CN202688007U - High-purity ammonium paratungstate preparation system - Google Patents
High-purity ammonium paratungstate preparation system Download PDFInfo
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- CN202688007U CN202688007U CN 201220212089 CN201220212089U CN202688007U CN 202688007 U CN202688007 U CN 202688007U CN 201220212089 CN201220212089 CN 201220212089 CN 201220212089 U CN201220212089 U CN 201220212089U CN 202688007 U CN202688007 U CN 202688007U
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Abstract
The utility model relates to a high-purity ammonium paratungstate preparation system which is characterized by comprising an ammonium paratungstate feeding bin, a calcining furnace, a tungsten trioxide bin, a tungsten trioxide dissolver, an ammonium tungstate solution filter, an ammonium tungstate solution storage tank, an ammonium tungstate evaporating crystallizer, an ammonium paratungstate crystal and crystallized mother liquor separator, an ammonium paratungstate crystal dryer, a high-purity ammonium paratungstate mixing bin, and a high-purity ammonium paratungstate product container, wherein the ammonium paratungstate feeding bin is used for containing preparation raw materials; the calcining furnace is used for calcining the preparation raw materials; produced tungsten trioxide is subjected to ammonia dissolving by the tungsten trioxide dissolver, and the ammonium tungstate solution storage tank is used for containing ammonium tungstate solution; the ammonium tungstate evaporating crystallizer is used for evaporating and crystallizing the generated ammonium tungstate solution; and the high-purity ammonium paratungstate product container is used for containing obtained high-purity ammonium paratungstate. Through the high-purity ammonium paratungstate preparation system, the processes of the high-purity APT (ammonium paratungstate) production technology are optimized, the quality of products is improved, and the production cost of the high-purity APT products is lowered.
Description
Technical field
The utility model relates to a kind of system that produces of high-purity ammonium paratungstate.
In this manual, term " ammonium paratungstate " is also referred to as APT.
In this manual, term " APT raw material " refers to GB zero level product APT.
In this manual, term " unacceptable product APT " is being commonly called as of APT product of exceeding standard of APT waste material, dirty material and various impurity etc.
In this manual, term " high-purity ammonium paratungstate " refers to that total impurities can be controlled in≤ammonium paratungstate within the 65ppm, i.e. the high-purity ammonium paratungstate of low impurity content, and GB zero level ammonium paratungstate product standard is total impurities≤177.5ppm.
In this manual, term " is produced raw material " and refers to that ion exchange method or extraction process produce reaches 0 grade of APT of GB (content of impurities≤177.5ppm) or the defective APT that produces in the production process (content of impurities 〉=177.5ppm).
In this manual, term " is metered in the evaporative crystallization pot " and refers to the volume size according to the evaporative crystallization pot, and the solution of metering certain volume is in the evaporative crystallization pot.
In this manual, the proportion size of surplus solution in evaporative crystallizer when term " evaporative crystallization terminal point proportion " refers to the evaporative crystallization end, the g/cm of unit
3
In this manual, a technics in the ion exchange process " used the ammonium salt desorb " and be in term, refers to that the resin that adsorbs tungsten escapes the tungsten in the resin with ammonium salt, becomes the process of ammonium tungstate solution.
In this manual, term " the first liquid-solid ratio " refers to that liquid-solid ratio is 2: 1-6: 1ml/g; And term " the second liquid-solid ratio " refers to that liquid-solid ratio is 2: 1-5: 1ml/g.
In this manual, term " the first ammonia concn " refers to that ammonia concn is 50-160g/l; And term " the second ammonia concn " refers to that ammonia concn is 60-150g/l.
Background technology
Tungsten is a kind of non-ferrous metal of infusibility, also is a kind of important strategic resource, is used widely because it has the premium propertiess such as fusing point is high, hardness is large, ductility is strong, wear-resisting and corrosion-resistant.
At present, the production of domestic APT mainly is ion exchange method and extraction process.
Ion exchange method is produced APT and is mainly used in wolframite, sheelite production APT.Alkali by the black and white tungsten ore decomposes the generation sodium tungstate solution; By ion exchange resin tungsten is adsorbed afterwards to a certain extent through the sodium wolframate thin up again, obtain ammonium tungstate solution with the ammonium salt desorb afterwards; The steam heated system of ammonium tungstate solution evaporates part water and ammonia obtains the ammonium paratungstate product.
Extraction process is produced APT and is mainly used in wolframite, sheelite, the assorted ore deposit of tungsten, reaches tungsten waste material production APT.By the assorted ore deposit of black and white tungsten ore, tungsten, and the roasting of tungsten waste material elder generation after again alkali decompose and generate sodium tungstate solution; Filter through removal of impurities again; The sodium tungstate solution that removal of impurities is good obtains ammonium tungstate solution through extraction and after stripping; Ammonium tungstate solution obtains the ammonium paratungstate product through evaporative crystallization again.
Two kinds of explained hereafter APT quality product out is generally GB zero level product, and all the other are GB first grade or unacceptable product.
Simultaneously, the unacceptable product APT that the APT that the APT waste material that ion exchange method and extraction process all can produce in process of production, dirty material and various impurity exceed standard etc. is commonly called as, this class APT mainly is to turn to by alkali dissolution to produce the sodium tungstate solution operation by traditional technology again, obtain general ammonium paratungstate product for ammonium tungstate solution by evaporative crystallization transition again.This technical process is long, the rate of recovery is low, production cost is high, and quality product belongs to and is generally GB zero level product or below the GB zero level product.
Also have the direct ammonia solvent of people APT on probation to generate ammonium tungstate, the ammonium tungstate solution evaporative crystallization obtains high-purity APT.There are two molten poor effect of the direct ammonia of problem: the one, APT in this system, APT dissolution process low conversion rate, and resulting ammonium tungstate solution concentration is also low; The 2nd, low-quality APT affects the quality of final APT product without effectively removal of impurities of calcining.
Along with the development of tungsten industry, more and more can not satisfy the needs of the high-quality tungsten deep processed product of production with the ammonium paratungstate product of existing ion-exchange, extraction process production.Such as used ammonium para-tungstate crystal powder such as the deep processed product of the high-quality tungsten of existing production and Wimet, most of single impurity content must be less than 1-5 * 10
-6The quality of ammonium paratungstate directly affects the quality of follow-up tungsten deep processed product, therefore wants the high purity ammonium paratungstate could satisfy the needs that modern industry is produced.
The utility model content
The purpose of this utility model provides a kind of system that produces of high-purity ammonium paratungstate, but its optimization production APT technological process, the high-purity ammonium paratungstate of acquisition low impurity content.
For this reason, the utility model provides a kind of system that produces of high-purity ammonium paratungstate, it is characterized in that, this system comprises the ammonium paratungstate feed hopper successively, calcining furnace, the tungstic oxide feed bin, the tungstic oxide dissolver, the ammonium tungstate solution strainer, the ammonium tungstate solution storage tank, the ammonium tungstate evaporative crystallizer, order of ammoniumparatungstate crystal and crystalline mother solution separator, the order of ammoniumparatungstate crystal moisture eliminator, the high-purity ammonium paratungstate blending bunker, and the container of high-purity ammonium paratungstate product, described ammonium paratungstate feed hopper holds produces raw material, and this produces the APT that reaches the content of impurities 〉=177.5ppm that produces in 0 grade of APT of GB or the production process that raw material comprises the content of impurities≤177.5ppm that produces with ion exchange method or extraction process; Raw material is produced in described calcining furnace calcining, and described tungstic oxide feed bin holds the tungstic oxide that generates; The tungstic oxide that described tungstic oxide dissolver ammonia dissolving is produced, described ammonium tungstate solution storage tank holds the ammonium tungstate solution through described ammonium tungstate solution strainer; Described ammonium tungstate evaporative crystallizer carries out evaporative crystallization to the ammonium tungstate solution that generates; Described order of ammoniumparatungstate crystal and crystalline mother solution separator, described order of ammoniumparatungstate crystal and crystalline mother solution separator fractional crystallization mother liquor and order of ammoniumparatungstate crystal, described order of ammoniumparatungstate crystal moisture eliminator are to remove the too much moisture content of ammonium paratungstate after the filtration, container that described high-purity ammonium paratungstate blending bunker is the high-purity ammonium paratungstate container that mixes different small batches, described high-purity ammonium paratungstate product to hold the high-purity ammonium paratungstate that obtains after mixing.
Preferably, described ammonium paratungstate feed hopper also holds APT waste material, dirty material.
Preferably, described calcining furnace is provided with the controller that inlet amount is 50-250kg/h, and calcining temperature is at 500-700 ℃ controller, and produces the transformation efficiency of raw material when tungstic oxide is produced in calcining and be at least 98.5% controller.
Preferably, be provided with the controller that described inlet amount is 100-200kg/h, and calcining temperature is 550-690 ℃ controller.
Preferably, it is 50-110 ℃ controller that described tungstic oxide dissolver is provided with solution temperature, and liquid-solid ratio is 2: the controller of 1-6: 1ml/g, the reaction times is the controller of 0.5-3h, and ammonia concn is the controller of 50-160g/l.
Preferably, be provided with described solution temperature and be 60-100 ℃ controller, liquid-solid ratio is 2: the controller of 1-5: 1ml/g, the reaction times is the controller of 1-2h, and ammonia concn is the controller of 60-150g/l.
Preferably, to be provided with pressure be 1-4kgf/cm to described ammonium tungstate evaporative crystallizer
2Controller, when evaporative crystallization finishes in the evaporative crystallizer proportion of surplus solution be 1.01-1.10g/cm
3Controller.
The principal feature of native system is, utilizes existing explained hereafter general APT out or the APT of underproof APT high-purity, is the process of a purification, and highly purified APT satisfies follow-up APT deep processing, produces high-quality tungsten product.
According to the utility model, produce the again system of ammonia dissolving of tungstic oxide by the APT calcining, efficiently solve the bad difficult problem of the direct ammonia dissolution process of APT solute effect; The APT calcination process has more effectively been removed the part troublesome impurity, has created condition for producing high-purity APT product.
The utility model has solved returns the main flow old technology after low-quality APT adopts alkali dissolution, has improved the rate of recovery of production process, has reduced production cost, but the high-purity APT product of while output.
Description of drawings
Fig. 1 is the schematic diagram according to the system that produces of high-purity ammonium paratungstate of the present utility model.
Embodiment
The utility model has been put forward the system for a kind of high purity ammonium paratungstate, take APT or unacceptable product APT as raw material, generates tungstic oxide by the APT calcining; The dissolving of tungstic oxide ammonia generates ammonium tungstate solution; The ammonium tungstate solution evaporative crystallization; APT oven dry, screening obtain high-purity APT, it is characterized in that: the APT calcining generates the tungstic oxide process, by control inlet amount control 50-250kg/h, calcining temperature is controlled at atmosphere in the 500-700 ℃ of stove, guarantees that the transformation efficiency of APT when tungstic oxide is produced in calcining reaches more than 98.5%.The preferred 100-200kg/h of inlet amount, the preferred 550-690 of calcining temperature ℃.In tungstic oxide ammonia dissolution process, the solution temperature during dissolving is controlled at 50-110 ℃, and liquid-solid ratio is controlled at 2: 1-6: 1ml/g, the reaction times is at 0.5-3h, ammonia concn 50-160g/l.The preferred 60-100 of temperature ℃, liquid-solid ratio preferred 2: 1-5: 1ml/g, preferred 1-2h of reaction times, the preferred 60-150g/l of ammonia concn.The ammonium tungstate solution of dissolving gained is metered into and carries out evaporative crystallization in the evaporative crystallization pot after filtering, and control evaporative crystallization steam is at 1-4kgf/cm
2, evaporative crystallization terminal point specific gravity control is at 1.01-1.10g/cm
3Obtain wet ammonium paratungstate.Wet ammonium paratungstate is removed excessive moisture by steam seasoning, to obtain the high-purity ammonium paratungstate product.
Fig. 1 shows the system of the major equipment composition that adopts in the technical process of high purity ammonium paratungstate.This system comprises successively: the container of ammonium paratungstate feed hopper 1, calcining furnace 2, tungstic oxide feed bin 3, tungstic oxide dissolver 4, ammonium tungstate solution strainer 5, ammonium tungstate solution storage tank 6, ammonium tungstate evaporative crystallizer 7, order of ammoniumparatungstate crystal and crystalline mother solution separator 8, order of ammoniumparatungstate crystal moisture eliminator 9, high-purity ammonium paratungstate blending bunker 10 and high-purity ammonium paratungstate product 11.
1, the APT calcining generates the tungstic oxide process.APT is inserted in the feeding warehouse, quantitatively at the uniform velocity APT is sent in the rotary kiln by screw feeder, temperature and atmosphere in the control rotary kiln, inlet amount 150kg/h, calcining temperature one is with 550 ℃, two to be with 640 ℃, three to be with 680 ℃.The transformation efficiency that changes into tungstic oxide through APT after the rotary kiln calcining reaches 98.85%.
2, tungstic oxide ammonia dissolution process, 150g/l ammonia soln temperature is controlled at 95 ℃, and liquid-solid ratio is controlled at 3: 1ml/g, add the tungstic oxide limit and stir, the reaction times obtains ammonium tungstate solution behind 1.5h, and filters.
3, ammonium tungstate solution is metered into and carries out evaporative crystallization in the evaporative crystallization pot after filtering, and control evaporative crystallization steam is at 1-4kgf/cm
2, when solution proportion near 1.05 the time, stopped heating carries out crystal and separates with mother liquor, obtains moisture ammonium paratungstate.
4, moisture ammonium paratungstate is removed excessive moisture by steam seasoning, to obtain the high-purity ammonium paratungstate product.
Embodiment 2
1, the APT calcining generates the tungstic oxide process.APT is inserted in the feeding warehouse, quantitatively at the uniform velocity APT is sent in the rotary kiln by screw feeder, temperature and atmosphere in the control rotary kiln, inlet amount 160kg/h, calcining temperature calcining temperature one is with 560 ℃, two to be with 650 ℃, three to be with 690 ℃.The transformation efficiency that changes into tungstic oxide through APT after the rotary kiln calcining reaches 99.05%.
2, tungstic oxide ammonia dissolution process, concentration are that 70g/l ammonia soln temperature is controlled at 100 ℃, and liquid-solid ratio is controlled at 4: 1ml/g, add tungstic oxide, and stir on the limit, and the reaction times obtains ammonium tungstate solution behind 2h, and filters.
3, ammonium tungstate solution is metered into and carries out evaporative crystallization in the evaporative crystallization pot after filtering, and control evaporative crystallization steam is at 1-4kgf/cm
2, when solution proportion near 1.06 the time, stopped heating carries out crystal and separates with mother liquor, obtains moisture ammonium paratungstate.
4, moisture ammonium paratungstate is removed excessive moisture by steam seasoning, to obtain the high-purity ammonium paratungstate product.
Table 1 is the quality contrast table of the high-purity ammonium paratungstate of zero level ammonium paratungstate and low impurity content.
Table 1
The system that produces according to a kind of high-purity ammonium paratungstate of the present utility model, can obtain nonferrous metal product--the high-purity ammonium paratungstate of low impurity content, its foreign matter content is low, and its total impurities is less than≤65ppm, can be used for producing the deep processed product such as tungsten powder, tungstenalloy of high-quality low impurity content.The high purity ammonium paratungstate is take APT as raw material, generates tungstic oxide by (1) APT calcining; (2) the tungstic oxide ammonia solvent generates ammonium tungstate; (3) the ammonium tungstate solution evaporative crystallization obtains APT; (4) APT oven dry, screening obtain high-purity APT ammonium paratungstate.
Claims (6)
1. the system that produces of a high-purity ammonium paratungstate, it is characterized in that, this system comprises the container of ammonium paratungstate feed hopper, calcining furnace, tungstic oxide feed bin, tungstic oxide dissolver, ammonium tungstate solution strainer, ammonium tungstate solution storage tank, ammonium tungstate evaporative crystallizer, order of ammoniumparatungstate crystal and crystalline mother solution separator, order of ammoniumparatungstate crystal moisture eliminator, high-purity ammonium paratungstate blending bunker and high-purity ammonium paratungstate product successively
Described ammonium paratungstate feed hopper is to hold the device of producing raw material;
Raw material is produced in described calcining furnace calcining, and described tungstic oxide feed bin holds the tungstic oxide that generates;
The tungstic oxide that described tungstic oxide dissolver ammonia dissolving is produced, described ammonium tungstate solution storage tank holds the ammonium tungstate solution through described ammonium tungstate solution strainer;
Described ammonium tungstate evaporative crystallizer carries out evaporative crystallization to the ammonium tungstate solution that generates;
Described order of ammoniumparatungstate crystal and crystalline mother solution separator fractional crystallization mother liquor and order of ammoniumparatungstate crystal;
Described order of ammoniumparatungstate crystal moisture eliminator is removed the too much moisture content of ammonium paratungstate after the filtration;
Described high-purity ammonium paratungstate blending bunker is for mixing the high-purity ammonium paratungstate container of different small batches;
The container of described high-purity ammonium paratungstate product holds and mixes the rear high-purity ammonium paratungstate that obtains.
2. the system that produces of high-purity ammonium paratungstate according to claim 1, it is characterized in that: described calcining furnace is provided with the controller that inlet amount is 50-250kg/h, calcining temperature is at 500-700 ℃ controller, and produces the transformation efficiency of raw material when tungstic oxide is produced in calcining and be at least 98.5% controller.
3. the system that produces of high-purity ammonium paratungstate according to claim 3 is characterized in that: be provided with the controller that described inlet amount is 100-200kg/h, and calcining temperature is 550-690 ℃ controller.
4. the system that produces of high-purity ammonium paratungstate according to claim 1, it is characterized in that: it is 50-110 ℃ controller that described tungstic oxide dissolver is provided with solution temperature, the first liquid-solid ratio controller, the reaction times is the controller of 0.5-3h, and the first ammonia concn controller.
5. the system that produces of high-purity ammonium paratungstate according to claim 5 is characterized in that: be provided with described solution temperature and be 60-100 ℃ controller, and the second liquid-solid ratio controller, the reaction times is the controller of 1-2h, and the second ammonia concn controller.
6. the system that produces of high-purity ammonium paratungstate according to claim 1, it is characterized in that: it is 1-4kgf/cm that described ammonium tungstate evaporative crystallizer is provided with pressure
2Controller, when evaporative crystallization finishes in the evaporative crystallizer proportion of surplus solution be 1.01-1.10g/cm
3Controller.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265080A (en) * | 2013-06-04 | 2013-08-28 | 广东翔鹭钨业股份有限公司 | Method for producing high-purity ammonium paratungstate from tungsten waste |
| CN103302299A (en) * | 2013-06-20 | 2013-09-18 | 安泰科技股份有限公司 | Preparation method of high-purity tungsten powder for large-scale integrated circuit |
| CN104909410A (en) * | 2015-06-18 | 2015-09-16 | 江西稀有金属钨业控股集团有限公司 | Preparation method of low-specific-surface tungsten trioxide |
| CN105016393A (en) * | 2015-08-07 | 2015-11-04 | 江西稀有金属钨业控股集团有限公司 | System and method for preparing blue tungsten high in specific surface area |
| CN109622989A (en) * | 2019-02-26 | 2019-04-16 | 江钨世泰科钨品有限公司 | A kind of preparation method of high-purity homogeneous needle-shaped purple tungsten powder |
-
2012
- 2012-05-11 CN CN 201220212089 patent/CN202688007U/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265080A (en) * | 2013-06-04 | 2013-08-28 | 广东翔鹭钨业股份有限公司 | Method for producing high-purity ammonium paratungstate from tungsten waste |
| CN103302299A (en) * | 2013-06-20 | 2013-09-18 | 安泰科技股份有限公司 | Preparation method of high-purity tungsten powder for large-scale integrated circuit |
| CN103302299B (en) * | 2013-06-20 | 2016-03-02 | 安泰科技股份有限公司 | A kind of preparation method of large scale integrated circuit high purity tungsten |
| CN104909410A (en) * | 2015-06-18 | 2015-09-16 | 江西稀有金属钨业控股集团有限公司 | Preparation method of low-specific-surface tungsten trioxide |
| CN105016393A (en) * | 2015-08-07 | 2015-11-04 | 江西稀有金属钨业控股集团有限公司 | System and method for preparing blue tungsten high in specific surface area |
| CN109622989A (en) * | 2019-02-26 | 2019-04-16 | 江钨世泰科钨品有限公司 | A kind of preparation method of high-purity homogeneous needle-shaped purple tungsten powder |
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