CN101381330B - Application of roasted product of magnesia-alumina hydrotalcite in adsorption treatment of naphthol green B - Google Patents
Application of roasted product of magnesia-alumina hydrotalcite in adsorption treatment of naphthol green B Download PDFInfo
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- CN101381330B CN101381330B CN2008101209254A CN200810120925A CN101381330B CN 101381330 B CN101381330 B CN 101381330B CN 2008101209254 A CN2008101209254 A CN 2008101209254A CN 200810120925 A CN200810120925 A CN 200810120925A CN 101381330 B CN101381330 B CN 101381330B
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- naphthol green
- roasting
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- application
- hydrotalcite
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- QBZIEGUIYWGBMY-FUZXWUMZSA-N (5Z)-5-hydroxyimino-6-oxonaphthalene-2-sulfonic acid iron Chemical compound [Fe].O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O.O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O.O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O QBZIEGUIYWGBMY-FUZXWUMZSA-N 0.000 title claims abstract description 54
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 46
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 46
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 38
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 230000008025 crystallization Effects 0.000 claims abstract description 4
- 229910001051 Magnalium Inorganic materials 0.000 claims description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000010009 beating Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 abstract description 20
- 239000000463 material Substances 0.000 abstract description 18
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 abstract 4
- 239000000243 solution Substances 0.000 description 26
- 239000000047 product Substances 0.000 description 21
- 239000011777 magnesium Substances 0.000 description 14
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 8
- 229910052749 magnesium Inorganic materials 0.000 description 8
- 230000000274 adsorptive effect Effects 0.000 description 7
- 238000011068 loading method Methods 0.000 description 7
- 238000009987 spinning Methods 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 150000001449 anionic compounds Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- -1 cation ion Chemical class 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002790 naphthalenes Chemical class 0.000 description 1
- 150000002891 organic anions Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
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- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides application of binary magnesium-aluminum hydrotalcite in absorption treatment of naphthol green B in a water body. A roasted product obtained by roasting the binary magnesium-aluminum hydrotalcite for 4 to 7 hours at a temperature of between 400 and 600 DEG C is used for adsorbing the naphthol green B in the water body, a general formula of the binary magnesium-aluminum hydrotalcite is [Mg<2+>(1-x)Al<3+>x(OH)2](CO2<2->)x/2.mH2O, wherein in the formula, x is the ratio of the amount of Al<3+> to Mg<2+>+Al<3+> and is more than 0.2 and less than 0.4, and m is the number of crystallization water. The application has the advantages that the roasted product of the binary magnesium-aluminum hydrotalcite is used for adsorbing the naphthol green B in wastewater solution, has high adsorption capacity and quick adsorption rate; and a material after the adsorption is easy to recover and reutilize.
Description
(1) technical field
The present invention relates to the application of product of roasting in the adsorption treatment naphthol green B of magnalium binary hydrotalcite.
(2) background technology
Dyestuffs industries is to produce the more industry of sewage in the chemical industry, and the waste water of discharging is to be difficult to effective problem that solves always in production and the use.Characteristics such as waste water from dyestuff has high COD, high chroma, organic composition is complicated, chemical property is stable, the microbiological deterioration degree is low adopt flocculation and biological oxidation process often can not reach satisfied effect.Naphthol green B is used for the dyeing of wool and some chemical & blended fabrics more as a kind of organic dye commonly used.Naphthol green B has good water-solubility, and the naphthalene nucleus in the molecule is more stable group, is difficult for oxidized degraded.Therefore, naphthol green B is considered to a kind of organism of difficult degradation of solubility.
Absorption method is as efficient sepn process, in the solute of solution separates, demonstrates significant meliority, is suitable for removing of naphthol green B in the waste water.But some natural sorbing materials are generally on the low side to the loading capacity of naphthol green B, so the efficient sorbing material of synthetic becomes the focus of present material and environment remediation research.
Hydrotalcite-based compound (Layered Double Hydroxides is called for short LDHs) is made up of the layers of metal hydroxides plate and the tradable interlayer anion of positively charged, and its chemical general formula is: [M
2+ (1-x)M
3+ x(OH)
2] (A
N-)
X/nMH
2O, wherein M
2+=Mg
2+, Ni
2+, Co
2+, Zn
2+, Cu
2+Deng divalent-metal ion; M
3+=Al
3+, Cr
3+, Fe
3+, Sc
3+Deng trivalent metal ion; X is M
3+/ M
2+Mol ratio, usually between 0.2~0.33; A
N-Be intercalant anion, as: CO
3 2-, NO
3 -, Cl
-, OH
-, SO
4 2-, PO
4 3-, C
6H
4(COO
-)
2Etc. inorganic and organic anion; M is the crystal water number.Hydrotalcite-based compound has bigger specific surface through roasting, has the particular structural memory effect simultaneously, makes it for the processing of negatively charged ion waste water application promise in clinical practice arranged.
There is the product of roasting of binary hydrotalcite to be used for the anionic introduction (CN1962046A) of adsorbing the heavy metal cation ion of waste water and containing heavy metal in the existing technology, do not see that also the product of roasting that the magnalium binary hydrotalcite is arranged is used for the report of adsorption treatment water body naphthol green B at present.
(3) summary of the invention
Low and cause shortcomings such as secondary pollution easily in order to overcome in the present technology naphthol green B processing efficiency, the invention provides the application in the naphthol green B in the adsorption treatment water body of magnalium binary hydrotalcite.
The technical scheme that the present invention adopts is:
The application of the product of roasting of magnalium binary hydrotalcite in the adsorption treatment naphthol green B; Said application is the naphthol green B that is used for adsorbed water body with the product of roasting that the magnalium binary hydrotalcite obtains in 400~600 ℃ of following roasting 4~7h, and said magnalium binary hydrotalcite general formula is: [Mg<sup >2+</sup><sub >(1-x)</sub>Al<sup >3+</sup><sub >x</sub>(OH)<sub >2</sub>] (CO<sub >2</sub><sup >2-</sup>)<sub >X/2</sub>MH<sub >2</sub>O, in the formula: x is Al<sup >3+</sup>/ (Mg<sup >2+</sup>+ Al<sup >3+</sup>) the ratio of amount of substance, 0.2<x<0.4 m is the crystal water number, usually between 2~6, for the MgAl amount of substance than the magnalium binary hydrotalcite that is 3, its m=4.
Preferably, said magnalium binary hydrotalcite general formula is: [Mg
2+ 0.75Al
3+ 0.25(OH)
2] (CO
2 2-)
0.1254H
2O.
Concrete, said being applied as: the product of roasting input of said magnalium binary hydrotalcite is contained in the water body of naphthol green B, and regulating water body pH is 8~12, under 40~65 ℃, carries out adsorption treatment 1~5h and removes the naphthol green B in the water body; The product of roasting quality consumption of said magnalium binary hydrotalcite is 4~10 times of naphthol green B quality in the water body.
In the treating processes, adopt the water bath with thermostatic control temperature control, with the pH value of the HCl regulator solution of the NaOH of 0.01mol/L and 0.01mol/L.
Said magnalium binary hydrotalcite can adopt ordinary method to obtain, and the present invention adopts two coprecipitation methods of dripping, and is specific as follows: Mg in forming according to the magnalium binary hydrotalcite
2+, Al
3+, OH
-And CO
2 2-The amount of substance proportioning is with Mg (NO
3)
26H
2O and Al (NO
3)
39H
2O is mixed with solution A, NaOH and Na
2CO
3Be mixed with solution B; Then solution A and solution B are dropped in the deionized water in stirring down simultaneously, constant temperature keeps pH of mixed between 8~10 down for 30 ℃, dropwises and continues to stir 0.5~2h; In 50~100 ℃ of crystallization 10~25h; Centrifugal, the making beating washing is to neutral, and 50~100 ℃ of drying 10~25h make said magnalium binary hydrotalcite.
In pending naphthol green B waste liquid, add a certain amount of magnalium binary hydrotalcite product of roasting, behind the stirring certain hour, get the mixed solution spinning, get the concentration that supernatant is analyzed naphthol green B.
The mensuration of naphthol green B concentration adopts visible spectrophotometry.
Material calculates with formula (1) the adsorptive capacity Q of naphthol green B in the solution, promptly
Q=(C
0-C
t)V/M (1)
Material calculates with formula (2) the clearance η of naphthol green B in the solution, promptly
η=C
t/C
0 (2)
Wherein, C
0And C
tBe respectively initial and the concentration of handling back solution naphthol green B, V is the volume of solution, and M is the quality of sorbent material.
The magnalium binary hydrotalcite product of roasting that is adopted among the present invention has very high loading capacity to the naphthol green B in the water body; When under following condition, adsorbing, loading capacity can reach 194mg/g, obviously is superior to general sorbing material: the quality of the sorbing material of input is 100mg; The concentration of handling naphthol green B is 200mg/L solution 100ml; Control pH value of solution value is 10, and temperature is 45 ℃, and adsorption time is 2h.
Sorbing material behind the absorption naphthol green B can be regenerated by roasting 2~5h in 300~500 ℃ of retort furnaces, and desorption efficient still can reach 96%.
Beneficial effect of the present invention is mainly reflected in: be used for adsorbing the naphthol green B of waste water solution with the product of roasting of magnalium binary hydrotalcite, loading capacity is high, and adsorption rate is fast, and the material easy recovery after the absorption is utilized.
(4) description of drawings
Fig. 1 is the graph of a relation of loading capacity and adsorption time among the embodiment 1~8.
Fig. 2 is the graph of a relation of loading capacity and pH among the embodiment 9~13.
Fig. 3 is the graph of a relation of loading capacity and temperature among the embodiment 14~19.
Fig. 4 is the graph of a relation of clearance and hydrotalcite calcining matter addition among the embodiment 20~24.
(5) embodiment
Below in conjunction with specific embodiment the present invention is described further, but protection scope of the present invention is not limited in this:
The product of roasting preparation of magnalium binary hydrotalcite:
With 0.15molMg (NO
3)
26H
2O150mL and 0.05molAl (NO
3)
39H
2O 150mL is mixed with solution A, with 0.4molNaOH 150mL and 0.025molNa
2CO
3150mL is mixed with solution B, then solution A and solution B is added drop-wise to respectively in the deionized water of 100mL, keeps 2 droplets/second rate of addition; 30 ℃ of constant temperature, violent stirring keeps pH between 8~10; Dropwise and continue to stir 2h, in 55 ℃ of crystallization 20h, centrifugal; The making beating washing is to neutral, and 80 ℃ of dry 18h make the magnalium binary hydrotalcite.
The above-mentioned magnalium binary hydrotalcite that makes obtains corresponding product of roasting at 500 ℃ of following roasting 5h.
Embodiment 1~8:
Prepare 8 parts of waste water that naphthol green B concentration is the 100ml of 200mg/L; Take by weighing the magnesium aluminum-hydrotalcite product of roasting of 8 parts of 100mg; Add respectively in pending the containing waste water that naphthol green B concentration is 200mg/L; HCl control pH value with the NaOH of 0.01mol/L and 0.01mol/L is 10, and temperature is 45 ℃, and churning time is respectively 20,40,60,80,100,120,140,160min.After the stirring, spinning is got supernatant and is measured adsorbed solution concentration, material to the adsorptive capacity of naphthol green B over time situation see Fig. 1.
Conclusion: at 100ml, concentration is in the naphthol green B waste water solution of 200mg/L, adds 100mg magnesium aluminum-hydrotalcite product of roasting, is 10 in the pH value, and temperature is under 45 ℃ the condition, behind 100min, to reach adsorption equilibrium.
Embodiment 9~13:
Prepare 5 parts of 100ml waste water that naphthol green B concentration is 200mg/L, take by weighing the magnesium aluminum-hydrotalcite product of roasting of 5 parts of 100mg, adding pending concentration respectively is in the naphthol green B waste water of 100mg/L; Controlled temperature is 45 ℃; Be respectively 4,6,8,10,12 with the NaOH of 0.01mol/L and the HCl adjusting pH of 0.01mol/L, churning time is 120min, after the stirring; Spinning is got supernatant and is measured adsorbed solution concentration.Material is seen Fig. 2 to the adsorptive capacity of naphthol green B with the changing conditions of pH.
Conclusion: in the concentration of 100ml is the naphthol green B waste water solution of 200mg/L, add 100mg magnesium aluminum-hydrotalcite product of roasting, temperature is 45 ℃, under different pH conditions, adsorbs, and when pH=10, adsorptive capacity is maximum, can reach 194mg/g.
Prepare six parts of waste water 100ml that naphthol green B concentration is 200mg/L; Take by weighing the magnesium aluminum-hydrotalcite product of roasting of six parts of 100mg; Adding pending concentration respectively is in the naphthol green B waste water of 100mg/L; With the NaOH of 0.01mol/L and the HCl control pH=10 of 0.01mol/L, temperature is respectively 25,35,45,55,65,75 ℃.After the stirring, churning time is 120min, and spinning is got supernatant and measured adsorbed solution concentration, obtains material the adsorptive capacity of naphthol green B is seen Fig. 3 with the variation of temperature situation.
Conclusion: in the concentration of 100ml is the naphthol green B waste water solution of 200mg/L, add 100mg magnesium aluminum-hydrotalcite product of roasting, pH=10 adsorbs under differing temps, and when temperature was 45 ℃, adsorptive capacity was maximum, can reach 194mg/g.
Prepare five parts of 100ml waste water that naphthol green B concentration is 200mg/L; Take by weighing 50,75,100,150, the magnesium aluminum-hydrotalcite product of roasting of 200mg; Adding pending concentration respectively is in the naphthol green B waste water of 200mg/L; With the NaOH of 0.01mol/L and the HCl control pH=10 of 0.01mol/L, temperature is respectively 45 ℃, and churning time is 120min.After the stirring, spinning is got supernatant and is measured adsorbed solution concentration, obtains material the clearance of naphthol green B is seen Fig. 4.
Conclusion: in the concentration of 100ml is the naphthol green B waste water solution of 200mg/L, add different mass magnesium aluminum-hydrotalcite product of roasting; PH=10; Temperature is under 45 ℃ the condition naphthol green B to be adsorbed, and clearance had reached and has been up to 97% when addition reached 100mg.
Embodiment 25:
Sorbing material behind the absorption naphthol green B is carried out thermogravimetric analysis; Obtain required maturing temperature, the material after the absorption at 500 ℃ of following roasting 5h, is taken by weighing the material 100mg after the recovery; Add in the naphthol green B waste water that pending concentration is 200ml/L; With the NaOH of 0.01mol/L and the HCl control pH=10 of 0.01mol/L, temperature is 45 ℃, and churning time is 120min.After the stirring, spinning is got supernatant and is measured adsorbed solution concentration, obtain material to the adsorptive capacity of naphthol green B still up to 184mg/g.
Claims (5)
1. the application of the product of roasting of magnalium binary hydrotalcite in the adsorption treatment naphthol green B; Said application is the naphthol green B that is used for adsorbed water body with the product of roasting that the magnalium binary hydrotalcite obtains in 400~600 ℃ of following roasting 4~7h, and said magnalium binary hydrotalcite general formula is: [Mg
2+ (1-x)Al
3+ x(OH)
2] (CO
3 2-)
X/2MH
2O, in the formula: x is Al
3+/ (Mg
2++ Al
3+) the ratio of amount of substance, 0.2<x<0.4, m is the crystal water number, 2≤m≤6.
2. application as claimed in claim 1 is characterized in that said magnalium binary hydrotalcite general formula is:
[Mg
2+ 0.75Al
3+ 0.25(OH)
2](CO
3 2-)
0.125·4H
2O。
3. according to claim 1 or claim 2 application; It is characterized in that said being applied as: the product of roasting input of said magnalium binary hydrotalcite is contained in the water body of naphthol green B; Regulating water body pH is 8~12, under 40~65 ℃, carries out adsorption treatment 1~5h and removes the naphthol green B in the water body; The product of roasting quality consumption of said magnalium binary hydrotalcite is 4~10 times of naphthol green B quality in the water body.
4. application as claimed in claim 3 is characterized in that in the adsorption treatment process pH value of regulating water body with the HCl solution of the NaOH solution of 0.01mol/L and 0.01mol/L.
5. according to claim 1 or claim 2 application is characterized in that said magnalium binary hydrotalcite is prepared by following method: Mg in forming according to the magnalium binary hydrotalcite
2+, Al
3+, OH
-And CO
3 2-The amount of substance proportioning is with Mg (NO
3)
26H
2O and Al (NO
3)
39H
2O is mixed with solution A, NaOH and Na
2CO
3Be mixed with solution B; Then solution A and solution B are dropped in the deionized water in stirring down simultaneously, constant temperature is controlled drop rate down for 30 ℃ and is kept pH of mixed between 8~10, dropwises and continues to stir 0.5~2h; In 50~100 ℃ of crystallization 10~25h; Centrifugal, the making beating washing is to neutral, and 50~100 ℃ of drying 10~25h make said magnalium binary hydrotalcite.
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CN102173440B (en) * | 2010-12-31 | 2013-07-31 | 浙江工业大学 | Magnesium/aluminium (Mg/Al) binary hydrotalcite and application thereof in treatment of chemical wastewater |
CN102424448A (en) * | 2011-11-01 | 2012-04-25 | 同济大学 | Method for removing perchlorate in water |
CN102502912A (en) * | 2011-11-03 | 2012-06-20 | 同济大学 | Method for removing halogen family oxysalt from water |
CN114082395A (en) * | 2020-08-25 | 2022-02-25 | 大连佳纯气体净化技术开发有限公司 | Mercaptan removal adsorbent and preparation method and application thereof |
CN113457212A (en) * | 2021-06-25 | 2021-10-01 | 中触媒新材料股份有限公司 | Preparation and use method of trapping agent for simultaneously improving purity and chromaticity of m-methylphenol |
Citations (3)
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---|---|---|---|---|
CN1142811A (en) * | 1993-12-23 | 1997-02-12 | 克罗斯菲尔德有限公司 | Effluent treatment with hydrotalcite |
CN1683071A (en) * | 2005-02-06 | 2005-10-19 | 浙江工业大学 | Use of zinc-magnesium-aluminium ternary hydrotalcite as nitrogen oxide adsorbent |
CN1962046A (en) * | 2006-10-20 | 2007-05-16 | 山东大学 | A heavy metal ion absorbent and application thereof in removal of heavy metal ion |
-
2008
- 2008-09-05 CN CN2008101209254A patent/CN101381330B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1142811A (en) * | 1993-12-23 | 1997-02-12 | 克罗斯菲尔德有限公司 | Effluent treatment with hydrotalcite |
CN1683071A (en) * | 2005-02-06 | 2005-10-19 | 浙江工业大学 | Use of zinc-magnesium-aluminium ternary hydrotalcite as nitrogen oxide adsorbent |
CN1962046A (en) * | 2006-10-20 | 2007-05-16 | 山东大学 | A heavy metal ion absorbent and application thereof in removal of heavy metal ion |
Non-Patent Citations (1)
Title |
---|
俞卫华等.镁铝水滑石的制备和脱硝性能的研究.《科技通报》.2003,第19卷(第4期),330-333. * |
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