CN101386424A - method for preparing modification forming magnalium hydrotalcite and application - Google Patents
method for preparing modification forming magnalium hydrotalcite and application Download PDFInfo
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- CN101386424A CN101386424A CNA2008101577612A CN200810157761A CN101386424A CN 101386424 A CN101386424 A CN 101386424A CN A2008101577612 A CNA2008101577612 A CN A2008101577612A CN 200810157761 A CN200810157761 A CN 200810157761A CN 101386424 A CN101386424 A CN 101386424A
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- hydrotalcite
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Abstract
The invention discloses a preparation method of a modified and molded Mg-Al hydrotalcite and the application thereof. When in preparation, a mixed saline solution and a mixed aqueous alkali, containing Mg<2+> and Al<3+>, are respectively prepared and then mixed. Aging and crystallization are carried out after complete reaction, and the Mg-Al hydrotalcite is obtained after filtration, washing and drying; the Mg-Al hydrotalcite and a bonding agent are added into a magnesium saline solution and the pH value of the obtained paste is adjusted. After reaction, centrifugal separation, drying and extrusion molding are carried out, and then the paste is dried, roasted and cooled to the room temperature. When in adsorption and ion exchange, the product of the invention does not block a bed body and is easy for separation after reaction, suitable for the treatment of phosphorus and nitrogen anions in aqueous solution, water of a sewage disposal plant, seawater and breeding wastewater. A good treatment effect is available and an effluent standard can be met. Furthermore, after use, the product has better absorption effects after desorption and regeneration, thereby being beneficial to the realization of industrialized application.
Description
Technical field
The present invention relates to a kind of preparation method and application of magnesium aluminum-hydrotalcite of modification forming.
Background technology
The hydrotalcite that nature exists is the hydroxyl carbonated of magnesium, aluminium, is called magnesium aluminum-hydrotalcite again, and its theoretical molecular formula is Mg
6Al
2(OH)
16(CO
3) 4H
2O.Magnesium aluminum-hydrotalcite is a kind of anion type laminated compound, has unique negatively charged ion interchangeability, positively charged ion collocation property and bigger specific surface area, is occupying crucial status aspect absorption, ion-exchange and the catalysis.But at present to the research of magnesium aluminum-hydrotalcite with use and mainly be confined to powder morphology, exist suspended solid easily to stop up to be difficult to separate after a body, the reaction and can't realize deficiency such as regeneration, so magnesium aluminum-hydrotalcite is subjected to bigger restriction in actual applications.Therefore, realize the practical application of magnesium aluminum-hydrotalcite aspect absorption and ion-exchange, magnesium aluminum-hydrotalcite must be carried out effective modification forming, make it have certain mechanical strength.
Along with prominent the flying of industrial and agricultural production developed, a large amount of sanitary sewages, trade effluent and agrochemical flow into river, lake, and the phosphorus nitrogen content in the corresponding water body is increased, and excessive phosphorus nitrogen not only can cause body eutrophication, and meeting polluted underground water source, thereby HUMAN HEALTH is caused serious harm.But according to the latest report of Britain publication Freshwater Biology and U.S. publication PNAS, phosphorus is the deciding factor that causes eutrophication, and what play a role mainly is active phosphorus.At present, China municipal sewage plant more than 80% based on flocculation sediment and biological process, not good to the treatment effect of inorganic pollutants such as phosphorus nitrogen, want to reach the water quality emission standard, must pass through tertiary treatment.Therefore, effectively control and the advanced treatment that reduces the concentration of phosphorus nitrogen in the waste water and micropollutant water has become new problem in the modern sewage disposal, develop and develop efficient sewage water treatment method and have important practical significance.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method and application of magnesium aluminum-hydrotalcite of modification forming, it can remedy the above-mentioned deficiency of prior art.
A kind of preparation method of magnesium aluminum-hydrotalcite of modification forming is characterized in that step is as follows: preparation contains Mg respectively
2+, Al
3+The mixed-salt aqueous solution and the mixed base aqueous solution, with the two mixing, question response wears out and crystallization after fully, after filtration, washing, drying obtain magnesium aluminum-hydrotalcite; This magnesium aluminum-hydrotalcite and binding agent are joined in the magnesium salt solution, the gram number that makes three kinds of solid quality sums is 1:5～15 with the ratio of the volume milliliter number of liquid, the pH value of regulating the gained soup compound is 9～12, reaction 15～180min, centrifugation, oven dry, extrusion moulding, 100～110 ℃ of oven dry down,, be cooled to room temperature then 350～700 ℃ of following roastings 1～4 hour.
The magnesium aluminum-hydrotalcite of above-mentioned modification forming is the application in the phosphorus nitrogen negatively charged ion in removing the aqueous solution, sewage work's water, seawater or breeding wastewater.
The magnesium aluminum-hydrotalcite of modification forming of the present invention is a kind of efficient sorbent material, is not easy to separate after a body, reaction are not stopped up in absorption during with ion-exchange and can realizes regenerating; Can solve the not good problem of phosphorus nitrogen treatment effect in the present water body, be applicable to the phosphorus nitrogen negatively charged ion in treating water solution, sewage work's water, seawater, the breeding wastewater, make it to reach emission standard, and stronger through adsorption effect behind the desorption and regeneration, lay a good foundation for realizing industrial applications.
Embodiment
Embodiment 1
The preparation method of the magnesium aluminum-hydrotalcite of modification forming
MgSO with 3000mol
4Al with 500mol
2(SO
4)
3(total amount is 4.0m to be mixed with mixed-salt aqueous solution
3), with the NaOH of 5000mol and the Na of 10000mol
2CO
3(total amount is 4.0m to be made into the mixed base aqueous solution
3), two kinds of aqueous solution are added complete mixing in the injection reactor by pipeline, control pH value is reacted under 8～9 condition, obtain oyster white pulpous state thing, directly add in the digestion tank and ceaselessly stirring this soup compound, after question response was complete, the seal aging jar was heated to 130 ℃, and to keep temperature be (130 ± 5) ℃, crystallization 24 hours adds plate-and-frame filter press with the material after the crystallization then, washs to filtrate with tap water and can not detect sulfate radical, this moment, pH value of filtrate was 7, material after will washing at last carries out spraying drying, and makes the import of spray-drying tower and temperature out remain on 300 ℃ and 120 ℃ respectively, obtains the magnesium aluminum-hydrotalcite of unmodified moulding; This magnesium aluminum-hydrotalcite and binding agent water glass are joined Mg (Ac)
2In the aqueous solution, making three kinds of solid mass ratioes is 47.5:2.5:50, and the gram number of three kinds of solid masses sums is 1:10 with the ratio of the milliliter number of liquid volume, uses NH
3H
2The pH value that O regulates above-mentioned soup compound is 10, react centrifugation after 1 hour, dry that pinch to hand can be agglomerating, make the cylindrical sorbent material that diameter is 2mm with the shaping of catalyst machine, 110 ℃ of oven dry down, then 350 ℃ of following roastings 3 hours, be cooled to the magnesium aluminum-hydrotalcite that obtains modification forming after the room temperature, preserve stand-by.
Above-mentioned MgSO
4And Al
2(SO
4)
3In the Mg/Al mol ratio be 2～3:1; Magnesium salts in the described magnesium salt solution can be MgCl
2, Mg (NO
3)
2, MgSO
4, Mg (Ac)
2, MgC
2O
4, MgCO
3, in the magnesium basic carbonate one or more; Described binding agent is silicon sol and/or water glass; Described magnesium aluminum-hydrotalcite, binding agent and three kinds of solid quality of magnesium salts are 5～99:0～10:1～95 than scope.
Embodiment 2
Unmodified moulding and magnesium aluminum-hydrotalcite modification forming remove the PO in the aqueous solution respectively
4 3-, P
3O
10 5-, NO
3 -, NO
2 -
With unmodified moulding with embodiment 1 in the magnesium aluminum-hydrotalcite of the modification forming that makes be that 1.1:10 is respectively charged in the adsorption column by blade diameter length ratio, adsorb respectively and remove PO in the aqueous solution
4 3-, P
3O
10 5-, NO
3 -, NO
2 -, their starting point concentrations separately are 50mg/L respectively in phosphorus or nitrogen, control the flow of this aqueous solution by adsorption column and are 5mL/min.Respectively according to national sewage comprehensive emission standard primary standard, national Drinking Water source quality primary standard and groundwater quality standard, with the concentration of phosphorus in the absorption rear solution is that the concentration of 0.5mg/L, nitre nitrogen is that the concentration of 10mg/L, nitrite nitrogen is the permission emission concentration of 1.0mg/L as phosphorus or nitrogen, be breakthrough point concentration, it is as shown in table 1 to obtain penetrating adsorptive capacity.Control is 5mL/min by the flow of adsorption column, removes PO
4 3-, P
3O
10 5-And NO
2 -After the magnesium aluminum-hydrotalcite of modification forming (remove NO with the NaOH of 0.1mol/L and the NaCl mixing solutions desorb of 3mol/L
3 -The back is with the NaOH desorb of 0.2mol/L) phosphorus or nitrogen concentration are constant substantially to the effluent liquid, contain 75g MgCl with 300mL then
2Aqueous solution regeneration after, reusable, it is as shown in table 1 to penetrate adsorptive capacity.
The magnesium aluminum-hydrotalcite of unmodified moulding of table 1 and modification forming is to PO in the aqueous solution
4 3-, P
3O
10 5-, NO
3 -, NO
2 -Penetrate adsorptive capacity (mg/g)
With PO
4 3-Be example, the magnesium aluminum-hydrotalcite of modification forming is to PO
4 3-To penetrate adsorptive capacity be 13.49mg/g the first time, the magnesium aluminum-hydrotalcite that is unmodified moulding is to PO
4 3-Penetrate more than 6 times of adsorptive capacity, and through behind twice of the desorption and regeneration, to PO
4 3-The adsorptive capacity that penetrates be 17.03 and 13.23mg/g.But find out the PO in the magnesium aluminum-hydrotalcite effective elimination aqueous solution of modification forming thus
4 3-, reusable behind desorption and regeneration, removal effect is strengthened to some extent.
Embodiment 3
The magnesium aluminum-hydrotalcite of modification forming removes the PO in the aqueous solution simultaneously
4 3-, P
3O
10 5-, NO
3 -, NO
2 -Is that 1.1:15 packs in the adsorption column with the magnesium aluminum-hydrotalcite of the modification forming that makes among the embodiment 1 by blade diameter length ratio, removes the PO in the aqueous solution simultaneously
4 3-, P
3O
10 5-, NO
3 -, NO
2 -, their starting point concentrations separately are 25mg/L respectively in phosphorus or nitrogen, and the control aqueous solution is 5mL/min by the flow of adsorption column.Each ionic breakthrough concentration obtains PO as described in example 2 above
4 3-, P
3O
10 5-, NO
2 -Time of break-through be 95,75,75min, and NO
3 -In 300min, do not penetrate always.Find out that thus the magnesium aluminum-hydrotalcite behind the modification forming can remove the PO in the aqueous solution simultaneously
4 3-, P
3O
10 5-, NO
3 -, NO
2 -Owing to have the effect of intensive competitive adsorption between the various ions, make P
3O
10 5-And NO
2 -When 75min, at first penetrate adsorption column, but to PO
4 3-And NO
3 -Still have stronger adsorptive power,, several adsorption column series connection can be used, improve the service efficiency of adsorption column in order to make full use of adsorption column.
Embodiment 4
The magnesium aluminum-hydrotalcite of modification forming removes the PO in the waste water after sewage work's secondary treatment simultaneously
4 3-, NO
3 -
Is that 1.1:10 packs in the adsorption column with the magnesium aluminum-hydrotalcite of the modification forming that makes among the embodiment 1 by blade diameter length ratio, removes the PO in the waste water after sewage work's secondary treatment simultaneously
4 3-And NO
3 -, their starting point concentration is respectively in phosphorus or nitrogen, is respectively 4.61,2.97mg/L, and waste water is 5mL/min by the flow of adsorption column after the secondary treatment of control sewage work.Each ionic breakthrough point concentration obtains PO as described in example 2 above
4 3-, NO
3 -In 540min, do not penetrate always; Control is 5mL/min by the flow of adsorption column, the magnesium aluminum-hydrotalcite of the modification forming after the absorption with the NaCl mixing solutions of the NaOH of 0.1mol/L and 3mol/L separate be drawn in the effluent liquid phosphorus or nitrogen concentration constant substantially, contain 75g MgCl with 300mL then
2Aqueous solution regeneration after, to PO
4 3-Time of break-through be 450min, and NO
3 -In 540min, do not penetrate always.The magnesium aluminum-hydrotalcite that modification forming is described to sewage work's secondary treatment after PO in the waste water
4 3-And NO
3 -Have the ability that removes more by force, and reusable behind desorption and regeneration.
Embodiment 5
The magnesium aluminum-hydrotalcite of modification forming removes the PO in the seawater of different locations, Qingdao
4 3-
With the magnesium aluminum-hydrotalcite of the modification forming that makes among the embodiment 1 is that 1.1:10 packs in the adsorption column by blade diameter length ratio all, removes the PO in wheat island, good day of sunlight and the Olympic Sailing competition shoreline seawater respectively
4 3-, the starting point concentration in these three location seawater is respectively 1.818,1.10,0.526 μ mol/L in phosphorus, and the control seawater is 5mL/min by the flow of adsorption column.According to the seawater quality primary standard, be that 0.48 μ mol/L is as PO in the seawater with the concentration of adsorbing back phosphorus
4 3-Breakthrough point concentration, the PO of wheat island place wherein
4 3-The adsorptive capacity that penetrates be PO in good day and the Olympic Sailing competition shoreline seawater of 0.29 μ g/g, sunlight
4 3-In 5h, do not penetrate always.The PO of the magnesium aluminum-hydrotalcite of modification forming to lower concentration in the seawater in different locations, Qingdao is described
4 3-Has the ability that removes more by force.
Embodiment 6
The magnesium aluminum-hydrotalcite of modification forming removes the PO in the breeding wastewater
4 3-
With the magnesium aluminum-hydrotalcite behind the modification forming that makes among the embodiment 1 is that 1.1:10 packs in the adsorption column by blade diameter length ratio all, removes the PO in the breeding wastewater
4 3-, starting point concentration is 25mg/L, the flow of control breeding wastewater by adsorption column is 5mL/min, with the concentration of phosphorus in the breeding wastewater of absorption back be 0.5mg/L as breakthrough point concentration, obtaining penetrating adsorptive capacity is 17.35mg/g.The magnesium aluminum-hydrotalcite that modification forming is described is to the PO in the breeding wastewater
4 3-Has the ability that removes more by force.
Liquid is 3～7mL/min by the flow range of adsorption column in the foregoing description 2～6, and blade diameter length ratio is 1.1:5～15.Control is 5mL/min by the flow of adsorption column, the magnesium aluminum-hydrotalcite of the modification forming after the absorption with the NaCl mixing solutions of the NaOH of 0～0.5mol/L and 0～5mol/L separate be drawn in the effluent liquid phosphorus or nitrogen concentration constant substantially, contain 50～150g MgCl with 300mL then
2Aqueous solution regeneration back reusable, and regeneration back effect is strengthened.
Claims (5)
1. the preparation method of the magnesium aluminum-hydrotalcite of a modification forming is characterized in that step is as follows: prepare respectively and contain Mg
2+, Al
3+The mixed-salt aqueous solution and the mixed base aqueous solution, with the two mixing, question response wears out and crystallization after fully, after filtration, washing, drying obtain magnesium aluminum-hydrotalcite; This magnesium aluminum-hydrotalcite and binding agent are joined in the magnesium salt solution, the gram number that makes three kinds of solid quality sums is 1:5～15 with the ratio of the volume milliliter number of liquid, the pH value of regulating the gained soup compound is 9～12, reaction 15～180min, centrifugation, oven dry, extrusion moulding, 100～110 ℃ of oven dry down,, be cooled to room temperature then 350～700 ℃ of following roastings 1～4 hour.
2. the magnesium aluminum-hydrotalcite of the described modification forming of claim 1 application in the phosphorus nitrogen negatively charged ion in removing the aqueous solution, sewage work's water, seawater or breeding wastewater.
3. the preparation method of the magnesium aluminum-hydrotalcite of modification forming as claimed in claim 1 is characterized in that the magnesium salts in the described magnesium salt solution is MgCl
2, Mg (Ac)
2, Mg (NO
3)
2, MgSO
4In one or more.
4. the preparation method of the magnesium aluminum-hydrotalcite of modification forming as claimed in claim 1 is characterized in that described binding agent is silicon sol and/or water glass.
5. the preparation method of the magnesium aluminum-hydrotalcite of modification forming as claimed in claim 1 is characterized in that described magnesium aluminum-hydrotalcite, binding agent and three kinds of solid quality of magnesium salts are 5～99:0～10:1～95 than scope.
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|---|---|---|---|
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101577612A CN101386424B (en) | 2008-10-14 | 2008-10-14 | Method for preparing modification forming magnalium hydrotalcite and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101386424A true CN101386424A (en) | 2009-03-18 |
| CN101386424B CN101386424B (en) | 2011-02-02 |
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ID=40476131
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|---|---|---|---|
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