CN105819513A - Method utilizing cold wind aeration technology to produce ultrafine APT - Google Patents
Method utilizing cold wind aeration technology to produce ultrafine APT Download PDFInfo
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- CN105819513A CN105819513A CN201610153505.0A CN201610153505A CN105819513A CN 105819513 A CN105819513 A CN 105819513A CN 201610153505 A CN201610153505 A CN 201610153505A CN 105819513 A CN105819513 A CN 105819513A
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- Prior art keywords
- aeration
- cold wind
- apt
- ultra
- fine
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention provides a method utilizing a cold wind aeration technology to produce ultrafine APT. The method comprises the following steps: (1) pumping a high purity ammonium tungstate solution with a concentration of 170 to 190 g/L to a crystallization kettle; (2) pumping compressed gas into the crystallization kettle to carry out an aeration pretreatment, and closing compressed gas when WO3 concentration reaches 280 to 300 g/L; (3) starting an air cooler set, setting the temperature in a range of 5 to 10 DEG C, evenly pumping the cold air into solution to carry out aeration, starting a stirring apparatus, controlling the rotation speed in a range of 50 to 60 r/min, and stopping aeration when WO3 concentration reaches 40 to 50 g/L; (4) after aeration, pumping the feed liquor into a plate-and-frame filter press to carry out press-filtering, washing, drying the solids by air blowing, recovering the filtrate, and finally carrying out static baking to obtain ultrafine APT.
Description
Technical field
The present invention relates to chemical production technical field, be specifically related to a kind of method producing ultra-fine APT with cold wind aeration system.
Background technology
The hydrometallurgical processes of tungsten is produced the method for APT (ammonium paratungstate) by ammonium tungstate mainly have evaporative crystallization, neutralize crystallization, freezing and crystallizing three kinds.Wherein evaporative crystallization technique is the prevailing technology used in producing APT present stage, is primarily due to evaporative crystallization and has a low cost, simple to operate, and produces the steady quality of APT, the advantages such as granularity is the most uniform.Its granule size of APT prepared by this kind of method is generally 25～50 μm, and shape differs, and belongs to coarse grained APT, produces ultrafine tungsten powder, ultrafine tungsten carbide difficulty with this kind of APT bigger；Neutralize crystallization more greatly and to be seldom applied in commercial production because of environmental pollution；The investment of freezing and crystallizing equipment needed thereby is relatively big, and energy consumption is higher, is the most also rarely employed.
The patent of invention of Application No. CN201010537187.0, a kind of micron-class superfine ammonium paratungstate and preparation method thereof are the preparation method we providing a kind of ultra-fine APT, and the method is to add surfactant OA in ammonium tungstate evaporation and crystal process to promote ammonium tungstate to produce micron-class superfine.OA is a kind of oil substances, thus introduces new impurity in process of production, so it has to pass through the process of oil removing so that production procedure increases, and equipment increases, and energy consumption increases.Its Fisher particle size of APT produced by this technique is in 1～5 μm, and its apparent density is 0.5～0.6g/m3。
Summary of the invention
In order to solve problems of the prior art, the invention provides a kind of method producing ultra-fine APT with cold wind aeration system.
Technical scheme is as follows:
By blasting compressed gas bubbling in production, bubble is taken away aqueous vapor so that WO3Concentration raises, then blasts cold wind cooling, reduces molecular potential so that it is rate of crystalline growth slows down, and finally gives the ultra-fine APT that Fisher particle size is 0.5～5 μm, and ultra-fine APT crystal shape is needle-like, comprises the following steps:
Step is 1.: the high purity tungsten acid ammonium solution that concentration is 170～190g/L is pumped to crystallization kettle；
Step is 2.: carry out aeration pretreatment to blasting compressed gas in the crystallization kettle that step is 1. described, it is desirable to solution under aeration environment can uniform stirring, work as WO3When concentration reaches 280～300g/L, close compressed air；
Step is 3.: starting cold wind unit, temperature is set to 5～10 DEG C, is uniformly blasted by cold wind and carries out aeration in the solution that step is 2. described, starts agitating device, and rotating speed controls, 50～60r/min, to work as WO3When concentration reaches 40～50g/L, stop aeration；
Step is 4.: the feed liquid after step 3. aeration being pumped into and carry out filter pressing in filter press, wash, dry up, filtrate recycles, and last static drying obtains ultra-fine APT.
In order to prevent APT oxidized, the temperature of described step 2. middle compressed gas is less than 20 DEG C.
In order to more preferably produce ultra-fine APT, during described step 3. middle aeration, gas entrance flow direction is identical with mixing direction, and described compressed gas refers to the compressed air after oil removing, dedusting or compressed nitrogen or compressed inert.
Starting stirring during in order to ventilate also to stir under the effect of air-flow, described step 2. middle compressed gas enters solution by serpentine pipe.
The present invention has the advantage that relative to prior art
1, the present invention carries aqueous vapor condensing crystallizing, green, energy-saving and environmental protection with air for power and carrier.
2, the present invention is without any reagent in crystallization process, will not introduce new impurity.
3, the present invention crystallize that flow process is short, equipment is few, simple to operate.
Detailed description of the invention
Below in conjunction with embodiment, a kind of method with the cold wind aeration system ultra-fine APT of production of the present invention is described in further detail.
Embodiment 1:
Step is 1.: the high purity tungsten acid ammonium solution that concentration is 180g/L is pumped to crystallization kettle；
Step is 2.: carry out aeration pretreatment to blasting compressed gas in crystallization kettle, this compressed gas is the compressed air after oil removing, dedusting or compressed nitrogen or compressed inert, temperature is less than 20 DEG C, when blasting, compressed gas enters solution by serpentine pipe, require solution energy uniform stirring under aeration environment, work as WO3When concentration reaches 290g/L, close compressed air；
Step is 3.: starting cold wind unit, temperature is set to 7 DEG C, is uniformly blasted by cold wind and carries out aeration in solution, starts agitating device, and rotating speed controls at 55r/min, and during aeration, to enter flow direction identical with mixing direction for gas, works as WO3When concentration reaches 45g/L, stop aeration；
Step is 4.: the feed liquid after aeration being pumped in filter press and carry out filter pressing, wash, dry up, filtrate recycles, and last static drying obtains ultra-fine APT, and crystal shape is needle-like, and the Fisher particle size of ultra-fine APT is 0.5～5 μm.
Embodiment 2:
Step is 1.: the high purity tungsten acid ammonium solution that concentration is 185g/L is pumped to crystallization kettle；
Step is 2.: carry out aeration pretreatment to blasting compressed gas in crystallization kettle, this compressed gas is the compressed air after oil removing, dedusting or compressed nitrogen or compressed inert, temperature is less than 20 DEG C, when blasting, compressed gas enters solution by serpentine pipe, require solution energy uniform stirring under aeration environment, work as WO3When concentration reaches 295g/L, close compressed air；
Step is 3.: starting cold wind unit, temperature is set to 8 DEG C, is uniformly blasted by cold wind and carries out aeration in solution, starts agitating device, and rotating speed controls at 55r/min, and during aeration, to enter flow direction identical with mixing direction for gas, works as WO3When concentration reaches 45g/L, stop aeration；
Step is 4.: the feed liquid after aeration being pumped in filter press and carry out filter pressing, wash, dry up, filtrate recycles, and last static drying obtains ultra-fine APT, and crystal shape is needle-like, and the Fisher particle size of ultra-fine APT is 0.5～5 μm.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.
Claims (8)
1. the method producing ultra-fine APT with cold wind aeration system, it is characterised in that by blasting compressed gas bubbling in production, bubble is taken away aqueous vapor so that WO3Concentration raises, then blasts cold wind cooling, reduces molecular potential so that it is rate of crystalline growth slows down, and finally gives ultra-fine APT.
A kind of method producing ultra-fine APT with cold wind aeration system, it is characterised in that the Fisher particle size producing the ultra-fine APT of gained is 0.5～5 μm.
A kind of method producing ultra-fine APT with cold wind aeration system, it is characterised in that comprise the following steps:
Step is 1.: the high purity tungsten acid ammonium solution that concentration is 170～190g/L is pumped to crystallization kettle；
Step is 2.: carry out aeration pretreatment to blasting compressed gas in the crystallization kettle that step is 1. described, it is desirable to solution under aeration environment can uniform stirring, work as WO3When concentration reaches 280～300g/L, close compressed air；
Step is 3.: starting cold wind unit, temperature is set to 5～10 DEG C, is uniformly blasted by cold wind and carries out aeration in the solution that step is 2. described, starts agitating device, and rotating speed controls, 50～60r/min, to work as WO3When concentration reaches 40～50g/L, stop aeration；
Step is 4.: the feed liquid after step 3. aeration being pumped into and carry out filter pressing in filter press, wash, dry up, filtrate recycles, and last static drying obtains ultra-fine APT.
A kind of method producing ultra-fine APT with cold wind aeration system, it is characterised in that the temperature of described step 2. middle compressed gas is less than 20 DEG C.
A kind of method producing ultra-fine APT with cold wind aeration system, it is characterised in that during described step 3. middle aeration, gas entrance flow direction is identical with mixing direction.
A kind of method producing ultra-fine APT with cold wind aeration system, it is characterised in that described compressed gas refers to the compressed air after oil removing, dedusting or compressed nitrogen or compressed inert.
A kind of method producing ultra-fine APT with cold wind aeration system, it is characterised in that described step 2. middle compressed gas enters solution by serpentine pipe.
8. a kind of method producing ultra-fine APT with cold wind aeration system as described in any one of claim 1 to 7, it is characterised in that described ultra-fine APT crystal shape is needle-like.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610153505.0A CN105819513B (en) | 2016-03-17 | 2016-03-17 | A kind of method that ultra-fine APT is produced with cold wind aeration system |
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| CN201610153505.0A CN105819513B (en) | 2016-03-17 | 2016-03-17 | A kind of method that ultra-fine APT is produced with cold wind aeration system |
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| CN105819513A true CN105819513A (en) | 2016-08-03 |
| CN105819513B CN105819513B (en) | 2017-09-19 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108837551A (en) * | 2018-07-28 | 2018-11-20 | 湖南懋天世纪新材料有限公司 | A kind of ultra-fine ammonium paratungstate evaporated crystallization device and method for crystallising |
| CN109987632A (en) * | 2019-04-29 | 2019-07-09 | 江西省科学院应用物理研究所 | A kind of method that chemical precipitation method prepares ultra-fine ammonium paratungstate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963933A (en) * | 2012-12-01 | 2013-03-13 | 中南大学 | Preparation method of ammonium paratungstate |
| CN204162450U (en) * | 2014-10-09 | 2015-02-18 | 江西稀有金属钨业控股集团有限公司 | A kind of system preparing ammonium tungstate solution |
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2016
- 2016-03-17 CN CN201610153505.0A patent/CN105819513B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963933A (en) * | 2012-12-01 | 2013-03-13 | 中南大学 | Preparation method of ammonium paratungstate |
| CN204162450U (en) * | 2014-10-09 | 2015-02-18 | 江西稀有金属钨业控股集团有限公司 | A kind of system preparing ammonium tungstate solution |
Non-Patent Citations (1)
| Title |
|---|
| 陈启元等: "仲钨酸铵结晶制备进展", 《有色金属》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108837551A (en) * | 2018-07-28 | 2018-11-20 | 湖南懋天世纪新材料有限公司 | A kind of ultra-fine ammonium paratungstate evaporated crystallization device and method for crystallising |
| CN108837551B (en) * | 2018-07-28 | 2024-04-02 | 湖南懋天世纪新材料有限公司 | Superfine ammonium paratungstate evaporation crystallization device and crystallization method |
| CN109987632A (en) * | 2019-04-29 | 2019-07-09 | 江西省科学院应用物理研究所 | A kind of method that chemical precipitation method prepares ultra-fine ammonium paratungstate |
| CN109987632B (en) * | 2019-04-29 | 2020-08-07 | 江西省科学院应用物理研究所 | Method for preparing superfine ammonium paratungstate by chemical precipitation method |
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| CN105819513B (en) | 2017-09-19 |
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Denomination of invention: Method utilizing cold wind aeration technology to produce ultrafine APT Effective date of registration: 20200616 Granted publication date: 20170919 Pledgee: Huarong Bank of Xiangjiang Limited by Share Ltd. Yiyang branch Pledgor: HUNAN MAOTIAN SHIJIE NEW MATERIALS Co.,Ltd. Registration number: Y2020980003142 |