7, 8, 9, 10 and 11 by using 2 mol/L HCl and 2 mol/L NaOH solutions.
Lanthanum magnesium modified sepiolite prepared in example 1 was weighed, each group was put into 0.5. 0.5 g, and each group was put into orthophosphate-containing simulated black and odorous water bodies of different pH values prepared in this example 500 mL, and the results were shown in FIG. 3 by shaking 24 h at 25℃and 200 rpm. Experimental results show that the lanthanum-magnesium modified sepiolite has a wide application range of pH for simulating orthophosphate in black and odorous water, and the adsorption quantity of the lanthanum-magnesium modified sepiolite to the orthophosphate is kept at 102 mg/g within the pH range of 6-9.
Example 4
10 groups of orthophosphate with the concentration of 200 mg/L are configured to simulate black and odorous water bodies, 2 mol/L HCl and 2 mol/L NaOH solution are used for regulating the pH value to 7.0+/-0.1, and Na with different concentrations (0, 50, 100 and 200 mg/L) is respectively added 2 SO 4 、NaCl、NaNO 3 And NaHCO 3 。
The lanthanum magnesium modified sepiolite prepared in example 1 was weighed, each group was put into 0.5. 0.5 g, and each group was put into 500 mL of the orthophosphate-containing simulated black and odorous water bodies with different concentrations of coexisting ions prepared in this example, and the results were shown in FIG. 4 by shaking 24 h at 25℃and 200 rpm. Experimental results show that the lanthanum-magnesium modified sepiolite has high selective adsorption on orthophosphate in simulated black and odorous water bodies, and common anions SO in the black and odorous water bodies 4 2- 、Cl - 、NO 3 - And HCO 3 - The influence on the removal of orthophosphate is small, and the adsorption quantity of lanthanum-magnesium modified sepiolite on orthophosphate is kept at 102 mg/g.
Example 5
7 groups of lanthanum-magnesium modified sepiolite prepared in example 1 were weighed and put into ultrapure water, the mass concentrations of the lanthanum-magnesium modified sepiolite are respectively 0, 0.01, 0.05, 0.1, 0.5, 1.0 and 5.0 g/L, the lanthanum-magnesium modified sepiolite is oscillated for 24 h at 25 ℃ and 200 rpm, and the lanthanum-magnesium modified sepiolite filtrate is obtained after the lanthanum-magnesium modified sepiolite filtrate is filtered by a 0.45-micrometer filter head. Inoculating the tested biological chlorella to OECD (economic Cooperation and development organization) culture containing different concentrations of lanthanum-magnesium modified sepiolite filtrateIn the culture medium, the initial algae density of algae cells is regulated to be 3.5X10 5 The samples were incubated in a constant temperature illumination incubator at 25℃for 24/mL and the biomass of Chlorella in the samples was measured at intervals of h, and the results are shown in FIG. 5. Experimental results show that the lanthanum-magnesium modified sepiolite filtrate has no inhibition effect on the growth of chlorella, and the lanthanum-magnesium modified sepiolite has low biological toxicity to natural water and low ecological safety risk.
Example 6
According to the working guidelines for urban black and odorous water body remediation, water samples of typical black and odorous water bodies 1 in certain cities are collected, and water quality detection results are shown in table 3:
TABLE 3 results of typical black and odorous Water body 1 Water quality detection
Lanthanum-loaded modified sepiolite (lanthanum: sepiolite mass ratio of 0.3:1.0) and magnesium-loaded modified sepiolite (magnesium: sepiolite mass ratio of 0.3:1.0) were prepared as in example 1, respectively.
The lanthanum-magnesium-modified sepiolite prepared in example 1, and the lanthanum-loaded modified sepiolite and magnesium-loaded modified sepiolite prepared in this example were weighed, each set was put into 0.5 g, and put into 500 mL actual black odorous water 1, respectively, and oscillated at 25 ℃ and 200 rpm for 24 h. The concentrations of total phosphorus and orthophosphate in the actual black odorous water 1 after adsorption are shown in fig. 6. Experimental results show that the concentrations of total phosphorus and orthophosphate in the actual black and odorous water body are respectively 0.092 mg/L and 0.064 mg/L after being treated by lanthanum-magnesium modified sepiolite, and the treatment effect of the lanthanum-magnesium modified sepiolite is superior to that of adding lanthanum-loaded modified sepiolite or magnesium-loaded modified sepiolite with the same quality, and the water quality standard of surface water II is achieved (GB 3838-2002).
Example 7
According to the working guidelines for urban black and odorous water body remediation, water samples of typical black and odorous water bodies 2 in certain cities are collected, and water quality detection results are shown in table 4:
TABLE 4 results of typical black and odorous Water body 2 Water quality detection
Lanthanum-magnesium-modified sepiolite prepared in example 1, and lanthanum-loaded modified sepiolite and magnesium-loaded modified sepiolite prepared in example 6 were weighed, each set was put into 0.15 g, put into 500 mL actual black odorous water, and shaken at 25 ℃ and 200 rpm for 24 h. The concentrations of total phosphorus and orthophosphate in the actual black and odorous water after adsorption are shown in fig. 7. Experimental results show that the concentrations of total phosphorus and orthophosphate in the actual black and odorous water body are respectively 0.088 mg/L and 0.082 mg/L after being treated by lanthanum-magnesium modified sepiolite, and the treatment effect of the lanthanum-magnesium modified sepiolite is superior to that of adding lanthanum-loaded modified sepiolite or magnesium-loaded modified sepiolite with the same quality, thereby achieving the water quality standard of surface water class II (GB 3838-2002).
Example 8
This example performs X-ray fluorescence analysis and BET specific surface area analysis on natural sepiolite and lanthanum magnesium modified sepiolite. Tables 5 and 6 show the X-ray fluorescence analysis results and BET specific surface area analysis of the adsorbents, respectively. The X-ray fluorescence analysis results show that the lanthanum-magnesium modified sepiolite is prepared from SiO 2 、MgO、La 2 O 3 、CaO、Fe 2 O 3 、Al 2 O 3 And other trace elements, the mass contents of which are 37.5%, 40.5%, 7.33%, 10.4%, 1.2%, 2.1% and 0.97%, respectively; BET specific surface area analysis showed that the lanthanum magnesium modified sepiolite had a BET specific surface area of 81 m 2 Per gram, pore volume of 0.34. 0.34 cm 3 /g, pore size 27 nm.
TABLE 5 composition of natural sepiolite and lanthanum magnesium modified sepiolite ingredients and content thereof
| Component (%) | SiO 2 | MgO | La 2 O 3 | CaO | Fe 2 O 3 | Al 2 O 3 | Others |
| Natural sepiolite | 59.63 | 18.07 | – | 15.46 | 1.43 | 3.50 | 1.91 |
| Lanthanum-magnesium modified sepiolite | 37.5 | 40.5 | 7.33 | 10.4 | 1.2 | 2.1 | 0.97 |
TABLE 6 specific surface area, pore volume and pore size of natural sepiolite and lanthanum magnesium modified sepiolite
| Sample of | Specific surface area (m) 2 /g） | Pore volume (cm) 3 /g） | Average pore diameter (nm) |
| Natural sepiolite | 67.98 | 0.15 | 18.53 |
| Lanthanum-magnesium modified sepiolite | 81.32 | 0.34 | 27.21 |
Claims (1)
1. The application of the lanthanum-magnesium modified sepiolite is characterized in that: the lanthanum-magnesium modified sepiolite has a spherical granular structure and is prepared from SiO 2 、MgO、La 2 O 3 、CaO、Fe 2 O 3 、Al 2 O 3 And other trace elements, the mass contents of which are 37.5%, 40.5%, 7.33%, 10.4%, 1.2%, 2.1% and 0.97%, respectively, and the BET specific surface area is 81 m 2 Per gram, pore volume of 0.34. 0.34 cm 3 /g, pore size 27 nm;
the lanthanum-magnesium modified sepiolite is used for dephosphorizing black and odorous water bodies:
1) The lanthanum-magnesium modified sepiolite is put into an actual black and odorous water body 1 or an actual black and odorous water body 2 which are collected, the concentration of total phosphorus and orthophosphate in the black and odorous water body 1 is 0.68 mg/L and 0.59 mg/L respectively, and the pH value is 7.72; the concentrations of total phosphorus and orthophosphate in the black and odorous water body 2 are respectively 1.36 mg/L and 1.22 mg/L, and the pH value is 7.31; the adding amount of the lanthanum-magnesium modified sepiolite in the actual black and odorous water body 1 and the actual black and odorous water body 2 is respectively 0.1 g/L and 0.3 g/L, the total phosphorus and orthophosphate in the actual black and odorous water body 1 and the actual black and odorous water body 2 are subjected to oscillation dispersion at 25 ℃ and 200 rpm for 24 h, the concentrations of the lanthanum-magnesium modified sepiolite after being treated are not more than 0.1 mg/L, the treatment effect of the lanthanum-magnesium modified sepiolite reaches the surface water II type water quality standard GB 3838-2002, the lanthanum-magnesium modified sepiolite is superior to that of lanthanum-loaded modified sepiolite or magnesium-loaded modified sepiolite prepared by the same method, the mass ratio of lanthanum to sepiolite in the lanthanum-modified sepiolite is 0.3:1.0, and the mass ratio of magnesium to sepiolite in the magnesium-modified sepiolite is 0.3:1.0;
the lanthanum-magnesium modified sepiolite is prepared by the following method: la (NO) 3 ) 3 ·6H 2 O and MgCl 2 ·6H 2 Mixing O according to the mass ratio of lanthanum element and magnesium element of 1:5, controlling the mass concentration of lanthanum nitrate to be 1-2 g/L, adding ultrapure water, stirring and dissolving to avoid the interference of other ions, and obtaining a mixed solution of lanthanum nitrate and magnesium chloride; adding natural sepiolite into the mixed solution of lanthanum nitrate and magnesium chloride according to the mass ratio of the natural sepiolite to lanthanum element 1:0.05 in the mixed solution of lanthanum nitrate and magnesium chloride, and mixing and stirring at 25 ℃ to dissolve the natural sepiolite to obtain an intermediate reaction solution; adjusting the pH value of the intermediate reaction solution to 11-11.5 by using 1-5 mol/L sodium hydroxide solution, stirring for 4-6 hours, carrying out suction filtration, drying a filter cake at 55-75 ℃ for 8-16 hours, grinding, and sieving with 0.15-mm aperture to obtain the lanthanum-magnesium modified sepiolite for dephosphorization of black and odorous water bodies;
the natural sepiolite is prepared by grinding, sieving with 0.15-mm aperture, and has specific surface area of 68 m 2 /g, pore volume of 0.15 cm 3 /g, natural sepiolite with a pore size of 19 nm.
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