CN101703917A - Magnetic nano hydroxyapatite adsorbent, preparation and application thereof - Google Patents
Magnetic nano hydroxyapatite adsorbent, preparation and application thereof Download PDFInfo
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- CN101703917A CN101703917A CN200910310387A CN200910310387A CN101703917A CN 101703917 A CN101703917 A CN 101703917A CN 200910310387 A CN200910310387 A CN 200910310387A CN 200910310387 A CN200910310387 A CN 200910310387A CN 101703917 A CN101703917 A CN 101703917A
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Abstract
The invention discloses a magnetic nano hydroxyapatite adsorbent, preparation and application thereof. Nano hydroxyapatite Ca10(PO4)6(OH)2 is used as a matrix of the adsorbent, and magnetic powder Fe3O3 is uniformly dispersed in the matrix, wherein the mass ratio of the nano hydroxyapatite to the magnetic powder Fe3O3 is (1.5-1):1. The preparation method comprises the following steps of: dissolving FeCl2 and FeCl3 with a mass ratio of (0.75-0.85):1 in deoxidized water; then adding an ammonia solution and uniformly stirring; simultaneously adding a Ca(NO3)2 solution and a (NH4)2HPO4 solution and uniformly stirring to obtain liliquoid; heating the liliquoid at the temperature of 90-100 DEG C; and then obtaining the magnetic nano hydroxyapatite adsorbent through cooling, separating, washing, drying and grinding. The magnetic nano hydroxyapatite adsorbent has large specific surface area, high adsorption efficiency, low cost and easy separation and can effectively remove heavy metal ions in waste water.
Description
Technical field
The present invention relates to a kind of inorganic material adsorbent and preparation and application, relate in particular to a kind of adsorbent and preparation and application that mainly constitutes by apatite.
Background technology
Heavy metal pollution is mainly from mining industry, metallurgy, machining, surface treatment and heavy industry etc.The method of removing the middle heavy metal ion of anhydrating is a lot, traditional method has chemical precipitation method, oxidation-reduction method, ferrite process, electrolysis, evaporation concentration method, ion-exchange-resin process etc., but these methods existence investments are big, operating cost is high, operational administrative is loaded down with trivial details and cause secondary pollution problems easily, can not effectively realize the utilization again of heavy metal and water resource simultaneously.At present, more in the practice is to adopt absorption method, and absorption method is because of its material cheaply is easy to get, cost is low, the good favor that is subjected to people of removal effect always.The adsorbent of removal heavy metal commonly used mainly contains active carbon, mesoporous material, clay, zeolite, shitosan and apatite etc., yet these adsorbents all exist shortcoming such as not easily separated after the little or absorption of adsorption capacity, therefore must strive to find new promising adsorbent.
Utilize inorganic material natural or that synthesize to become the research field of a hot topic as adsorbent in recent years, its main cause be between inorganic adsorbent and adsorbate active force a little less than, and inorganic adsorbent has great heat endurance, thereby makes that the regeneration of inorganic adsorbent is fairly simple.Yet, because traditional inorganic adsorbent specific area is little, so adsorption capacity is lower.
Nano material has great specific area, so the nano material that is formed by inorganic matter has become one of widely used adsorbent.As a kind of nano material absorbent of being made up of inorganic matter, it has higher biocompatibility and absorption property to nanometer hydroxyapatite (being called for short HAP), and has been widely used in the removal of heavy metal ion.At present, in the majority with the compound and the nanometer hydroxyapatite of research hydroxyapatite, hydroxyapatite both at home and abroad as the relevant report of adsorbent, but as the nano hydroxyapatite adsorbent of adsorption treatment heavy metal ion, its performance and effect also have the space of further improving and promoting.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, provide that a kind of specific area is big, adsorption efficiency is high, cost is low, the segregative magnetic nano hydroxyapatite adsorbent that magnetic separation technique is combined with adsorption process, preparation method and application with this adsorbent magnetic nano hydroxyapatite adsorbent that match, with low cost and simple to operate also are provided simultaneously.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is a kind of magnetic nano hydroxyapatite adsorbent, it is characterized in that: described adsorbent is to be matrix with the nanometer hydroxyapatite, evenly is dispersed with Magnaglo Fe in the matrix
2O
3, the molecular formula of described nanometer hydroxyapatite is Ca
10(PO
4)
6(OH)
2, described nanometer hydroxyapatite and described Magnaglo Fe
2O
3Mass ratio be (1.5～1): 1.
As a total technical conceive, the present invention also provides a kind of preparation method of magnetic nano hydroxyapatite adsorbent, and its operating procedure is as follows: under room temperature and inert gas shielding, be (0.75～0.85) with mass ratio: 1 FeCl
2And FeCl
3(also can be the crystalline hydrate of frerrous chloride and iron chloride, for example FeCl
24H
2O, FeCl
36H
2O etc.) be dissolved in the deoxidized water, in this solution, add ammonia spirit (concentration of ammonia spirit is preferably 25%～28% in known scope) then and stir and obtain precipitated liquid, will distinguish the Ca (NO behind the adjust pH again
3)
2Solution and (NH
4)
2HPO
4Solution joins in the described precipitated liquid simultaneously, wherein Ca (NO
3)
2With FeCl
2Mol ratio satisfy (18～18.5): 1, (NH
4)
2HPO
4With FeCl
2Mol ratio satisfy (10～11): 1, get liliquoid after stirring, this liliquoid is heated under 90 ℃～100 ℃ temperature (in known scope, be preferably 2h～3h) heat time heating time, cool to room temperature is also aging then, the sediment of gained of will wearing out at last separates, spend deionised water to neutral, obtain magnetic nano hydroxyapatite adsorbent after drying, the grinding.
Among the above-mentioned preparation method, the Ca (NO behind the described adjust pH
3)
2Solution, (NH
4)
2HPO
4The pH value of solution all preferably is controlled at 10～11.
As a total technical conceive, the present invention also provides a kind of application of magnetic nano hydroxyapatite adsorbent, it is characterized in that: with the heavy metal ion in the described adsorbent removal waste water, described heavy metal comprises one or more in copper, lead, zinc, cobalt, nickel, manganese, cadmium, mercury, tungsten, the molybdenum, and described adsorbent consumption in waste water is 0.1g/L～0.2g/L.
In the above-mentioned application, the pH value when described adsorbent carries out adsorption treatment in waste water preferably is controlled at 5～8, and the time of adsorption treatment preferably is controlled at 12h～24h.
Compared with prior art, the invention has the advantages that: magnetic nano hydroxyapatite adsorbent provided by the invention is a kind of new adsorbent that magnetic separation technique is combined with adsorption process, not only have the characteristics that the nano particle specific area is big, surface atom easily combines with other atom, ion, and because synthetic nano particle has magnetic, thereby be easy to from pending solution, separate.Magnetic nano hydroxyapatite among the present invention is compared with adsorbents such as active carbon, zeolite, clay, shitosans, and not only specific area is bigger, and adsorption efficiency is higher, and preparation is simple, with low cost, is easy to separate from solution and recycle.Match with magnetic nano hydroxyapatite adsorbent of the present invention, the present invention also provides this magnetic nano hydroxyapatite adsorbent corresponding preparation method and using method, this method is not only simple to operate, with low cost, and can effectively realize the suitability for industrialized production of this magnetic nano hydroxyapatite adsorbent, realize its effective absorption and processing to heavy metal ions in wastewater, adopt magnetic nano hydroxyapatite adsorbent of the present invention basicly stable more than 75% to removal rate of heavy metal in the waste water, reach as high as 95%, will obviously be better than existing nano hydroxyapatite adsorbent, this improvement for heavy metal pollution in the future waste water provides new approach.
Description of drawings
Fig. 1 is the sem photograph of magnetic nano hydroxyapatite adsorbent in the embodiment of the invention 1;
Fig. 2 is the X ray energy dispersion analysis (EDA) figure of magnetic nano hydroxyapatite adsorbent in the embodiment of the invention 1;
Fig. 3 is the magnetization curve figure of magnetic nano hydroxyapatite adsorbent in the embodiment of the invention 1.
The specific embodiment
Embodiment 1:
A kind of magnetic nano hydroxyapatite adsorbent, this adsorbent are to be matrix with the nanometer hydroxyapatite, evenly are dispersed with Magnaglo Fe in the matrix
2O
3, the molecular formula of nanometer hydroxyapatite is Ca
10(PO
4)
6(OH)
2, nanometer hydroxyapatite and Magnaglo Fe
2O
3Mass ratio be about 1.36, i.e. Magnaglo Fe
2O
3Mass fraction in this adsorbent is about 42.4%.
The preparation method of the magnetic nano hydroxyapatite adsorbent that present embodiment is above-mentioned is as follows:
In room temperature and feed under the atmosphere of nitrogen, with the FeCl of 1.85mmoL
24H
2The FeCl of O and 3.7mmoL
36H
2O is dissolved in the deoxidized water of 30mL, adds 25% ammonia spirit 10mL then and carry out mechanical agitation 15min in this solution, obtains precipitated liquid after stirring, and the pH value is transferred to the Ca (NO of 11 50mL respectively again
3)
2(the NH of (containing solute 33.67mmol) and 50mL
4)
2HPO
4(containing solute 20mmol) solution dropwise joins in this precipitated liquid simultaneously and carries out mechanical agitation, get the dark brown liliquoid after stirring, this liliquoid is heated 2h under 90 ℃ of temperature, cool to room temperature and aging 12h～24h then, the sediment of gained of will wearing out at last separates with magnet, spend deionised water again to neutral, the product after the washing is placed baking oven dry 4h under 90 ℃ of temperature, after cooling, grind and obtain finished product.Can judge tentatively that from the physical behavior and the chemical reaction basic principle of finished product finished product is a magnetic nano hydroxyapatite adsorbent.
With the surface topography that the above-mentioned finished product that makes places 10000 times ESEM to observe down this finished product, its sem photograph as shown in Figure 1, this finished surface is loose porous as can be seen from Figure 1, and huge specific area is arranged.Again by this finished product of X ray energy dispersion analysis (EDA), its analysis result as shown in Figure 2, mainly contain Ca, P, Fe and four kinds of elements of O as seen from Figure 2 in this finished product (because the content of protium is less, so the intensity of absworption peak a little less than, so do not make sign), Ca element wherein also can carry out ion-exchange with heavy metal ion, these character and characteristics have proved further that all this finished product belongs to a kind of nano hydroxyapatite adsorbent, make the absorption of this ABSORBENTS ABSORPTION metal ion become possibility.Again this finished product is carried out magnetization test, from the test after magnetization curve figure (as shown in Figure 3) as can be seen, this nano hydroxyapatite adsorbent has stronger magnetic, and outward appearance is sepia, and this explanation is dispersed with Magnaglo Fe in this nano hydroxyapatite adsorbent
2O
3, belong to magnetic nano hydroxyapatite adsorbent of the present invention, therefore can make it be easy to from solution, separate by magnet.
Embodiment 2:
The magnetic nano hydroxyapatite adsorbent of the present invention that makes among the embodiment 1 is added to the Cd that contains of each 20mL respectively
2+, Zn
2+Waste water in (initial concentration of every kind of heavy metal ions in wastewater is shown in Table 1), the consumption of this adsorbent is 0.1g/L in every kind of waste water, regulate pH value to 5.0 ± 0.1, at room temperature utilize the absorption of vibrating of constant temperature water bath oscillator, with magnet this adsorbent is separated from above-mentioned waste water behind the 24h, and measured the Cd that is not adsorbed in the waste water with atomic absorption spectrophotometry
2+, Zn
2+Content, measurement result is as shown in table 1 below.
Table 1: the content of heavy metal ions in wastewater before and after handling
| Heavy metal ions in wastewater | Initial concentration (mg/L) | Residual concentration (mg/L) | Clearance |
| ??Cd 2+ | ??220.93 | ??17.02 | ??92.3％ |
| ??Zn 2+ | ??126.75 | ??12.67 | ??90.0％ |
Embodiment 3:
Add the magnetic nano hydroxyapatite adsorbent of the present invention that makes among the embodiment 1 to 20mL and contain Cd
2+And Zn
2+In the waste water of two heavy metal species ions (initial concentration of each heavy metal ion is shown in Table 2 in the waste water), the consumption of adsorbent is 0.1g/L, regulate pH value to 5.0 ± 0.1, at room temperature utilize the absorption of vibrating of constant temperature water bath oscillator, with magnet this adsorbent is separated from above-mentioned waste water behind the 24h, and measured the Cd that is not adsorbed in the waste water with atomic absorption spectrophotometry
2+, Zn
2+Content.Listed in the table 2 and utilized magnetic nano hydroxyapatite adsorbent to handle simultaneously to contain Cd
2+And Zn
2+Waste water the time removal effect.
Table 2: the content of heavy metal ions in wastewater before and after handling
| Heavy metal ions in wastewater | Initial concentration (mg/L) | Residual concentration (mg/L) | Clearance |
| ??Cd 2+ | ??223.75 | ??37.1 | ??83.4％ |
| ??Zn 2+ | ??128 | ??23.56 | ??81.6％ |
Embodiment 4:
The magnetic nano hydroxyapatite adsorbent of the present invention that makes among the embodiment 1 is added to the Cd that contains of each 20mL respectively
2+, Zn
2+Waste water in (initial concentration of every kind of heavy metal ions in wastewater is shown in Table 3), the consumption of adsorbent is 0.1g/L, regulate pH value to 8.0 ± 0.1, at room temperature utilize the absorption of vibrating of constant temperature water bath oscillator, with magnet this adsorbent is separated from above-mentioned waste water behind the 24h, and measured the Cd that is not adsorbed in the waste water with atomic absorption spectrophotometry
2+, Zn
2+Content.Listed in the table 3 and when pH=8, utilized the magnetic nano hydroxyapatite adsorbent processing to contain Cd
2+With contain Zn
2+Removal effect during waste water.
Table 3: the content of heavy metal ions in wastewater before and after handling
| Heavy metal ions in wastewater | Initial concentration (mg/L) | Residual concentration (mg/L) | Clearance |
| ??Cd 2+ | ??223.75 | ??12.53 | ??94.4％ |
| ??Zn 2+ | ??128 | ??11.14 | ??91.3％ |
Embodiment 5:
The magnetic nano hydroxyapatite adsorbent of the present invention that makes among the embodiment 1 is added to the Cd that contains of each 20mL respectively
2+, Zn
2+Waste water in (initial concentration of every kind of heavy metal ions in wastewater is shown in Table 4), the consumption of adsorbent is 0.2g/L, regulate pH value to 5.0 ± 0.1, at room temperature utilize the absorption of vibrating of constant temperature water bath oscillator, with magnet this adsorbent is separated from above-mentioned waste water behind the 24h, and measured the Cd that is not adsorbed in the waste water with atomic absorption spectrophotometry
2+, Zn
2+Content.Utilize magnetic nano hydroxyapatite adsorbent to handle when having listed consumption at adsorbent in the table 4 and contain Cd for 0.2g/L
2+And Zn
2+Removal effect during waste water.
Table 4: the content of heavy metal ions in wastewater before and after handling
| Heavy metal ions in wastewater | Initial concentration (mg/L) | Residual concentration (mg/L) | Clearance |
| ??Cd 2+ | ??220.93 | ??8.33 | ??96.2％ |
| ??Zn 2+ | ??126.75 | ??8.12 | ??93.6％ |
Claims (7)
1. magnetic nano hydroxyapatite adsorbent is characterized in that: described adsorbent is to be matrix with the nanometer hydroxyapatite, evenly is dispersed with Magnaglo Fe in the matrix
2O
3, the molecular formula of described nanometer hydroxyapatite is Ca
10(PO
4)
6(OH)
2, described nanometer hydroxyapatite and described Magnaglo Fe
2O
3Mass ratio be (1.5～1): 1.
2. the preparation method of a magnetic nano hydroxyapatite adsorbent, its operating procedure is as follows: under room temperature and inert gas shielding, be (0.75～0.85) with mass ratio: 1 FeCl
2And FeCl
3Be dissolved in the deoxidized water, in this solution, add ammonia spirit then and stir and obtain precipitated liquid, will distinguish the Ca (NO behind the adjust pH again
3)
2Solution and (NH
4)
2HPO
4Solution joins in the described precipitated liquid simultaneously, wherein Ca (NO
3)
2With FeCl
2Mol ratio satisfy (18～18.5): 1, (NH
4)
2HPO
4With FeCl
2Mol ratio satisfy (10～11): 1, get liliquoid after stirring, this liliquoid is heated under 90 ℃～100 ℃ temperature, cool to room temperature is also aging then, the sediment of gained of will wearing out at last separates, spend deionised water to neutral, obtain magnetic nano hydroxyapatite adsorbent after drying, the grinding.
3. preparation method according to claim 2 is characterized in that: the concentration of described ammonia spirit is 25%～28%.
4. according to claim 2 or 3 described preparation methods, it is characterized in that: the Ca (NO behind the described adjust pH
3)
2Solution, (NH
4)
2HPO
4The pH value of solution is 10～11.
5. according to claim 2 or 3 described preparation methods, it is characterized in that: the time of described liliquoid heating is 2h～3h.
6. the application of a magnetic nano hydroxyapatite adsorbent, it is characterized in that: with the heavy metal ion in the described adsorbent removal waste water, described heavy metal comprises one or more in copper, lead, zinc, cobalt, nickel, manganese, cadmium, mercury, tungsten, the molybdenum, and described adsorbent consumption in waste water is 0.1g/L～0.2g/L.
7. application according to claim 6 is characterized in that: the pH value when described adsorbent carries out adsorption treatment in waste water is controlled at 5～8, and the time of adsorption treatment is controlled at 12h～24h.
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