CN103523800A - Method for recovering excess sodium hydroxide in tungsten smelting crude sodium tungstate solution - Google Patents
Method for recovering excess sodium hydroxide in tungsten smelting crude sodium tungstate solution Download PDFInfo
- Publication number
- CN103523800A CN103523800A CN201310438500.9A CN201310438500A CN103523800A CN 103523800 A CN103523800 A CN 103523800A CN 201310438500 A CN201310438500 A CN 201310438500A CN 103523800 A CN103523800 A CN 103523800A
- Authority
- CN
- China
- Prior art keywords
- tungsten
- sodium tungstate
- sodium
- evaporation
- coarse
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for recovering excess sodium hydroxide in a tungsten smelting crude sodium tungstate solution. The method comprises the steps of mixing a tungsten ore raw material and water according to the volume ratio of 10: 3, then adding into a ball mill for ball milling to obtain tungsten ore slurry, adding a sodium hydroxide solution into the tungsten ore slurry to perform alkali autoclaving to obtain alkali autoclaved slurry, and performing pressure filtration on the alkali autoclaved slurry twice so as to obtain a crude sodium tungstate solution; pumping the crude sodium tungstate solution into a feeding and preheating device; enabling sodium tungstate crystal slurry obtained by separation after the well preheated crude sodium tungstate solution sequentially passes through a three-effect evaporation unit, a one-effect evaporation unit and a two-effect evaporation unit for evaporation and crystallization to enter a plate frame for pressure filtration so as to obtain a concentrated odium hydroxide solution and sodium tungstate crystals. The method disclosed by the invention has the advantages of high degree of automation, convenience in operation and capabilities of greatly reducing energy consumption, reducing later-stage wastewater neutralization control burden, reducing labor cost, reducing labor intensity and being easy to implement, and is in line with the national policies of reducing cost, increasing efficiency, saving energy and reducing emission.
Description
Technical field
The present invention relates to tungsten technical field of smelting, be mainly concerned with the recovery method that a kind of tungsten is smelted excess hydrogen sodium oxide in coarse sodium tungstate.
Background technology
Along with the continuous exploitation of tungsten ore resource, the especially high-grade wolframite reserves of tungsten concentrate are fewer and feweri, and the chats that white tungsten fine ore and foreign matter content are higher becomes the main source of tungsten raw materials for metallurgy in the future.In prior art, the smelting of white tungsten fine ore and chats generally adopts high basic pressure digestion technology, and throwing alkali number is generally 2.8～4 times of theoretical amount, superfluous NaOH and WO in the coarse sodium tungstate obtaining after the press filtration of basic pressure digestion slurry
3mass ratio reach 0.7～1.2, even higher, if do not reclaimed, not only subsequent handling is brought to disadvantageous effect, and finally also will consume after sulfuric acid neutralizes it and could discharge.No matter therefore from reduce starting material unit consumption, reduce production costs or have the necessity that reclaims superfluous NaOH tungsten smelting coarse sodium tungstate from the angle of environment protection, energy-saving and emission-reduction.
The recovery method that current tungsten is smelted superfluous NaOH in coarse sodium tungstate is mainly condensing crystal method, and the single-effect evaporation crystallizing pan steam indirect heating that adopts band to stir reaches the object of condensing crystal.Condensing crystal ratio juris is that the changes in solubility of sodium wolframate under different naoh concentrations is large, rising along with naoh concentration, the solubleness of sodium wolframate is successively decreased, so along with constantly concentrating of sodium hydroxide solution, it is more and more that sodium wolframate crystallization just occurs, thereby both are separated.Facts have proved, there is the problems such as energy consumption is high, efficiency is low, running cost is high, level of automation is low, environmental protection pressure is large in the recovery that adopts this original evaporation technique to carry out superfluous NaOH in tungsten smelting coarse sodium tungstate.
Chinese patent CN102963911A has announced a kind of method that sodium tungstate solution from tungsten is smelted reclaims remaining alkali, boiling still mixed liquor out by the filtrate the liquid-solid separation of pressure filter from pressing, with being pumped into triple effect evaporation crystallizer, first enter and in first preheating tube, carry out preheating, then enter an effect evaporative crystallizer, the secondary steam that one effect evaporation concentration produces is as the thermal source of two effect evaporation concentration, and the sodium wolframate crystal that two effect evaporative crystallizers are separated out send plate-and-frame filter press to carry out solid-liquid separation; Concentrated solution continues to enter in Three-effect concentration device, and the sodium wolframate crystal that triple effect evaporation crystallizer is separated out carries out solid-liquid separation through plate-and-frame filter press; The sodium wolframate crystal that two effect evaporative crystallizers and triple effect evaporation crystallizer are separated out together enters plate-and-frame filter press and carries out solid-liquid separation; Filtrate enters storage tank and presses boiling procedure to join alkali in order to return, and filter residue is discharged in dissolving tank.The weak point of the method is: the one, and the system of three-effect downstream evaporator technique adopting, larger than three-effect counter flow or triple effect mixed flow process energy consumption, for example basic industry is processed containing NaOH 125～135g/L, the solution of NaCl 190～210g/L is produced NaOH concentration while being 42～50% liquid caustic soda, adopt NaOH consumption steam per ton 3.5～3.8t of system of three-effect downstream evaporator, adopt NaOH consumption steam per ton 2.6～2.8t of three-effect counter flow/triple effect mixed flow evaporation, energy consumption significantly reduces than system of three-effect downstream evaporator; Two is that two effect evaporative crystallization sections have existed sodium wolframate crystal to separate out, though be furnished with brilliant mouthful, along with the rising of mixed liquid concentration, viscosity strengthens gradually, still easily causes the fouling of heating tube side, causes plugging to occur.
The inventive method adopts triple effect mixed flow method of evaporating to reclaim excess hydrogen sodium oxide in tungsten smelting coarse sodium tungstate, in triple effect evaporation and an effect evaporative process, sodium wolframate crystallization is considerably less, there will not be plugging phenomenon, not only reduced sodium hydroxide cost recovery, energy-conserving and environment-protective, and improved sodium wolframate percent crystallization in massecuite.
Summary of the invention
The object of the invention is the problem existing in order to solve above-mentioned prior art, and a kind of technique providing simple, be easy to realize, energy consumption is low, wide adaptability, tungsten that level of automation is high are smelted superfluous NaOH in coarse sodium tungstate recovery method.
The present invention is to disclose the recovery method that a kind of tungsten is smelted coarse sodium tungstate excess hydrogen sodium oxide for the technical scheme solving the problems of the technologies described above, and it is characterized in that, comprises the following steps:
Step 1, by tungsten ore raw material and water by volume 10:3 mix and add ball milling in ball mill to obtain tungsten ore slurry, in described tungsten ore slurry, add sodium hydroxide solution, described sodium hydroxide solution addition is that in described sodium hydroxide solution, sodium hydrate content is 1.0～1.4 times of tungstic oxide content in described tungsten ore raw material, the described tungsten ore stock pump that adds described sodium hydroxide solution is entered to be with in the middle pressure reactor stirring afterwards and carry out basic pressure digestion acquisition basic pressure digestion slurry, described basic pressure digestion slurry obtains coarse sodium tungstate after twice press filtration;
Step 2, described coarse sodium tungstate is sent in the reinforced primary heater unit of triple effect evaporation crystallizer through fresh feed pump, when described coarse sodium tungstate preheating temperature reaches the boiling temperature of triple effect evaporation modular heater, described coarse sodium tungstate pumps into the evaporation unit of triple effect evaporation unit, evaporation concentration is carried out vapor-liquid separation by triple effect fractional crystallization device, separating obtained residue vapor enters condensing works, separating obtained once concentration liquid enters the evaporation unit of an effect evaporation element, and evaporation concentration is carried out vapor-liquid separation by an effect fractional crystallization device;
Step 3, described once concentration liquid carries out after vapor-liquid separation through a described effect fractional crystallization device, separating obtained primary steam enters the evaporation unit of two effect evaporation elements as heating source, separating obtained secondary concentration liquid enters the evaporation unit of two effect evaporation elements, and condensing crystal carries out vapor-liquid separation by two effect fractional crystallization devices;
Step 4, described secondary concentration liquid is through two effect fractional crystallization devices, separating obtained secondary steam enters the evaporation unit of described triple effect evaporation unit as heat source, separating obtained sodium wolframate magma enters filter press, filtrate is that concentrated sodium hydroxide solution returns to ammonium paratungstate production flow process, and filter residue is after the press filtration of sodium wolframate dissolution of crystals, to enter tungsten to smelt the front solution preparation operation of ion-exchange.
Preferably, described in described step 1, liquid-solid ratio is 1～1.2:1 during basic pressure digestion.
Preferably, described in described step 1, in coarse sodium tungstate, containing sodium hydroxide mass concentration, be that 80～150g/L and tungstic oxide mass concentration are 150～180g/L.
Preferably, the cold in-water temperature of described condensing works is 32～35 ℃, and leaving water temperature(LWT) is 38～40 ℃.
Preferably, the water of condensation being obtained by described condensing works can return to described ammonium paratungstate production flow process.
Preferably, the temperature in of the raw steam of evaporation unit of an effect evaporation element is 155 ℃ described in described step 3, and vapor pressure is 0.3～0.5MPa.
Preferably, described in described step 4, secondary concentration liquid mass percent concentration is less than 42%.
In described basic pressure digestion process, to the amount of adding sodium hydroxide in described tungsten ore slurry, be generally, 2.8～4.0 times of theoretical consumption alkali, described theoretical alkali charge is one ton of tungstic oxide (WO
3) consumption 0.345t sodium hydroxide, such as: one ton of tungsten ore raw material is containing 0.5 ton of WO
3, one ton of tungsten ore consumes sodium hydroxide:
1t×0.5t×0.345×(2.8～4.0)＝(0.5～0.7)t。
The invention has the beneficial effects as follows that the inventive method adopts triple effect mixed flow evaporation technology, the low-temperature evaporation of realizing solution under vacuum state is concentrated, and concentrated effect is good, and energy consumption is low, and environmental protection pressure is little, and level of automation is high; The inventive method is by the strict mass percent concentration of controlling the sodium wolframate of triple effect evaporation unit and the separating obtained concentrated solution of an effect evaporation element, effectively prevent that sodium wolframate crystallization from occurring, thereby effectively stop the fouling of well heater tube side, good effect of heat exchange, consumes the energy low; The inventive method is concentrated crystallization sodium wolframate at two effect evaporation elements, makes sodium wolframate organic efficiency high; After excess hydrogen sodium oxide in coarse sodium tungstate is reclaimed, can reduce follow-up tungsten and smelt liquid processing cost after ion-exchange, reduce the use sulfuric acid amount that regulates pH value in tungsten smelting wastewater disposal process, greatly reduce the expenditure with cost that expends of resource.In a word, the inventive method level of automation is high, easy to operate, than absorption method intermittently, energy-conservation and low the present invention of labour intensity is than traditional single-effect evaporation crystallization process, can significantly reduce energy consumption, alleviate in later stage waste water and administer burden, reduce cost of labor, reduce labour intensity, level of automation is high, easy to operate, easily realize, and meets the policy of national cost efficiency, energy-saving and emission-reduction.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet that tungsten of the present invention is smelted the recovery method of excess hydrogen sodium oxide in coarse sodium tungstate.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail, to make those skilled in the art can implement according to this with reference to specification sheets word.
Embodiment 1
As shown in Figure 1, in tungsten smelting coarse sodium tungstate, the recovery method of excess hydrogen sodium oxide is:
Step 1, by tungsten ore raw material and water by volume 10:3 mix and add ball milling in ball mill to obtain tungsten ore slurry, in described tungsten ore slurry, add sodium hydroxide solution, described sodium hydroxide solution addition is that in described sodium hydroxide solution, sodium hydrate content is 1.0 times of tungstic oxide content in described tungsten ore raw material, afterwards the described tungsten ore stock pump that adds described sodium hydroxide solution is entered in the middle pressure reactor that band stirs, to carry out basic pressure digestion and obtain basic pressure digestion slurry, during basic pressure digestion, liquid-solid ratio is generally 1～1.2:1, described basic pressure digestion slurry obtains coarse sodium tungstate after twice press filtration,
Wherein, in described coarse sodium tungstate, containing sodium hydroxide and tungstic oxide mass concentration, be respectively 80g/L and 150g/L;
Step 2, described coarse sodium tungstate is sent in the reinforced primary heater unit of triple effect evaporation crystallizer through fresh feed pump, when described coarse sodium tungstate preheating temperature reaches the boiling temperature of triple effect evaporation modular heater, described coarse sodium tungstate is pumped into the evaporation unit of described triple effect evaporation unit, evaporation concentration is carried out vapor-liquid separation by triple effect fractional crystallization device, separating obtained residue vapor enters condensing works, separating obtained once concentration liquid enters the evaporation unit of an effect evaporation element, and evaporation concentration is carried out vapor-liquid separation by an effect fractional crystallization device;
Wherein, described condensing works cold in-water temperature is 32 ℃～35 ℃, and leaving water temperature(LWT) is 38 ℃～40 ℃, and in described once concentration liquid, sodium wolframate mass percent concentration is 27.2%
Step 3, described once concentration liquid carries out after vapor-liquid separation through a described effect fractional crystallization device, separating obtained primary steam enters the evaporation unit of two effect evaporation elements as heating source, separating obtained secondary concentration liquid enters the evaporation unit of two effect evaporation elements, and condensing crystal carries out vapor-liquid separation by two effect fractional crystallization devices;
Wherein, the temperature in of the raw steam of evaporation unit of a described effect evaporation element is 155 ℃, and vapor pressure is 0.5MPa, and in described secondary concentration liquid, sodium wolframate mass percent concentration is 40.5%;
Step 4, described secondary concentration liquid carries out after vapor-liquid separation through described two effect fractional crystallization devices, separating obtained secondary steam enters the evaporation unit of described triple effect evaporation unit as heating source, it is that concentrated sodium hydroxide solution returns to ammonium paratungstate production flow process that separating obtained sodium wolframate magma enters filter press gained filtrate, and gained filter residue is that sodium wolframate crystal enters the front solution preparation operation of tungsten smelting ion-exchange.
Wherein, in described filtrate, the concentration of sodium hydroxide is 308g/L, WO
3concentration be 36g/L, WO
3percent crystallization in massecuite be 94.0%, the rate of recovery of sodium hydroxide is 96.3%.
Embodiment 2
As shown in Figure 1, in tungsten smelting coarse sodium tungstate, the recovery method of excess hydrogen sodium oxide is:
Step 1, by tungsten ore raw material and water by volume 10:3 mix and add ball milling in ball mill to obtain tungsten ore slurry, in described tungsten ore slurry, add sodium hydroxide solution, described sodium hydroxide solution addition is that in described sodium hydroxide solution, sodium hydrate content is 1.2 times of tungstic oxide content in described tungsten ore raw material, afterwards the described tungsten ore stock pump that adds described sodium hydroxide solution is entered in the middle pressure reactor that band stirs, to carry out basic pressure digestion and obtain basic pressure digestion slurry, during basic pressure digestion, liquid-solid ratio is generally 1～1.2:1, described basic pressure digestion slurry obtains coarse sodium tungstate after twice press filtration,
Wherein, in described coarse sodium tungstate, containing sodium hydroxide and tungstic oxide mass concentration, be respectively 100g/L and 165g/L;
Step 2, described coarse sodium tungstate is sent in the reinforced primary heater unit of triple effect evaporation crystallizer through fresh feed pump, when described coarse sodium tungstate preheating temperature reaches the boiling temperature of triple effect evaporation modular heater, described coarse sodium tungstate is pumped into the evaporation unit of described triple effect evaporation unit, evaporation concentration is carried out vapor-liquid separation by triple effect fractional crystallization device, separating obtained residue vapor enters condensing works, separating obtained once concentration liquid enters the evaporation unit of an effect evaporation element, and evaporation concentration is carried out vapor-liquid separation by an effect fractional crystallization device;
Wherein, described condensing works cold in-water temperature is 32 ℃～35 ℃, and leaving water temperature(LWT) is 38 ℃～40 ℃, and in described once concentration liquid, sodium wolframate mass percent concentration is 28.0%
Step 3, described once concentration liquid carries out after vapor-liquid separation through a described effect fractional crystallization device, separating obtained primary steam enters the evaporation unit of two effect evaporation elements as heating source, separating obtained secondary concentration liquid enters the evaporation unit of two effect evaporation elements, and condensing crystal carries out vapor-liquid separation by two effect fractional crystallization devices;
Wherein, the temperature in of the raw steam of evaporation unit of a described effect evaporation element is 155 ℃, and vapor pressure is 0.5MPa, and in described secondary concentration liquid, sodium wolframate mass percent concentration is 41.3%;
Step 4, described secondary concentration liquid carries out after vapor-liquid separation through described two effect fractional crystallization devices, separating obtained secondary steam enters the evaporation unit of described triple effect evaporation unit as heating source, it is that concentrated sodium hydroxide solution returns to ammonium paratungstate production flow process that separating obtained sodium wolframate magma enters filter press gained filtrate, and gained filter residue is that sodium wolframate crystal enters the front solution preparation operation of tungsten smelting ion-exchange.
Wherein, in described filtrate, the concentration of sodium hydroxide is 353g/L, WO
3concentration be 24g/L, WO
3percent crystallization in massecuite be 96.0%, the rate of recovery of sodium hydroxide is 97.1%.
Embodiment 3
As shown in Figure 1, in tungsten smelting coarse sodium tungstate, the recovery method of excess hydrogen sodium oxide is:
Step 1, by tungsten ore raw material and water by volume 10:3 mix and add ball milling in ball mill to obtain tungsten ore slurry, in described tungsten ore slurry, add sodium hydroxide solution, described sodium hydroxide solution addition is that in described sodium hydroxide solution, sodium hydrate content is 1.4 times of tungstic oxide content in described tungsten ore raw material, afterwards the described tungsten ore stock pump that adds described sodium hydroxide solution is entered in the middle pressure reactor that band stirs, to carry out basic pressure digestion and obtain basic pressure digestion slurry, during basic pressure digestion, liquid-solid ratio is generally 1～1.2:1, described basic pressure digestion slurry obtains coarse sodium tungstate after twice press filtration,
Wherein, in described coarse sodium tungstate, containing sodium hydroxide and tungstic oxide mass concentration, be respectively 150g/L and 180g/L;
Step 2, described coarse sodium tungstate is sent in the reinforced primary heater unit of triple effect evaporation crystallizer through fresh feed pump, when described coarse sodium tungstate preheating temperature reaches the boiling temperature of triple effect evaporation modular heater, described coarse sodium tungstate is pumped into the evaporation unit of described triple effect evaporation unit, evaporation concentration is carried out vapor-liquid separation by triple effect fractional crystallization device, separating obtained residue vapor enters condensing works, separating obtained once concentration liquid enters the evaporation unit of an effect evaporation element, and evaporation concentration is carried out vapor-liquid separation by an effect fractional crystallization device;
Wherein, described condensing works cold in-water temperature is 32 ℃～35 ℃, and leaving water temperature(LWT) is 38 ℃～40 ℃, and in described once concentration liquid, sodium wolframate mass percent concentration is 28.7%
Step 3, described once concentration liquid carries out after vapor-liquid separation through a described effect fractional crystallization device, separating obtained primary steam enters the evaporation unit of two effect evaporation elements as heating source, separating obtained secondary concentration liquid enters the evaporation unit of two effect evaporation elements, and condensing crystal carries out vapor-liquid separation by two effect fractional crystallization devices;
Wherein, the temperature in of the raw steam of evaporation unit of a described effect evaporation element is 155 ℃, and vapor pressure is 0.5MPa, and in described secondary concentration liquid, sodium wolframate mass percent concentration is 41.7%;
Step 4, described secondary concentration liquid carries out after vapor-liquid separation through described two effect fractional crystallization devices, separating obtained secondary steam enters the evaporation unit of described triple effect evaporation unit as heating source, it is that concentrated sodium hydroxide solution returns to ammonium paratungstate production flow process that separating obtained sodium wolframate magma enters filter press gained filtrate, and gained filter residue is that sodium wolframate crystal enters the front solution preparation operation of tungsten smelting ion-exchange.
Wherein, in described filtrate, the concentration of sodium hydroxide is 373g/L, WO
3concentration be 17g/L, WO
3percent crystallization in massecuite be 96.3%, the rate of recovery of sodium hydroxide is 97.4%.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in specification sheets and embodiment, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other modification, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend of describing.
Claims (8)
1. tungsten is smelted a recovery method for excess hydrogen sodium oxide in coarse sodium tungstate, it is characterized in that, comprises the following steps:
Step 1, by tungsten ore raw material and water by volume 10:3 mix and add ball milling in ball mill to obtain tungsten ore slurry, in described tungsten ore slurry, add sodium hydroxide solution, described sodium hydroxide solution addition is that in described sodium hydroxide solution, sodium hydrate content is 1.0～1.4 times of tungstic oxide content in described tungsten ore raw material, the described tungsten ore stock pump that adds described sodium hydroxide solution is entered to be with in the middle pressure reactor stirring afterwards and carry out basic pressure digestion acquisition basic pressure digestion slurry, described basic pressure digestion slurry obtains coarse sodium tungstate after twice press filtration;
Step 2, described coarse sodium tungstate is sent in the reinforced primary heater unit of triple effect evaporation crystallizer through fresh feed pump, when described coarse sodium tungstate preheating temperature reaches the boiling temperature of triple effect evaporation modular heater, described coarse sodium tungstate is pumped into the evaporation unit of described triple effect crystalline element, evaporation concentration is carried out vapor-liquid separation by triple effect fractional crystallization device, separating obtained residue vapor enters condensing works, separating obtained once concentration liquid enters the evaporation unit of an effect evaporation element, and evaporation concentration is carried out vapor-liquid separation by an effect fractional crystallization device;
Step 3, described once concentration liquid carries out after vapor-liquid separation through an effect fractional crystallization device of a described effect evaporation element, separating obtained primary steam enters the evaporation unit of two effect evaporation elements as heating source, separating obtained secondary concentration liquid enters the evaporation unit of two effect evaporation elements, and condensing crystal carries out vapor-liquid separation by two effect fractional crystallization devices;
Step 4, described secondary concentration liquid carries out after vapor-liquid separation through two effect fractional crystallization devices of described two effect evaporation elements, separating obtained secondary steam enters the evaporation unit of described triple effect evaporation unit as heating source, it is that concentrated sodium hydroxide solution returns to ammonium paratungstate production flow process that separating obtained sodium wolframate magma enters filter press gained filtrate, and gained filter residue is that sodium wolframate crystal enters the front solution preparation operation of tungsten smelting ion-exchange.
2. tungsten as claimed in claim 1 is smelted the recovery method of excess hydrogen sodium oxide in coarse sodium tungstate, it is characterized in that, liquid-solid ratio is 1～1.2:1 during basic pressure digestion described in described step 1.
3. tungsten as claimed in claim 1 is smelted the recovery method of excess hydrogen sodium oxide in coarse sodium tungstate, it is characterized in that, in coarse sodium tungstate, containing sodium hydroxide and tungstic oxide mass concentration, be respectively 80～150g/L and 150～180g/L described in described step 1.
4. tungsten as claimed in claim 1 is smelted the recovery method of excess hydrogen sodium oxide in coarse sodium tungstate, it is characterized in that, the cold in-water temperature of described condensing works is 32 ℃～35 ℃, and leaving water temperature(LWT) is 38 ℃～40 ℃.
5. tungsten as claimed in claim 1 is smelted the recovery method of excess hydrogen sodium oxide in coarse sodium tungstate, it is characterized in that, the water of condensation being obtained by described condensing works can return to described ammonium paratungstate production flow process.
6. tungsten as claimed in claim 1 is smelted the recovery method of excess hydrogen sodium oxide in coarse sodium tungstate, it is characterized in that, the temperature in of the raw steam of evaporation unit of an effect evaporation element is 155 ℃ described in described step 3, and vapor pressure is 0.3～0.5MPa.
7. tungsten as claimed in claim 1 is smelted the recovery method of excess hydrogen sodium oxide in coarse sodium tungstate, it is characterized in that, secondary concentration liquid mass percent concentration is less than 42% described in described step 4.
8. tungsten as claimed in claim 1 is smelted the recovery method of excess hydrogen sodium oxide in coarse sodium tungstate, it is characterized in that, ammonium paratungstate production flow process comprises basic pressure digestion operation and ball milling operation etc. described in described step 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310438500.9A CN103523800B (en) | 2013-09-24 | 2013-09-24 | Method for recovering excess sodium hydroxide in tungsten smelting crude sodium tungstate solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310438500.9A CN103523800B (en) | 2013-09-24 | 2013-09-24 | Method for recovering excess sodium hydroxide in tungsten smelting crude sodium tungstate solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103523800A true CN103523800A (en) | 2014-01-22 |
| CN103523800B CN103523800B (en) | 2015-01-07 |
Family
ID=49926223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310438500.9A Active CN103523800B (en) | 2013-09-24 | 2013-09-24 | Method for recovering excess sodium hydroxide in tungsten smelting crude sodium tungstate solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103523800B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556231A (en) * | 2014-12-27 | 2015-04-29 | 山东天维膜技术有限公司 | Preparation method of sodium tungstate solution and method for recovering alkaline in preparation process |
| CN104789772A (en) * | 2015-04-06 | 2015-07-22 | 桂林理工大学 | Energy-saving and consumption-reducing method for alkaline leaching of scheelite |
| CN109824064A (en) * | 2019-03-25 | 2019-05-31 | 中南大学 | The method of sodium carbonate is recycled from sodium tungstate leachate |
| CN110551892A (en) * | 2019-10-17 | 2019-12-10 | 中国恩菲工程技术有限公司 | mineral separation device containing tungsten-tin concentrate |
| CN110760703A (en) * | 2019-11-20 | 2020-02-07 | 中国有色集团（广西）平桂飞碟股份有限公司 | Method for recovering tungsten from waste APT powder |
| CN115353148A (en) * | 2022-08-31 | 2022-11-18 | 赣州有色冶金研究所有限公司 | Method for recovering sodium hydroxide from sodium tungstate alkali cooking liquor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5788938A (en) * | 1996-06-05 | 1998-08-04 | Osram Sylvania Inc. | Recovery of tungsten from ferrotungsten |
| JP2008150251A (en) * | 2006-12-19 | 2008-07-03 | Nippon Rensui Co Ltd | Method of manufacturing ammonium tungstate aqueous solution |
| CN102963911A (en) * | 2012-11-14 | 2013-03-13 | 中湘钨业股份有限公司 | Method of recycling residual alkali from sodium tungstate solution in tungsten smelting |
| CN103103359A (en) * | 2012-11-23 | 2013-05-15 | 陈泉兴 | Method for regenerating APT (ammonium paratungstate) by use of APT waste low-grade tungsten slag |
-
2013
- 2013-09-24 CN CN201310438500.9A patent/CN103523800B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5788938A (en) * | 1996-06-05 | 1998-08-04 | Osram Sylvania Inc. | Recovery of tungsten from ferrotungsten |
| JP2008150251A (en) * | 2006-12-19 | 2008-07-03 | Nippon Rensui Co Ltd | Method of manufacturing ammonium tungstate aqueous solution |
| CN102963911A (en) * | 2012-11-14 | 2013-03-13 | 中湘钨业股份有限公司 | Method of recycling residual alkali from sodium tungstate solution in tungsten smelting |
| CN103103359A (en) * | 2012-11-23 | 2013-05-15 | 陈泉兴 | Method for regenerating APT (ammonium paratungstate) by use of APT waste low-grade tungsten slag |
Non-Patent Citations (2)
| Title |
|---|
| 刘扬林等: ""电渗析法脱除粗钨酸钠中的游离碱研究"", 《株洲师范高等专科学校学报》 * |
| 徐志昌等: ""双极性膜电渗析法回收钨酸钠溶液中的游离氢氧化钠"", 《中国钼业》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556231A (en) * | 2014-12-27 | 2015-04-29 | 山东天维膜技术有限公司 | Preparation method of sodium tungstate solution and method for recovering alkaline in preparation process |
| CN104789772A (en) * | 2015-04-06 | 2015-07-22 | 桂林理工大学 | Energy-saving and consumption-reducing method for alkaline leaching of scheelite |
| CN109824064A (en) * | 2019-03-25 | 2019-05-31 | 中南大学 | The method of sodium carbonate is recycled from sodium tungstate leachate |
| CN110551892A (en) * | 2019-10-17 | 2019-12-10 | 中国恩菲工程技术有限公司 | mineral separation device containing tungsten-tin concentrate |
| CN110760703A (en) * | 2019-11-20 | 2020-02-07 | 中国有色集团（广西）平桂飞碟股份有限公司 | Method for recovering tungsten from waste APT powder |
| CN110760703B (en) * | 2019-11-20 | 2021-09-03 | 中国有色集团（广西）平桂飞碟股份有限公司 | Method for recovering tungsten from waste APT powder |
| CN115353148A (en) * | 2022-08-31 | 2022-11-18 | 赣州有色冶金研究所有限公司 | Method for recovering sodium hydroxide from sodium tungstate alkali cooking liquor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103523800B (en) | 2015-01-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103523800B (en) | Method for recovering excess sodium hydroxide in tungsten smelting crude sodium tungstate solution | |
| CN106007133B (en) | A kind of desulfurization wastewater concentration and evaporation, crystallization, salt separating technology | |
| Rioyo et al. | Lithium extraction from spodumene by the traditional sulfuric acid process: A review | |
| CN105585194B (en) | One kind contains Na+、K+、NH4+、Cl‑、SO42‑、NO3‑The highly concentrated effluent brine method of comprehensive utilization of coal chemical industry | |
| CN100455512C (en) | Method for preparing battery-stage monohydrate lithium hydroxide | |
| CN103570043B (en) | Method for producing high-purity potassium chloride solution for preparation of potassium carbonate and co-producing low sodium salt | |
| CN104532283B (en) | A kind of light salt brine replaces method and the device of part refined brine electrolysis caustic soda | |
| CN1486931A (en) | Production process of lithium hydroxide monohydrate | |
| CN102041380A (en) | Production process for extracting lithium from ore with low-temperature method | |
| CN113105138A (en) | Method and system for water washing dechlorination of waste incineration fly ash and evaporation mass-separation crystallization of water washing liquid | |
| CN102491379A (en) | Method for preparing high-purity magnesium oxide with high boron salt lake brine | |
| CN101607739A (en) | Closed cycle process for crystalline mother solution of ammonium paratungstate | |
| CN102963911A (en) | Method of recycling residual alkali from sodium tungstate solution in tungsten smelting | |
| CN102502740A (en) | Method for preparing high-alkali high-causticity-ratio solution and improving traditional seed precipitation efficiency | |
| CN101070168B (en) | Method for producing sodium nitrate | |
| CN105384293B (en) | A kind of processing method of the vanadium wastewater after the deamination that cleans | |
| CN114854986A (en) | Method for producing lithium carbonate by leaching spodumene ore with nitric acid | |
| CN106119541B (en) | A kind of method of oxalic acid precipitation rare earth | |
| CN103663505A (en) | Method for treating potassium feldspar according to sub-molten salt method to prepare potassium carbonate | |
| CN102912129A (en) | Method for recycling tungsten in liquids after tungsten smelting exchanges | |
| CN103408046B (en) | Method for separating sodium and magnesium from laterite-nickel ore smelting primary wastewater | |
| CN113493213A (en) | Process and equipment for recycling and zero discharge of wastewater containing sodium chloride and sodium sulfate | |
| CN212955279U (en) | Recovery unit who contains chromium aluminiferous mud | |
| CN104556231A (en) | Preparation method of sodium tungstate solution and method for recovering alkaline in preparation process | |
| CN104743586A (en) | Joint production method of alkali leaching of aluminium in Bayer red mud and aluminium oxide decomposed mother liquid evaporation for salt elimination |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |