CN103569986A - Microwave assisted synthetic method of lead hydroxyapatite - Google Patents
Microwave assisted synthetic method of lead hydroxyapatite Download PDFInfo
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- CN103569986A CN103569986A CN201210474488.2A CN201210474488A CN103569986A CN 103569986 A CN103569986 A CN 103569986A CN 201210474488 A CN201210474488 A CN 201210474488A CN 103569986 A CN103569986 A CN 103569986A
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- hydroxyapatite
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- plumbous
- lead
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Abstract
The invention belongs to the technical field of artificial synthesis of minerals, and particularly relates to a synthetic method of a lead hydroxyapatite material. The synthetic method is characterized in that a microwave assisted method is used for synthesizing lead hydroxyapatite. According to the technical scheme, the synthetic method comprises the following steps of: mixing lead nitrate and diammonium hydrogen phosphate serving as raw materials according to a molar ration of lead to phosphorus being 1.67; regulating the pH value of a mixed solution to 8.0-10.0 by using ammonia, wherein the water bath temperature is 20-80 DEG C; carrying out microwave synthesis for 15 minutes under the conditions of condensing reflux and strong magnetic stirring; cooling, and then washing deposits for 3-5 times by using distilled water; drying solids in a drying oven at 80 DEG C for 12 hours; grinding to obtain the lead hydroxyapatite. The lead hydroxyapatite prepared by utilizing the method disclosed by the invention has the advantages of good crystallinity degree, high purity and high yield (higher than 95%). The synthetic method disclosed by the invention has the advantages of simple and easily available raw materials, low cost, simple and easily controlled process, high reaction rate, low-temperature synthesis, and the like; the powder can be used in the fields of High Performance Liquid Chromatography materials, methane exclusive catalyst materials, and the like.
Description
Technical field
The invention belongs to the synthetic technical field of inorganic materials, relate in particular to the artificial synthesis of plumbous hydroxyapatite.
Background technology
Plumbous hydroxyapatite (Pb
10(PO
4)
6(OH)
2) be that lead ion isomorph is replaced hydroxyapatite (Ca
10(PO
4)
6(OH)
2) in calcium ion after formed a kind of phosphate mineral.The introducing of external lead ion can affect degree of crystallinity, pattern, lattice parameter and the stability of hydroxyapatite structure, makes plumbous hydroxyapatite show many exclusive structural performances and obtains many special application.The sorbent material that it can be used as high performance liquid chromatography is isolated protein or other biological molecule optionally, can also accelerate as effective catalyst the oxidation coupling reaction of methane.
The preparation method of current plumbous hydroxyapatite mainly contains: solid reaction process, hydrothermal synthesis reaction method, liquid-phase precipitation reaction method etc.The process of solid reaction process is simple, but its speed of response is slow, and reaction time is long, and raw material needs to grind, easy pickup in process, the poor activity of product; Hydrothermal synthesis reaction method can obtain good plumbous hydroxyapatite monocrystalline, but to equipment require highly, cost is high.
With respect to solid reaction process and hydrothermal synthesis reaction method, the advantage such as liquid-phase precipitation reaction method has reaction conditions gentleness, and product purity is high, and technique is simple and by synthetic for plumbous hydroxyapatite more.The people such as Shigeru Sugiyama are with lead hydroxynitrate Pb (NO
3)
25PbO and phosphoric acid H
3pO
4for raw material, control the pH of suspension in 11 left and right, under boiling state, stir 3h, by filtering, after washing, be deposited in dry a whole night at 100 ℃, calcine 3h at 500 ℃, obtain plumbous hydroxyapatite (Sugiyama S.; Nakanishi T.; Ishimura T.; Moriga T.; Hayashi H.; Shigemoto N.; Moffat J.B. Preparation, characterization, and thermal stability of lead hydroxyapatite, Joural of Solid State Chemistry, 1999,143:296-302.).The people such as Zhiliang Xiu are with cetyl trimethylammonium bromide CTAB, the plumbous Pb (CH of acetate trihydrate
3cOO)
23H
2o and primary ammonium phosphate NH
4h
2pO
4for raw material, control the pH of suspension in 8 left and right, (25 ℃, 100 ℃ and 150 ℃) successive reaction 12h under differing temps, obtains plumbous hydroxyapatite (Xiu Z.L. after filtration, washing precipitation; Lv M.K.; Gu F.; Wang S.F.; Xu D.; Yuan D.R. Synthesis and characterization of lead phosphate hydroxyapatite nanoparticles, Inorganic Chemistry Communications, 2004,7:604-606.).The people such as Jai Hyun Park are with four water-calcium nitrate Ca (NO
3)
24H
2o, Secondary ammonium phosphate (NH
4)
2hPO
4, ammonium chloride NH
4cl and lead nitrate Pb (NO
3)
2for precursor, control the pH of suspension in 9 left and right, fully stir 2h at 90 ℃, by filtering, after washing, being deposited in dry a whole night at 110 ℃, in 400 ℃ of calcining 3h, obtain plumbous hydroxyapatite (the Park J.H of non-stoichiometric; Lee D.W.; Im S.W., Lee Y.H.; Suh D.J.; Jun K.W.; Lee K.Y. Oxidative coupling of methane using non-stoichiometric lead hydroxyapatite catalyst mixtures, Fuel, 2012,94:433-439.).But these methods all exist reaction time longer, the shortcoming that cost is higher.Therefore, develop a kind of not only simply but also efficiently preparation method synthesize fast plumbous hydroxyapatite, tool is of great significance.
Summary of the invention
The object of this invention is to provide a kind of plumbous hydroxyapatite fast preparation method.
In order to realize above-mentioned object, the present invention adopts following steps to realize: take lead nitrate and Secondary ammonium phosphate as raw material, the ratio that is 1.67 in plumbous phosphorus mol ratio is mixed, with ammoniacal liquor, regulate the pH value of mixed solution 8.0 ~ 10.0, under condensing reflux and strong magnetic agitation condition, microwave synthesizes 15min, then obtains plumbous hydroxyapatite through processes such as filtering, wash, be dry.
The invention has the beneficial effects as follows: the plumbous hydroxylapatite crystal degree that utilizes the inventive method to prepare is good, purity is high, productive rate high (being greater than 95%).The advantages such as it is simple and easy to get, with low cost that the inventive method has raw material, and technique is simple and easy to control, speed of reaction is fast, can low temperature synthetic, its powder can be used for the fields such as high performance liquid chromatography sorbing material and the exclusive catalyzer of methane.
Accompanying drawing explanation
The XRD powder diagram that accompanying drawing is the plumbous hydroxyapatite that adopts the inventive method and prepare.
Embodiment
embodiment 1:
(1) lead nitrate solution that compound concentration is 0.5mol/L is A solution; Compound concentration is the ammonium dibasic phosphate solution of 0.3mol/L, is B solution.Respectively get the A of 50ml and B solution in there-necked flask, after mixing, and with ammoniacal liquor, to regulate the pH value of mixed solution be 8 ~ 10, formation mixed solution C;
(2) mixed solution C is placed in to microwave extracting synthesizer, under condensing reflux and strong magnetic agitation condition, bath temperature is 80 ℃, and microwave power is 700W, and microwave synthesizes 15min;
(3) after step (2) gained material is filtered, use first water centrifuge washing throw out 3 ~ 5 times;
(4) by the dry 12h in the baking oven of 80 ℃ that is deposited in of gained after step (3) centrifuge washing, after grinding, obtain product.From the XRD powder diagram of Fig. 1, this product is plumbous hydroxyapatite, and better crystallinity degree, the purity of product are high.
embodiment 2:
In example 1, the condition of (1), (3) and (4) is constant, changes the bath temperature in step (2) into 50 ℃, obtains plumbous hydroxyapatite.
embodiment 3:
In example 1, the condition of (1), (3) and (4) is constant, changes the bath temperature in step (2) into 20 ℃, obtains plumbous hydroxyapatite.
Claims (4)
1. the microwave rapid synthetic method of plumbous hydroxyapatite, it is characterized in that technical scheme comprises the following steps: take water miscible lead salt and phosphoric acid salt as raw material, the ratio that is 1.67 in plumbous phosphorus mol ratio is mixed, with ammoniacal liquor, regulate the pH value of mixed solution, under condensing reflux and strong magnetic agitation condition, microwave method is synthetic fast, through processes such as filtering, wash, be dry, obtains plumbous hydroxyapatite.
2. the microwave rapid synthetic method of plumbous hydroxyapatite according to claim 1, is characterized in that: described water miscible lead salt and phosphoric acid salt are respectively lead nitrate and Secondary ammonium phosphate.
3. the microwave rapid synthetic method of plumbous hydroxyapatite according to claim 1, is characterized in that: the pH value of mixed solution need be controlled at 8 ~ 10.
4. the microwave rapid synthetic method of plumbous hydroxyapatite according to claim 1, is characterized in that: microwave method fast synthetic condition is: bath temperature is 20 ~ 80 ℃; Microwave power is 700W; The microwave time is 15min.
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|---|---|---|---|
| CN201210474488.2A CN103569986A (en) | 2012-11-21 | 2012-11-21 | Microwave assisted synthetic method of lead hydroxyapatite |
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|---|---|---|---|
| CN201210474488.2A CN103569986A (en) | 2012-11-21 | 2012-11-21 | Microwave assisted synthetic method of lead hydroxyapatite |
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|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112079341A (en) * | 2020-09-06 | 2020-12-15 | 桂林理工大学 | Preparation method and application of lead-calcium-fluorapatite solid solution |
| CN112142026A (en) * | 2020-09-06 | 2020-12-29 | 桂林理工大学 | Preparation method and application of lead-fluorapatite solid solution |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1843903A (en) * | 2006-04-18 | 2006-10-11 | 蒋建军 | Preparation method of polycondensing lead phosphate and detection method thereof |
-
2012
- 2012-11-21 CN CN201210474488.2A patent/CN103569986A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1843903A (en) * | 2006-04-18 | 2006-10-11 | 蒋建军 | Preparation method of polycondensing lead phosphate and detection method thereof |
Non-Patent Citations (3)
| Title |
|---|
| A. LAGHZIZILA ET AL.: "Electrical behavior of hydroxyapatites M10(PO4)6(OH)2 (M 5 Ca, Pb, Ba)", 《MATERIALS RESEARCH BULLETIN》, vol. 36, 31 December 2001 (2001-12-31), pages 2 - 1 * |
| E. LERNER ET AL.: "Enhanced maturation of hydroxyapatite from aqueous solutions using microwave irradiation", 《JOURNAL OF MATERIALS SCIENCE: MATERIALS IN MEDICINE》, vol. 2, 31 December 1991 (1991-12-31), pages 2 - 2 * |
| 周吉峙等: "铅羟基磷灰石的形成与稳定性", 《无机材料学报》, vol. 24, no. 2, 31 March 2009 (2009-03-31), pages 259 - 263 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112079341A (en) * | 2020-09-06 | 2020-12-15 | 桂林理工大学 | Preparation method and application of lead-calcium-fluorapatite solid solution |
| CN112142026A (en) * | 2020-09-06 | 2020-12-29 | 桂林理工大学 | Preparation method and application of lead-fluorapatite solid solution |
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Application publication date: 20140212 |