CN111892090A - Preparation method of nano calcium tungstate - Google Patents
Preparation method of nano calcium tungstate Download PDFInfo
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- CN111892090A CN111892090A CN202010927457.2A CN202010927457A CN111892090A CN 111892090 A CN111892090 A CN 111892090A CN 202010927457 A CN202010927457 A CN 202010927457A CN 111892090 A CN111892090 A CN 111892090A
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- tungstate
- ball
- preparation
- ball milling
- calcium chloride
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- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 32
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 21
- 239000011575 calcium Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 14
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 10
- 239000001110 calcium chloride Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 239000000376 reactant Substances 0.000 claims abstract description 4
- 229960005069 calcium Drugs 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229960002713 calcium chloride Drugs 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 8
- 239000010431 corundum Substances 0.000 claims description 8
- 239000011224 oxide ceramic Substances 0.000 claims description 8
- JXSUUUWRUITOQZ-UHFFFAOYSA-N oxygen(2-);yttrium(3+);zirconium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Y+3].[Y+3].[Zr+4].[Zr+4] JXSUUUWRUITOQZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- LLSDKQJKOVVTOJ-UHFFFAOYSA-L calcium chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Ca+2] LLSDKQJKOVVTOJ-UHFFFAOYSA-L 0.000 claims description 5
- 229940052299 calcium chloride dihydrate Drugs 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 239000004677 Nylon Substances 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- FDMFQOCGNBYKPY-UHFFFAOYSA-N calcium;dioxido(dioxo)tungsten Chemical compound [Ca+2].[O-][W]([O-])(=O)=O FDMFQOCGNBYKPY-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010303 mechanochemical reaction Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000003801 milling Methods 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- QWMFKVNJIYNWII-UHFFFAOYSA-N 5-bromo-2-(2,5-dimethylpyrrol-1-yl)pyridine Chemical compound CC1=CC=C(C)N1C1=CC=C(Br)C=N1 QWMFKVNJIYNWII-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 229910004829 CaWO4 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crushing And Grinding (AREA)
Abstract
The invention discloses a preparation method of nano calcium tungstate, which comprises the following steps: (1) weighing tungstate and calcium chloride according to the preparation amount and the stoichiometric ratio; (2) putting the reactant weighed in the step (1) into a ball milling tank, putting the ball milling tank into a ball mill for ball milling for 1-3 hours, and taking out a ball milling product and a milling ball; (3) and (3) taking out the ground product obtained in the step (2), and washing, filtering and drying to obtain the nano calcium tungstate powder. The method takes common tungstate and calcium chloride as raw materials, prepares nano calcium tungstate with good dispersibility and uniform size by a mechanochemical reaction method, has the characteristics of low equipment requirement, high synthesis yield and no additive, is green and environment-friendly in synthesis process and low in preparation cost, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of inorganic nano material preparation, and relates to a preparation method of a calcium tungstate nano material.
Technical Field
Calcium tungstate is an important inorganic functional material, and is an effective luminescent material under the excitation of X rays, electron beams and ultraviolet rays due to the special crystal structure and energy band structure of the calcium tungstate, so that the calcium tungstate has very wide application in the fields of fluorescent and photoelectronic display devices, luminescent coatings, optical fiber devices, biological materials and the like. At present, the main methods for preparing calcium tungstate materials include hydrothermal/solvothermal methods (CN 102701282B), microemulsion methods (CN 1958884 a), ultrasonic chemistry methods (CN 106365203B), microwave radiation methods (CN 102718262B), etc., most of the synthetic products are nanowires, micro-blocks or micro-spheres, etc., and there is still a large space for improving and optimizing the morphology control and controllable synthesis of calcium tungstate nanomaterials.
In the last decade, mechanochemical reaction methods have attracted great research interest due to the characteristics of no or little solvent, high yield, little pollution, short time consumption, low energy consumption, simple operation and equipment, easy industrialization and the like, and have become a new way for developing green chemistry and technology. So far, no literature report is available for preparing the nano calcium tungstate material by adopting a mechanochemical method.
Disclosure of Invention
The invention aims to provide a preparation method of nano calcium tungstate, which is characterized in that common tungstate and calcium chloride are used as raw materials, a mechanochemical reaction method is adopted to obtain materials, and the materials are washed, filtered and dried to obtain the nano calcium tungstate with uniform size and good dispersibility.
The invention is realized by the following technical scheme.
A preparation method of nano calcium tungstate is characterized by comprising the following steps:
(1) weighing tungstate and calcium chloride according to a stoichiometric ratio;
(2) putting the reactant weighed in the step (1) into a ball mill for ball milling for 1-3 hours, and taking out a ball milling product and a grinding ball;
(3) and (3) washing, filtering and drying the ball-milled product obtained in the step (2) to obtain the nano calcium tungstate.
More specifically, the calcium chloride in the step (1) is calcium chloride dihydrate or anhydrous calcium chloride.
More specifically, the tungstate in the step (1) is one or more of alkali metal tungstate, ammonium paratungstate and ammonium metatungstate.
More specifically, the ball mill in the step (2) is a planetary ball mill, a stirring mill, a roller ball mill or a vibration mill.
More specifically, the material of the ball milling pot in the step (2) is yttrium zirconium oxide ceramic, stainless steel, agate, corundum, tungsten carbide, polytetrafluoroethylene or nylon, and the material of the grinding ball is yttrium zirconium oxide ceramic, stainless steel, agate, corundum or tungsten carbide.
More specifically, the drying in the step (3) is drying for 1-4 hours in an air-blast drying oven at 40-100 ℃.
The main advantages of the invention are: (1) the product calcium tungstate has small granularity, good dispersibility and uniform size; (2) the invention takes common tungstate and calcium chloride as raw materials, prepares the nano calcium tungstate by a mechanochemical method, has the characteristics of low equipment requirement, high synthesis yield and no additive, has green and environment-friendly synthesis process and low preparation cost, and is very suitable for industrial production.
Drawings
Figure 1 XRD pattern of sample of example 1.
FIG. 2 SEM photograph of the sample of example 1.
Detailed Description
The invention will be further illustrated by the following examples.
A preparation method of nano calcium tungstate is characterized by comprising the following steps:
(1) weighing tungstate and calcium chloride according to the stoichiometric ratio of the reaction formula; the calcium chloride is calcium chloride dihydrate or anhydrous calcium chloride; the tungstate is one or more of alkali metal tungstate, ammonium paratungstate and ammonium metatungstate.
(2) Putting the reactant weighed in the step (1) into a ball mill for ball milling for 1-3 hours, and taking out a ball milling product and a grinding ball; the ball mill is a planetary ball mill, a stirring mill, a roller ball mill or a vibration mill; the material of the ball milling tank is yttrium zirconium oxide ceramic, stainless steel, agate, corundum, tungsten carbide, polytetrafluoroethylene or nylon, and the material of the grinding ball is yttrium zirconium oxide ceramic, stainless steel, agate, corundum or tungsten carbide.
(3) Washing, filtering and drying the ball-milled product obtained in the step (2), wherein the drying is carried out for 1-4 hours in a forced air drying oven at the temperature of 40-100 ℃; thus obtaining the nano calcium tungstate.
Example 1
Accurately weighing 15g of sodium tungstate dihydrate and 10g of calcium chloride dihydrate, placing the sodium tungstate dihydrate and the calcium chloride dihydrate in a 250ml of polytetrafluoroethylene ball milling tank, wherein the grinding ball is made of corundum, carrying out ball milling for 3 hours by using a planetary ball mill, taking out a ball milling product and the grinding ball, washing the ball milling product for three times, filtering, and drying in a 60 ℃ air-blast drying oven for 2 hours to obtain the nano calcium tungstate powder. XRD analysis of the sample was performed, and the results are shown in FIG. 1, XRD pattern and CaWO4The JCDPS number is matched with 85-0443, which shows that calcium tungstate powder is obtained; SEM analysis is carried out on the sample, and the result is shown in figure 2, and the calcium tungstate powder is uniformly dispersed and has no obvious agglomeration phenomenon.
In the above embodiment of the invention, the ball milling pot is made of polytetrafluoroethylene, or yttrium zirconium oxide ceramic, stainless steel, agate, corundum, tungsten carbide, nylon and other materials, and has good wear resistance and no pollution to products. Similarly, the material of the grinding ball can also be yttrium zirconium oxide ceramic, stainless steel, agate, tungsten carbide and the like.
The ball mill in the present invention may be a stirring mill, a tumbling mill or a vibration mill.
The above examples are only partial embodiments of the present invention, and those skilled in the art can make routine changes based on the spirit of the present invention, and also fall into the protection scope of the present invention.
Claims (6)
1. A preparation method of nano calcium tungstate is characterized by comprising the following steps:
(1) weighing tungstate and calcium chloride according to the preparation amount and the stoichiometric ratio;
(2) putting the reactant weighed in the step (1) into a ball mill for ball milling for 1-3 hours, and taking out a ball milling product and a grinding ball;
(3) and (3) washing, filtering and drying the ball-milled product obtained in the step (2) to obtain the nano calcium tungstate.
2. The method according to claim 1, wherein the calcium chloride in the step (1) is calcium chloride dihydrate or anhydrous calcium chloride.
3. The method according to claim 1, wherein the tungstate in step (1) is one or more of alkali tungstate, ammonium paratungstate, and ammonium metatungstate.
4. The method according to claim 1, wherein the ball mill in the step (2) is a planetary ball mill, a stirring mill, a roller ball mill or a vibration mill.
5. The preparation method according to claim 1, wherein the material of the ball milling pot in the step (2) is yttrium zirconium oxide ceramic, stainless steel, agate, corundum, tungsten carbide, polytetrafluoroethylene or nylon, and the material of the grinding ball is yttrium zirconium oxide ceramic, stainless steel, agate, corundum or tungsten carbide.
6. The method according to claim 1, wherein the drying in the step (3) is carried out in a forced air oven at 40 to 100 ℃ for 1 to 4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010927457.2A CN111892090A (en) | 2020-09-07 | 2020-09-07 | Preparation method of nano calcium tungstate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010927457.2A CN111892090A (en) | 2020-09-07 | 2020-09-07 | Preparation method of nano calcium tungstate |
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| CN111892090A true CN111892090A (en) | 2020-11-06 |
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| CN202010927457.2A Pending CN111892090A (en) | 2020-09-07 | 2020-09-07 | Preparation method of nano calcium tungstate |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101224906A (en) * | 2008-02-01 | 2008-07-23 | 福建金鑫钨业有限公司 | Method for preparing low apparent density wolframic acid |
| CN102701282A (en) * | 2012-05-14 | 2012-10-03 | 无锡润鹏复合新材料有限公司 | Preparation method of CaWO4 hollow spheres |
| CN102718262A (en) * | 2012-03-02 | 2012-10-10 | 河北联合大学 | Preparation of nanowire assembled calcium tungstate spherical structure |
| CN103418370A (en) * | 2013-09-05 | 2013-12-04 | 桂林理工大学 | Visible-light responsive photocatalyst Ca3WO6 and preparing method thereof |
| CN106007713A (en) * | 2016-07-08 | 2016-10-12 | 天津大学 | High-quality-factor calcium tungstate series microwave dielectric ceramic |
| WO2016187993A1 (en) * | 2015-05-22 | 2016-12-01 | 北京赛科康仑环保科技有限公司 | Method for recovering and disposing waste scr denitrification catalyst |
-
2020
- 2020-09-07 CN CN202010927457.2A patent/CN111892090A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101224906A (en) * | 2008-02-01 | 2008-07-23 | 福建金鑫钨业有限公司 | Method for preparing low apparent density wolframic acid |
| CN102718262A (en) * | 2012-03-02 | 2012-10-10 | 河北联合大学 | Preparation of nanowire assembled calcium tungstate spherical structure |
| CN102701282A (en) * | 2012-05-14 | 2012-10-03 | 无锡润鹏复合新材料有限公司 | Preparation method of CaWO4 hollow spheres |
| CN103418370A (en) * | 2013-09-05 | 2013-12-04 | 桂林理工大学 | Visible-light responsive photocatalyst Ca3WO6 and preparing method thereof |
| WO2016187993A1 (en) * | 2015-05-22 | 2016-12-01 | 北京赛科康仑环保科技有限公司 | Method for recovering and disposing waste scr denitrification catalyst |
| CN106007713A (en) * | 2016-07-08 | 2016-10-12 | 天津大学 | High-quality-factor calcium tungstate series microwave dielectric ceramic |
Non-Patent Citations (1)
| Title |
|---|
| 程琳: "高能球磨法制备硅酸镁、钨酸盐纳米粉体及其陶瓷微波介电性能的研究", 《工程科技Ⅰ辑》 * |
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Address after: 341000 second floor of standard workshop, building 17, Jinling science and Technology Park, Ganzhou economic and Technological Development Zone, Ganzhou City, Jiangxi Province Applicant after: Jiangxi Shanna New Material Technology Co.,Ltd. Address before: 341000 second floor of standard workshop, building 17, Jinling science and Technology Park, Ganzhou economic and Technological Development Zone, Nanchang City, Jiangxi Province Applicant before: Jiangxi Shanna New Material Technology Co.,Ltd. |
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Application publication date: 20201106 |