CN102071466A - Method for preparing lead molybdate polycrystalline material - Google Patents
Method for preparing lead molybdate polycrystalline material Download PDFInfo
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- CN102071466A CN102071466A CN 201010604439 CN201010604439A CN102071466A CN 102071466 A CN102071466 A CN 102071466A CN 201010604439 CN201010604439 CN 201010604439 CN 201010604439 A CN201010604439 A CN 201010604439A CN 102071466 A CN102071466 A CN 102071466A
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- lead
- molybdate
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- polycrystal
- salt
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Abstract
The invention discloses a method for preparing a lead molybdate polycrystalline material and relates to a method for preparing a polycrystalline lead molybdate raw material used for preparing the lead molybdate polycrystalline material. The method is characterized in that: soluble lead salt and insoluble ammonium molybdate serve as raw materials in the preparation process, and the method comprises the following steps of: dissolving the lead salt in water to prepare saturated solution, and adding the insoluble ammonium molybdate into the saturated lead salt solution; regulating the pH value, heating, evaporating and concentrating with stirring to recrystallize the lead salt, filtering and drying; and calcining to prepare the lead molybdate polycrystalline material. The method for preparing the lead molybdate polycrystalline material effectively solves the problems that solid powder is hard to mix or hard to filter through a wet process and volatilizes at high temperature and the like, and the prepared lead molybdate polycrystalline material has stable raw material components, pure color and low impurity content.
Description
Technical field
A kind of preparation method of lead molybdate polycrystal relates to a kind of preparation method who is used to prepare the polycrystalline lead molybdate raw material of lead molybdate single crystal material.
Background technology
Lead molybdate (PbMoO
4) crystal is a kind of good acousto-optic medium material, has high acousto-optic quality factor M
Z〉=36.0 * 10
-18s
3/ g, low acoustic loss, good specific acoustic resistance coupling, can be used as acousto-optic accent shop device and acousto-optic deflection device is the optical modulation crystal, it is modern main acousto-optic crsytal material, be widely used for fields such as laser display, printing, printing and fax, and aspect such as the optical memory of the scanning of TV and large screen display, photonic computer and laser communication.
At present, the preparation method of lead molybdate single crystal generally adopts seed crystal crystal pulling method or falling crucible method, is about to plumbous oxide and molybdenum oxide, according to the 1:1 mixed in molar ratio, and high temperature growth down.But since pressed powder plumbous oxide and molybdenum oxide difficulty mix, and volatilization is in various degree arranged at high temperature, make the crystal chemistry composition of growth depart from former proportioning, crystal mass descends.Also can synthesize the lead molybdate polycrystal raw material earlier, carry out high temperature again and lift/degrowth in crucible, the lead molybdate single crystal performance quality of this method preparation is better.Synthetic method generally adopts precipitator method preparation, is raw material with solubility lead salt and Ammonium Heptamolybdate promptly, generates the lead molybdate precipitation in the aqueous solution.But also there is certain problem in this method: the lead molybdate particle that is settled out is tiny, and approximate cow's milk shape is difficult to filter, and easily adsorbs impurity, and the raw material color jaundice after the oven dry is more difficult to get the final stoichiometry product.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provide a kind of and can effectively solve pressed powder batch mixing difficulty or problems such as the wet method filtration is difficult, the following volatilization of high temperature, the lead molybdate polycrystal raw material stable components of preparation, the preparation method of the lead molybdate polycrystal that foreign matter content is low.
The objective of the invention is to be achieved through the following technical solutions.
A kind of preparation method of lead molybdate polycrystal, it is characterized in that it is raw material that solubility lead salt and insoluble ammonium molybdate are at first selected in its preparation process employing, lead salt dissolved make saturated solution in the water, in this solution, add insoluble ammonium molybdate again, under agitation heating evaporation concentrates, make the lead salt recrystallization, filter, dry, the lead molybdate polycrystal is made in last roasting.
The preparation method of a kind of lead molybdate polycrystal of the present invention, it is characterized in that with lead salt dissolve make in the water saturated solution process be with lead salt under 40～60 ℃ of temperature, the saturated solution that is dissolved in the water and makes.
The preparation method of a kind of lead molybdate polycrystal of the present invention, after it is characterized in that adding insoluble ammonium molybdate in the lead salt saturated solution, regulating the pH value with acid/alkali is 5.5～7.0.
The preparation method of a kind of lead molybdate polycrystal of the present invention is characterized in that the heating evaporation concentration process is evaporated at 1/2 o'clock with amount of liquid, stops heating and stirring, carries out solid-liquid separation.
The preparation method of a kind of lead molybdate polycrystal of the present invention is characterized in that it is 500～550 ℃ of roastings 5～6 hours that lead molybdate polycrystal process is made in roasting.
The preparation method of a kind of lead molybdate polycrystal of the present invention is characterized in that the solubility lead salt is lead acetate, lead nitrate, is preferably lead acetate.
The preparation method of a kind of lead molybdate polycrystal of the present invention is characterized in that insoluble ammonium molybdate is ammonium tetramolybdate, ammonium octamolybdate or ammomium dodecamolybdate, is preferably ammonium tetramolybdate, more preferably ammomium dodecamolybdate.
The preparation method of a kind of lead molybdate polycrystal of the present invention is characterized in that the Pb:Mo mol ratio in preparation process solubility lead salt and the insoluble ammonium molybdate is 2:1.
The preparation method of a kind of lead molybdate polycrystal of the present invention at first produces the full solution that closes of lead salt, adds insoluble ammonium molybdate, make the lead salt recrystallization, in this process, insoluble ammonium molybdate is washed, the separating impurity element, filter the synthetic lead molybdate of last roasting then.Efficiently solve pressed powder batch mixing difficulty or wet method and filter problems such as difficulty, the following volatilization of high temperature, the lead molybdate polycrystal raw material stable components of preparing, chemistry is than Pb:Mo=0.99～1, and color is pure, and foreign matter content is low.
Embodiment
A kind of preparation method of lead molybdate polycrystal at first selects the solubility lead salt, as lead acetate (Pb (CH
3COO)
23H
2O), lead nitrate (Pb (NO
3)
2), lead salt to be dissolved make saturated solution in the water, temperature is 40～60 ℃, adds insoluble ammonium molybdate again, as ammonium tetramolybdate ((NH
4)
2Mo
4O
132H
2O, ATM), ammonium octamolybdate ((NH
4)
4Mo
8O
26, AOM), ammomium dodecamolybdate ((NH
4)
2Mo
12MoO
406H
2O, AMM), regulating the pH value with acid/alkali is 5.5～7.0, stirs, evaporation at constant temperature makes lead salt reduce and recrystallization with rate of water added, obtains washing at this process ammonium molybdate.To be evaporated during to amount of liquid 1/2, stop heating and stir, solid-liquid separation, oven dry solid are placed solid in the crucible again, 500～550 ℃ of roastings 5～6 hours, obtain the lead molybdate polycrystal raw material.
Embodiment 1
With 0.8 mole of Pb (NO
3)
2(purity 99.99%) is dissolved in the pure water fully, makes saturated solution, 60 ℃ of temperature.Add 0.1 mole of ATM(purity 99.99%), stir, regulate pH value 5.5, evaporation at constant temperature with nitric acid/ammoniacal liquor; To be evaporated during to amount of liquid 1/2, stop heating and stir, solid-liquid separation, oven dry solid are placed solid in the crucible then, 550 ℃ of roastings 6 hours, obtain the lead molybdate polycrystal raw material.According to the lead molybdate product that this method obtains, chemical than Pb:Mo=0.99～1, foreign matter content iron, cobalt, nickel, copper, chromium, manganese≤1 * 10
-4%.
Embodiment 2
With 0.8 mole of Pb (CH
3COO)
23H
2O(purity 99.99%), be dissolved in fully in the pure water, make saturated solution, 50 ℃ of temperature.Add 0.05 mole of AOM(purity 99.99%), stir, regulate pH value 6.0, evaporation at constant temperature with acetate/ammoniacal liquor; To be evaporated during to amount of liquid 1/2, stop heating and stir, solid-liquid separation, oven dry solid are placed solid in the crucible then, 500 ℃ of roastings 5 hours, obtain the lead molybdate polycrystal raw material.According to the lead molybdate product that this method obtains, chemical than Pb:Mo=0.99～1, foreign matter content iron, cobalt, nickel, copper, chromium, manganese≤1 * 10
-4%.
Embodiment 3
With 0.52 mole of Pb (CH
3COO)
23H
2O(purity 99.99%), be dissolved in fully in the pure water, make saturated solution, 40 ℃ of temperature.Add 0.02 mole of AMM(purity 99.99%), stir, regulate pH value 7.0, evaporation at constant temperature with acetate/ammoniacal liquor; To be evaporated during to amount of liquid 1/2, stop heating and stir, solid-liquid separation, oven dry solid are placed solid in the crucible then, 520 ℃ of roastings 5 hours, obtain the lead molybdate polycrystal raw material.According to the lead molybdate product that this method obtains, chemical than Pb:Mo=0.99～1, foreign matter content iron, cobalt, nickel, copper, chromium, manganese≤1 * 10
-4%.
Claims (5)
1. the preparation method of a lead molybdate polycrystal, it is characterized in that it is raw material that solubility lead salt and insoluble ammonium molybdate are at first selected in its preparation process employing, lead salt dissolved make saturated solution in the water, in the lead salt saturated solution, add insoluble ammonium molybdate again, stir, evaporation at constant temperature concentrates, and makes the lead salt recrystallization, filter, dry, the lead molybdate polycrystal is made in last roasting.
2. the preparation method of a kind of lead molybdate polycrystal according to claim 1, it is characterized in that with lead salt dissolve make in the water saturated solution process be with lead salt under 40～60 ℃ of temperature, the saturated solution that is dissolved in the water and makes.
3. the preparation method of a kind of lead molybdate polycrystal according to claim 1, after it is characterized in that adding insoluble ammonium molybdate in the lead salt saturated solution, regulating the pH value with acid/alkali is 5.5～7.0.
4. the preparation method of a kind of lead molybdate polycrystal according to claim 1 is characterized in that the evaporation at constant temperature process is evaporated at 1/2 o'clock with amount of liquid, stops heating and stirring, carries out solid-liquid separation.
5. the preparation method of a kind of lead molybdate polycrystal according to claim 1 is characterized in that it is 500～550 ℃ of roastings 5～6 hours that lead molybdate polycrystal process is made in roasting.
6.The preparation method of a kind of lead molybdate polycrystal according to claim 1 is characterized in that the solubility lead salt is lead acetate, lead nitrate, is preferably lead acetate.
7.The preparation method of a kind of lead molybdate polycrystal according to claim 1 is characterized in that insoluble ammonium molybdate is ammonium tetramolybdate, ammonium octamolybdate or ammomium dodecamolybdate, is preferably ammonium tetramolybdate, more preferably ammomium dodecamolybdate.
8.The preparation method of a kind of lead molybdate polycrystal according to claim 1 is characterized in that preparation process solubility lead salt is that Pb:Mo mol ratio in lead acetate and the insoluble ammonium molybdate is 2:1.
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|---|---|---|---|
| CN201010604439A CN102071466B (en) | 2010-12-24 | 2010-12-24 | Method for preparing lead molybdate polycrystalline material |
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| CN102071466A true CN102071466A (en) | 2011-05-25 |
| CN102071466B CN102071466B (en) | 2012-10-17 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103359791A (en) * | 2013-07-03 | 2013-10-23 | 吉林化工学院 | Vanadic acid-chrome molybdate mixed cluster polyacid compound structure and preparation method |
| CN103387263A (en) * | 2013-07-11 | 2013-11-13 | 洛阳理工学院 | Lead molybdate nano crystal material and preparation method thereof |
| CN105016389A (en) * | 2015-07-14 | 2015-11-04 | 首都师范大学 | Carbon shell-coated lead molybdate nanocrystal and preparation method thereof |
| CN113463179A (en) * | 2021-06-09 | 2021-10-01 | 郑州大学 | Preparation method of large-size beta-type ammonium tetramolybdate single crystal particles |
| KR102505673B1 (en) | 2022-08-04 | 2023-03-03 | 주식회사 지엠엔지니어링 | High Expansion Foam Firefighting Drone |
Citations (4)
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|---|---|---|---|---|
| US3653814A (en) * | 1970-08-03 | 1972-04-04 | Bell Telephone Labor Inc | Technique for the growth of single crystal lead molybdate |
| JPS57145100A (en) * | 1981-02-26 | 1982-09-07 | Tohoku Metal Ind Ltd | Preparation of light-modulating medium made of lead molybdate single crystal |
| JPH0393629A (en) * | 1989-09-05 | 1991-04-18 | Taki Chem Co Ltd | Production of lead molybdate for raw material of single crystal |
| CN1635194A (en) * | 2003-12-30 | 2005-07-06 | 宁波大学 | Falling crucible method growth process for lead molybdate single crystal |
-
2010
- 2010-12-24 CN CN201010604439A patent/CN102071466B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3653814A (en) * | 1970-08-03 | 1972-04-04 | Bell Telephone Labor Inc | Technique for the growth of single crystal lead molybdate |
| JPS57145100A (en) * | 1981-02-26 | 1982-09-07 | Tohoku Metal Ind Ltd | Preparation of light-modulating medium made of lead molybdate single crystal |
| JPH0393629A (en) * | 1989-09-05 | 1991-04-18 | Taki Chem Co Ltd | Production of lead molybdate for raw material of single crystal |
| CN1635194A (en) * | 2003-12-30 | 2005-07-06 | 宁波大学 | Falling crucible method growth process for lead molybdate single crystal |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103359791A (en) * | 2013-07-03 | 2013-10-23 | 吉林化工学院 | Vanadic acid-chrome molybdate mixed cluster polyacid compound structure and preparation method |
| CN103387263A (en) * | 2013-07-11 | 2013-11-13 | 洛阳理工学院 | Lead molybdate nano crystal material and preparation method thereof |
| CN103387263B (en) * | 2013-07-11 | 2015-02-11 | 洛阳理工学院 | Lead molybdate nano crystal material and preparation method thereof |
| CN105016389A (en) * | 2015-07-14 | 2015-11-04 | 首都师范大学 | Carbon shell-coated lead molybdate nanocrystal and preparation method thereof |
| CN113463179A (en) * | 2021-06-09 | 2021-10-01 | 郑州大学 | Preparation method of large-size beta-type ammonium tetramolybdate single crystal particles |
| KR102505673B1 (en) | 2022-08-04 | 2023-03-03 | 주식회사 지엠엔지니어링 | High Expansion Foam Firefighting Drone |
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| Publication number | Publication date |
|---|---|
| CN102071466B (en) | 2012-10-17 |
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