CN114715941B - Preparation method of high-purity lead tungstate powder - Google Patents
Preparation method of high-purity lead tungstate powder Download PDFInfo
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- CN114715941B CN114715941B CN202210562479.2A CN202210562479A CN114715941B CN 114715941 B CN114715941 B CN 114715941B CN 202210562479 A CN202210562479 A CN 202210562479A CN 114715941 B CN114715941 B CN 114715941B
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- NKTZYSOLHFIEMF-UHFFFAOYSA-N dioxido(dioxo)tungsten;lead(2+) Chemical compound [Pb+2].[O-][W]([O-])(=O)=O NKTZYSOLHFIEMF-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000000843 powder Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims abstract description 28
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 15
- 239000000084 colloidal system Substances 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 12
- 239000012066 reaction slurry Substances 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- -1 tungstate ions Chemical class 0.000 description 3
- 229910000004 White lead Inorganic materials 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002059 diagnostic imaging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000002600 positron emission tomography Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
Abstract
The invention belongs to the technical field of chemical materials, and discloses a preparation method of high-purity lead tungstate powder. The method comprises the steps of selecting analytically pure ammonium tungstate and analytically pure lead nitrate as raw materials, dripping a lead nitrate solution into the ammonium tungstate solution at a certain speed for chemical reaction, and then aging, ammonia water treatment and washing reaction products to obtain high-purity lead tungstate powder with the purity of more than 4N. The preparation process is simple and controllable, and is convenient for large-scale production.
Description
Technical Field
The invention belongs to the technical field of chemical materials, and relates to a preparation method of high-purity lead tungstate powder.
Background
The lead tungstate has a molecular formula of PbWO 4, is a novel scintillation material, has the characteristics of high density, high absorption coefficient, short radiation, high irradiation hardness, rapid luminescence attenuation and the like, and can be applied to the medical imaging fields such as positron emission tomography.
The properties of lead tungstate crystals increase with increasing purity. The preparation of the high-purity lead tungstate powder has unique application value, can provide raw materials for the later-stage growth of lead tungstate monocrystal, and can more efficiently explore the influence of ion doping of different types and different concentrations on the morphology of the lead tungstate crystal.
Patent document CN102774888a discloses a preparation method of lead tungstate nano powder, which uses self-emulsifying property of reactant to stabilize microemulsion, and obtains nano lead tungstate powder. However, the document does not address the preparation of high purity lead tungstate powder.
Patent document CN101973583a discloses a preparation method of high-scintillation lead tungstate powder, which is controlled by coprecipitation chemical reaction conditions to obtain lead tungstate grains with special morphology and two-phase coexistence structure containing granular tetragonal nano grains and lath monoclinic micro grains. Although the lead tungstate crystal grains with special morphology have high flicker performance after heat treatment, the high-purity lead tungstate powder is not researched.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a preparation method of high-purity lead tungstate powder, which realizes the preparation of 4N and above high-purity lead tungstate powder and provides raw material guarantee for the growth of high-quality lead tungstate crystals.
In order to achieve the above object, the present invention provides the following specific technical solutions.
The preparation method of the high-purity lead tungstate powder comprises the following steps:
Step S1, respectively selecting analytically pure ammonium tungstate and analytically pure lead nitrate as raw materials to prepare an ammonium tungstate solution and a lead nitrate solution;
step S2, dropwise adding the lead nitrate solution into the ammonium tungstate solution at a certain rate, and stirring for chemical reaction;
Step S3, ageing the reaction slurry obtained in the step S2, and then filtering to obtain lead tungstate precipitate;
s4, putting the lead tungstate precipitate into ammonia water, stirring, and filtering to obtain lead tungstate colloid;
and S5, washing and drying the lead tungstate colloid to obtain high-purity lead tungstate powder with the purity of more than 4N.
In a part of the preferred embodiments of the present invention, the temperature of the ammonia water in step S4 is 60 to 80 ℃. The inventor creatively discovers that the solubility of impurities in the lead tungstate precipitate in ammonia water at 60-80 ℃ is larger, and the lead tungstate can obtain better primary purification effect.
In a part of the preferred embodiments of the present invention, the concentration of the lead nitrate solution is 5 to 10mol/L, and the concentration of the ammonium tungstate solution is 1 to 5mol/L.
Further, in a part of the preferred embodiments of the present invention, in the step S2, the rate of dropping the lead nitrate solution into the ammonium tungstate solution is 50 to 500ml/S.
In a preferred embodiment of the present invention, the stirring speed in step S2 is 500 to 1000rpm.
In a part of the preferred embodiments of the present invention, the aging time in step S3 is 2 to 5 hours.
In a preferred embodiment of the present invention, the washing in step S5 is performed in the following manner: washing with pure water or ultrapure water, washing with absolute ethyl alcohol, and circulating.
In some preferred embodiments of the present invention, the temperature of the drying in step S5 is 60 to 100 ℃.
Compared with the prior art, the invention has the following obvious beneficial effects:
(1) The analytical grade ammonium tungstate and the analytical grade lead nitrate are selected as raw materials, so that the problem of low product purity caused by low raw material purity is solved.
(2) Before washing, the lead tungstate precipitate is stirred in ammonia water, so that a lead tungstate colloid which is purified for the first time can be obtained, and the purity of the product is further ensured.
(3) The lead tungstate product with the purity of more than 4N can be prepared by the preparation method.
(4) The preparation process is a coprecipitation process, and the process is simple and controllable, and is convenient for large-scale production.
Detailed Description
The following detailed description of the invention is merely exemplary and explanatory and should not be taken as limiting the scope of the invention. Furthermore, the features in the embodiments of the present document and in the different embodiments can be combined accordingly by a person skilled in the art from the description of the present document.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1
The embodiment comprises the following steps:
(1) Under the room temperature condition, 1094mL of ammonium tungstate solution with the concentration of 1mol/L and 2500mL of lead nitrate solution with the concentration of 5mol/L are respectively prepared by deionized water, analytical grade ammonium tungstate and analytical grade lead nitrate, and the ammonium tungstate is excessive by 5 mol%;
(2) Pouring the prepared lead nitrate solution into a constant-pressure dropping funnel, and uniformly dropping the lead nitrate solution into the prepared ammonium tungstate solution at a rate of 50mL/s, wherein lead ions react with tungstate ions in the dropping process to generate lead tungstate precipitates; in the reaction process, the stirring speed of the reaction system is 500r/min;
(3) After the dropwise addition of the lead nitrate solution is completed, stirring and reacting for 1h, standing for 2h, and ageing the reaction slurry;
(4) Filtering the aged slurry, putting the solid phase into ammonia water at 60 ℃ and stirring for 30min, and then filtering to obtain lead tungstate colloid;
(5) Repeatedly washing the lead tungstate colloid with pure water and absolute ethyl alcohol, and then drying at 60 ℃ to obtain white lead tungstate powder.
Comparative example 1
The comparative example differs from example 1 only in that there is no ammonia water treatment step described in step (4).
Example 2
The embodiment comprises the following steps:
(1) Under the room temperature condition, 855mL of ammonium tungstate solution with the concentration of 8mol/L and 3500mL of lead nitrate solution with the concentration of 8mol/L are respectively prepared by deionized water, analytical grade ammonium tungstate and analytical grade lead nitrate, and the ammonium tungstate is excessive by 10 mol percent;
(2) Pouring the prepared lead nitrate solution into a constant-pressure dropping funnel, and uniformly dropping the lead nitrate solution into the prepared ammonium tungstate solution at a rate of 200mL/s, wherein lead ions react with tungstate ions in the dropping process to generate lead tungstate precipitates; in the reaction process, the stirring speed of the reaction system is 750r/min;
(3) After the dropwise adding of the lead nitrate solution is completed, continuously stirring the reaction slurry for 2 hours, standing for 3 hours, and aging the reaction slurry;
(4) Filtering the aged reaction slurry, putting the solid phase into 70 ℃ ammonia water, stirring for 50min, and filtering to obtain primarily purified lead tungstate colloid;
(5) Repeatedly washing and filtering the lead tungstate colloid with pure water and absolute ethyl alcohol for five times to obtain a high-purity lead tungstate colloid; and drying the high-purity lead tungstate colloid at 80 ℃ to obtain high-purity lead tungstate powder.
Example 3
The embodiment comprises the following steps:
(1) Under the room temperature condition, respectively preparing 1200mL of ammonium tungstate solution with the concentration of 5mol/L and 6000mL of lead nitrate solution with the concentration of 10mol/L by using deionized water, analytical grade ammonium tungstate and analytical grade lead nitrate, wherein the ammonium tungstate is excessive by 20 mol%;
(2) Pouring the prepared lead nitrate solution into a constant-pressure dropping funnel, and uniformly dropping the lead nitrate solution into the prepared ammonium tungstate solution at a rate of 500mL/s, wherein lead ions react with tungstate ions in the dropping process to generate lead tungstate precipitates; in order to ensure the reaction to be sufficient, the reaction system is stirred in the reaction process, and the stirring speed is 1000r/min;
(3) After the dropwise adding of the lead nitrate solution is completed, continuously stirring the reaction slurry for 5 hours, standing for 4 hours, and aging the reaction slurry;
(4) Filtering the aged reaction slurry, putting the solid phase into 80 ℃ ammonia water, stirring for 60min, and filtering to obtain the primarily purified lead tungstate colloid.
(5) Repeatedly washing and filtering the lead tungstate colloid with ultrapure water and absolute ethyl alcohol for ten times to obtain high-purity lead tungstate colloid, and drying at 100 ℃ to obtain white lead tungstate powder.
The purity of the lead tungstate powders obtained in examples 1 to 3 and comparative example 1 was measured by ICP-MS, and the measurement results are shown in Table 1.
TABLE 1 impurity and content of lead tungstate powder
According to the purity detection result of the lead tungstate powder, the reaction slurry after aging can be initially purified in ammonia water.
The above embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to apply equivalents and modifications according to the technical solution and the concept of the present invention within the scope of the present invention.
Claims (7)
1. The preparation method of the high-purity lead tungstate powder is characterized by comprising the following steps of:
Step S1, respectively selecting analytically pure ammonium tungstate and analytically pure lead nitrate as raw materials to prepare an ammonium tungstate solution and a lead nitrate solution;
step S2, dropwise adding the lead nitrate solution into the ammonium tungstate solution at a certain rate, and stirring for chemical reaction;
Step S3, ageing the reaction slurry obtained in the step S2, and then filtering to obtain lead tungstate precipitate;
s4, putting the lead tungstate precipitate into ammonia water, stirring, and filtering to obtain lead tungstate colloid; the temperature of the ammonia water is 60-80 ℃;
and S5, washing and drying the lead tungstate colloid to obtain high-purity lead tungstate powder with the purity of more than 4N.
2. The method according to claim 1, wherein the concentration of the lead nitrate solution is 5 to 10mol/L, and the concentration of the ammonium tungstate solution is 1 to 5mol/L.
3. The method according to claim 2, wherein in step S2, the rate of dropping the lead nitrate solution into the ammonium tungstate solution is 50 to 500ml/S.
4. The method according to claim 1, wherein the stirring speed in step S2 is 500 to 1000rpm.
5. The method according to claim 1, wherein the aging time in step S3 is 2 to 5 hours.
6. The method of claim 1, wherein the washing in step S5 is performed by: pure water or ultrapure water washing, and absolute ethanol washing.
7. The method according to claim 1, wherein the temperature of the drying in step S5 is 60-100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210562479.2A CN114715941B (en) | 2022-05-23 | Preparation method of high-purity lead tungstate powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210562479.2A CN114715941B (en) | 2022-05-23 | Preparation method of high-purity lead tungstate powder |
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| Publication Number | Publication Date |
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| CN114715941A CN114715941A (en) | 2022-07-08 |
| CN114715941B true CN114715941B (en) | 2024-06-07 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973583A (en) * | 2010-10-28 | 2011-02-16 | 中国科学院上海硅酸盐研究所 | Preparation method of lead tungstate powder with high scintillation property |
| CN102303903A (en) * | 2011-08-19 | 2012-01-04 | 天津市化学试剂研究所 | Method for preparing high-purity lead titanate |
| CN104891576A (en) * | 2015-05-06 | 2015-09-09 | 陕西省紫阳县湘贵锰业有限公司 | Preparation method of manganese sulfate monohydrate |
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973583A (en) * | 2010-10-28 | 2011-02-16 | 中国科学院上海硅酸盐研究所 | Preparation method of lead tungstate powder with high scintillation property |
| CN102303903A (en) * | 2011-08-19 | 2012-01-04 | 天津市化学试剂研究所 | Method for preparing high-purity lead titanate |
| CN104891576A (en) * | 2015-05-06 | 2015-09-09 | 陕西省紫阳县湘贵锰业有限公司 | Preparation method of manganese sulfate monohydrate |
Non-Patent Citations (2)
| Title |
|---|
| Precipitation of tungstates of silver and lead;M.C. Mehra, K. Kant;Journal of Inorganic and Nuclear Chemistry;第25卷(第7期);896-899 * |
| 陈春椿.重要无机化学反应.上海科学技术出版社,1982,(第二版),514. * |
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