CN107720823A - The preparation method of nanoscale Zinc vanadate - Google Patents
The preparation method of nanoscale Zinc vanadate Download PDFInfo
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- CN107720823A CN107720823A CN201711114937.1A CN201711114937A CN107720823A CN 107720823 A CN107720823 A CN 107720823A CN 201711114937 A CN201711114937 A CN 201711114937A CN 107720823 A CN107720823 A CN 107720823A
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- preparation
- vanadate
- zinc
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- zinc sulfate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to the preparation method of nanoscale Zinc vanadate, belongs to vanadium technical field of fine.The technical problems to be solved by the invention are to provide the preparation method of nanoscale Zinc vanadate, and this method is that ammonium poly-vanadate is bonding agent using more potassium vanadates and zinc sulfate as raw material.Nanoscale Zinc vanadate can be prepared using the inventive method, and product purity is more than 99.5%.The inventive method technique is simple, wide adaptation range, cost are low, has very high Social benefit and economic benefit.
Description
Technical field
The present invention relates to the preparation method of nanoscale Zinc vanadate, belongs to vanadium technical field of fine.
Background technology
In recent years, Zinc vanadate micro/nano material is due to the nano effect dramatically different with traditional body phase material, and
There is the application prospect of light in the fields such as catalysis oxidation, luminescence generated by light and energy storage.For above-mentioned advantage, develop novel system
Preparation Method, and its relative growth mechanism is studied, so as to control thing phase, pattern, dimension and the size of product, to realizing such material
Comprehensive utilization it is significant.At present, have been reported that using high temperature solid-state method and hydrothermal synthesis method prepare metal Zinc vanadate it is micro-/
Nano material.
《The preparation and surface characteristic research of nanometer Zinc vanadate》Using hydrothermal synthesis method, using zinc nitrate and sodium metavanadate as original
Material, studied preparing nanoscale Zinc vanadate, as a result successfully synthesize Zinc vanadate, and by ESEM to synthesis
Zinc vanadate material surface pattern is observed.
Patent CN103130277A provides one kind using zinc acetate, sodium vanadate as raw material, and water is solvent, and zinc metal sheet serves as a contrast for deposition
Bottom, the method for preparing zinc vanadate nanorod.This method reduces postprocessing working procedures, preparation process without using surfactant
Simply, raw material and preparation process are environmentally safe, meet the industrialized production of environmental requirement.
The content of the invention
It is an object of the invention to provide the preparation method of nanoscale Zinc vanadate.
The invention provides the preparation method of nanoscale Zinc vanadate, using more potassium vanadates and zinc sulfate as raw material, ammonium poly-vanadate
For bonding agent.
Further, described preparation method comprises the following steps:A, more potassium vanadates, zinc sulfate and ammonium poly-vanadate are dissolved
Yu Shuizhong is reacted, and reaction is filtered after terminating;B, filtrate is reacted at 90~200 DEG C under conditions of 0.2~2Mpa, after reaction terminates
Filtering, filter cake is collected, is produced.
Further, the molar ratio of more potassium vanadates and zinc sulfate is (1:2)~(1:5).
Preferably, the molar ratio of more potassium vanadates and zinc sulfate is (1:2)~(1:4).
Further, the molar ratio of more potassium vanadates and ammonium poly-vanadate is (1:0.1)~(1:0.01).
Further, the solid volume ratio of step a liquid is (2:1)~(10:1).
Further, the temperature of step a reactions is 40 DEG C~100 DEG C;Preferably, temperature is 80 DEG C~100 DEG C.
Further, the step a reaction time is 40~80min.
Further, the time of step b reactions is 40min~10h;Preferably, 40~100min.
The invention provides the preparation method of nanoscale Zinc vanadate, this method is more using more potassium vanadates and zinc sulfate as raw material
Ammonium vanadate is bonding agent, nanoscale Zinc vanadate can be prepared, and product purity is more than 99.5%.The letter of the inventive method technique
List, wide adaptation range, cost are low, have very high Social benefit and economic benefit
Embodiment
The raw material that is used in the specific embodiment of the invention, equipment are known product, are obtained by buying commercially available prod.
Embodiment 1 prepares nanoscale Zinc vanadate using the inventive method
Take the more potassium vanadates of 1mol, 2mol zinc sulfate, 0.01mol ammonium poly-vanadate to be well mixed, add the pure of 2 times of volumes
Water, 90 DEG C are heated to, react 40min, filter off except insoluble impurities.
Mixed solution is added in high-temperature high-pressure reaction kettle, controlling reaction temperature be 200 DEG C, reaction pressure adjust to
0.2Mpa, reacts 100min, filtering, and filter cake dries 2h in 100 DEG C of baking oven, produces nanoscale Zinc vanadate.
Embodiment 2 prepares nanoscale Zinc vanadate using the inventive method
Take the more potassium vanadates of 1mol, 4mol zinc sulfate, 0.1mol ammonium poly-vanadate to be well mixed, add the pure of 10 times of volumes
Water, 100 DEG C are heated to, react 60min, filter off except insoluble impurities.
Mixed solution is added in high-temperature high-pressure reaction kettle, controlling reaction temperature be 100 DEG C, reaction pressure adjust to
2Mpa, reacts 40min, filtering, and filter cake dries 10h in 90 DEG C of baking oven, produces nanoscale Zinc vanadate.
Embodiment 3 prepares nanoscale Zinc vanadate using the inventive method
Take the more potassium vanadates of 1mol, 3mol zinc sulfate, 0.05mol ammonium poly-vanadate to be well mixed, add the pure of 10 times of volumes
Water, 80 DEG C are heated to, react 80min, filter off except insoluble impurities.
Mixed solution is added in high-temperature high-pressure reaction kettle, controlling reaction temperature be 90 DEG C, reaction pressure adjust to
1Mpa, reacts 80min, filtering, and filter cake dries 5h in 80 DEG C of baking oven, produces nanoscale Zinc vanadate.
Claims (8)
1. the preparation method of nanoscale Zinc vanadate, it is characterized in that:Using more potassium vanadates and zinc sulfate as raw material, ammonium poly-vanadate is combination
Agent.
2. preparation method as claimed in claim 1, it is characterized in that:Comprise the following steps:A, by more potassium vanadates, zinc sulfate and more
Ammonium vanadate is dissolved in the water reaction, and reaction is filtered after terminating;B, filtrate is reacted at 90~200 DEG C under conditions of 0.2~2Mpa,
Reaction is filtered after terminating, and is collected filter cake, is produced.
3. preparation method as claimed in claim 1 or 2, it is characterized in that:The molar ratio of more potassium vanadates and zinc sulfate is (1:2)
~(1:5);Preferably, the molar ratio of more potassium vanadates and zinc sulfate is (1:2)~(1:4).
4. preparation method as claimed in claim 1 or 2, it is characterized in that:The molar ratio of more potassium vanadates and ammonium poly-vanadate is (1:
0.1)~(1:0.01).
5. preparation method as claimed in claim 2, it is characterized in that:The solid volume ratio of step a liquid is (2:1)~(10:1).
6. preparation method as claimed in claim 2, it is characterized in that:The temperature of step a reactions is 40 DEG C~100 DEG C;Preferably,
Temperature is 80 DEG C~100 DEG C.
7. preparation method as claimed in claim 2, it is characterized in that:The step a reaction time is 40~80min.
8. preparation method as claimed in claim 2, it is characterized in that:The time of step b reactions is 40min~10h;Preferably,
40~100min.
Priority Applications (1)
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CN201711114937.1A CN107720823A (en) | 2017-11-13 | 2017-11-13 | The preparation method of nanoscale Zinc vanadate |
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CN201711114937.1A CN107720823A (en) | 2017-11-13 | 2017-11-13 | The preparation method of nanoscale Zinc vanadate |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102140691A (en) * | 2011-02-12 | 2011-08-03 | 河北联合大学 | Method for synthesizing vanadium acid zinc micro/nanowire material by adopting hydrothermal method |
CN103130277A (en) * | 2013-02-28 | 2013-06-05 | 安徽工业大学 | Method for preparing zinc vanadate nanorod |
CN106186063A (en) * | 2016-07-20 | 2016-12-07 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of preparation method of nanoscale Zinc vanadate |
-
2017
- 2017-11-13 CN CN201711114937.1A patent/CN107720823A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102140691A (en) * | 2011-02-12 | 2011-08-03 | 河北联合大学 | Method for synthesizing vanadium acid zinc micro/nanowire material by adopting hydrothermal method |
CN103130277A (en) * | 2013-02-28 | 2013-06-05 | 安徽工业大学 | Method for preparing zinc vanadate nanorod |
CN106186063A (en) * | 2016-07-20 | 2016-12-07 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of preparation method of nanoscale Zinc vanadate |
Non-Patent Citations (1)
Title |
---|
王彦笛: "钒酸锌纳米材料的可控制备", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Application publication date: 20180223 |