CN112028122A - Microwave solid phase preparation method of nano calcium tungstate - Google Patents
Microwave solid phase preparation method of nano calcium tungstate Download PDFInfo
- Publication number
- CN112028122A CN112028122A CN202010927462.3A CN202010927462A CN112028122A CN 112028122 A CN112028122 A CN 112028122A CN 202010927462 A CN202010927462 A CN 202010927462A CN 112028122 A CN112028122 A CN 112028122A
- Authority
- CN
- China
- Prior art keywords
- tungstate
- putting
- microwave
- calcium chloride
- nano calcium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/126—Microwaves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Electromagnetism (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a microwave solid-phase 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 mixing device for premixing for 10 minutes; (3) putting the uniformly mixed materials in the step (2) into a crucible, putting the crucible into a microwave oven, and continuously reacting for 10-15 minutes; (4) and (4) taking out the product obtained in the step (3), 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 microwave radiation method, has the characteristics of low equipment requirement, short synthesis time, high synthesis yield, no additive, green and environment-friendly synthesis process and low 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 synthesized 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, the solid phase reaction method has 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, thereby arousing great research interest and becoming a new way for developing green chemistry and technology. The microwave radiation method is a technology which is applied to modern synthesis research by utilizing the characteristics of rapid heating, homogenization, selectivity and the like of the microwave radiation method under the condition of microwaves. The invention combines the advantages of the solid phase method and the microwave radiation method to realize the rapid preparation of the nano calcium tungstate, and the whole chemical reaction can be completed under the action of the microwave only by the self crystal water of the reactant without any solvent or additive in the preparation process. So far, no literature report is available for preparing the nano calcium tungstate material by combining a solid phase method and a microwave radiation method.
Disclosure of Invention
The invention aims to provide a solid-phase microwave preparation method of nano calcium tungstate, which takes common tungstate and calcium chloride as raw materials, obtains a reaction product through microwave irradiation, and can obtain the nano calcium tungstate with uniform size and good dispersibility through washing, filtering and drying.
The invention is realized by the following technical scheme.
A microwave solid phase preparation method of nano calcium tungstate 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 mixing device for premixing for 10 minutes;
(3) putting the uniformly mixed materials in the step (2) into a crucible, putting the crucible into a microwave reaction device, and heating for 10-15 minutes;
(4) and (4) taking out the product obtained in the step (3), and washing, filtering and drying to obtain the nano calcium tungstate powder.
More particularly, the calcium chloride in step (1) is calcium chloride dihydrate or anhydrous calcium chloride.
More particularly, the tungstate in the step (1) is one or more of alkali metal tungstate, ammonium paratungstate and ammonium metatungstate.
More particularly, the mixing device in the step (2) is a planetary ball mill, a stirring mill, a roller ball mill or a vibration mill.
More particularly, the microwave reaction device in the step (3) is a household or industrial microwave oven.
More particularly, the drying in the step (4) is carried out for 1-4 hours in a blast drying oven at 40-60 ℃.
The main advantages of the invention are: (1) the product calcium tungstate is white nano powder with small granularity, good dispersibility and uniform size; (2) the method takes common tungstate and calcium chloride as raw materials, prepares the nano calcium tungstate by a microwave radiation method, has the characteristics of low equipment requirement, short synthesis time, high synthesis yield and no additive, is green and environment-friendly in synthesis process and low in 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.
FIG. 3 SEM photograph of the sample of example 2.
Detailed Description
The invention will be further illustrated by the following examples.
A microwave solid phase preparation method of nano calcium tungstate comprises the following steps:
(1) weighing tungstate and calcium chloride according to the preparation amount and the stoichiometric ratio; the calcium chloride is calcium chloride dihydrate or anhydrous calcium chloride, and 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 mixing device for premixing for 10 minutes; the mixing device is a planetary ball mill, a stirring mill, a roller ball mill or a vibration mill. The microwave reaction device is a household or industrial microwave oven.
(3) Putting the uniformly mixed materials in the step (2) into a crucible, putting the crucible into a microwave reaction device, and heating for 10-15 minutes;
(4) and (4) taking out the product obtained in the step (3), washing, filtering, drying, and drying for 1-4 hours at 40-60 ℃ in a forced air drying oven to obtain the nano calcium tungstate powder.
Example 1
Accurately weighing 15g of sodium tungstate dihydrate and 10g of calcium chloride dihydrate, and putting the weighed reactants into a planetary ball mill for premixing for 10 minutes; then, the uniformly mixed materials are put into a crucible and put into a household microwave oven to continuously react for 15 minutes; and taking out the obtained product, washing, filtering and drying 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 of the sample shows that the calcium tungstate powder has small particle size and uniform dispersion as shown in FIG. 2.
Example 2
Accurately weighing 15g of ammonium paratungstate and 10g of anhydrous calcium chloride, and putting the weighed reactants into a planetary ball mill for premixing for 10 minutes; then, the uniformly mixed materials are put into a crucible and put into a household microwave oven for continuous reaction for 10 minutes; and taking out the obtained product, washing, filtering and drying to obtain the nano calcium tungstate powder. SEM analysis of the samples is shown in FIG. 3.
The mixing device in the invention can also be a stirring mill, a roller ball 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 microwave solid phase 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 mixing device for premixing for 10 minutes;
(3) putting the uniformly mixed materials in the step (2) into a crucible, putting the crucible into a microwave reaction device, and heating for 10-15 minutes;
(4) and (4) taking out the product obtained in the step (3), and washing, filtering and drying to obtain the nano calcium tungstate powder.
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 mixing device in step (2) is a planetary ball mill, a stirring mill, a roller ball mill or a vibration mill.
5. The method according to claim 1, wherein the microwave reactor in the step (3) is a household or industrial microwave oven.
6. The method according to claim 1, wherein the drying in the step (4) is carried out in a forced air oven at 40 to 60 ℃ for 1 to 4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010927462.3A CN112028122B (en) | 2020-09-07 | 2020-09-07 | Microwave solid phase preparation method of nano calcium tungstate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010927462.3A CN112028122B (en) | 2020-09-07 | 2020-09-07 | Microwave solid phase preparation method of nano calcium tungstate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112028122A true CN112028122A (en) | 2020-12-04 |
| CN112028122B CN112028122B (en) | 2023-01-31 |
Family
ID=73584851
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010927462.3A Active CN112028122B (en) | 2020-09-07 | 2020-09-07 | Microwave solid phase preparation method of nano calcium tungstate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112028122B (en) |
Citations (7)
| 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 |
| CN103771520A (en) * | 2014-01-24 | 2014-05-07 | 重庆文理学院 | Preparation method of twinborn spheroidal calcium tungstate microcrystallines |
| WO2016187994A1 (en) * | 2015-05-22 | 2016-12-01 | 北京赛科康仑环保科技有限公司 | Recycling and remanufacturing method for spent scr denitrification catalyst |
| CN106745275A (en) * | 2017-01-24 | 2017-05-31 | 南昌大学 | A kind of preparation method of hydration tungstic trioxide nano-slice |
| CN109607612A (en) * | 2018-12-24 | 2019-04-12 | 孙昕 | Vanadium in a kind of discarded SCR denitration, tungsten, titanium resource recycling method |
-
2020
- 2020-09-07 CN CN202010927462.3A patent/CN112028122B/en active Active
Patent Citations (7)
| 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 |
| CN103771520A (en) * | 2014-01-24 | 2014-05-07 | 重庆文理学院 | Preparation method of twinborn spheroidal calcium tungstate microcrystallines |
| WO2016187994A1 (en) * | 2015-05-22 | 2016-12-01 | 北京赛科康仑环保科技有限公司 | Recycling and remanufacturing method for spent scr denitrification catalyst |
| CN106745275A (en) * | 2017-01-24 | 2017-05-31 | 南昌大学 | A kind of preparation method of hydration tungstic trioxide nano-slice |
| CN109607612A (en) * | 2018-12-24 | 2019-04-12 | 孙昕 | Vanadium in a kind of discarded SCR denitration, tungsten, titanium resource recycling method |
Non-Patent Citations (1)
| Title |
|---|
| 米远祝等: "微波法合成红色长余辉磷光粉CaWO4∶Eu3+的研究", 《湖北民族学院学报》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112028122B (en) | 2023-01-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110451525B (en) | Method for rapidly preparing Prussian blue analogue with monoclinic crystal structure | |
| CN106881079B (en) | A kind of two dimensional oxidation tungsten/niobic acid tin nanometer sheet-piece composite material preparation method | |
| CN103265546B (en) | A kind of method without template synthesis azotized carbon nano fiber | |
| CN101746826B (en) | Method for preparing niobium pentoxide hollow nanosphere | |
| CN111790412A (en) | Method for producing carbon compound by reducing carbon dioxide | |
| CN107349943A (en) | The preparation method of bismuth stannate/silver-colored silver chlorate plasma nano composite photocatalyst material | |
| CN111057399B (en) | Preparation method of rare earth doped clay mineral-based bismuth yellow hybrid pigment with adjustable fluorescence and color | |
| CN109179349A (en) | A kind of Carbon Nitride Crystal and preparation method thereof | |
| CN112028122B (en) | Microwave solid phase preparation method of nano calcium tungstate | |
| CN108722486A (en) | A kind of preparation method of narrowband carbonitride modification ferrous metals organic backbone composite photo-catalyst | |
| CN100534908C (en) | Process for preparing In2O3 nano-wire | |
| CN103833086A (en) | Preparation method of flaky iron trioxide | |
| CN109264782A (en) | A kind of method that low pressure doping prepares pucherite | |
| CN103570031B (en) | Hydrothermal technique prepares BaCuSi 2o 6and BaCu 2si 2o 7the method of pigment | |
| CN100486901C (en) | Synthesis method of cobaltosic oxide nano-tube | |
| CN100487075C (en) | Method of preparing composite europium samarium stannate nano fluorescent powder | |
| CN105032471B (en) | A kind of visible light-responded nano-TiO2The preparation of/Zeolite composite materials | |
| CN108609658B (en) | Preparation method of reduced tungsten oxide/nitrogen-doped graphene compound | |
| CN114293321B (en) | Low-cost room-temperature rapid batch preparation method and equipment for special-shaped vanadium oxide nanofibers and aggregates thereof | |
| CN111892090A (en) | Preparation method of nano calcium tungstate | |
| CN105195145A (en) | Method of preparing PN heterogeneous composite photocatalyst | |
| CN102674459B (en) | Preparation method of flaky zinc molybdate microcrystal | |
| CN101402468A (en) | Method for producing monodisperse pulmbous sulfide nanospheres | |
| CN111569879A (en) | Method for preparing silicate/carbon composite material by using attapulgite and application thereof | |
| CN101580233A (en) | Method for synthesizing CdSe nanosphere |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
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. |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |