CN102963911A - Method of recycling residual alkali from sodium tungstate solution in tungsten smelting - Google Patents
Method of recycling residual alkali from sodium tungstate solution in tungsten smelting Download PDFInfo
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Abstract
The invention discloses a method of recycling residual alkali from sodium tungstate solution in tungsten smelting, which comprises the steps of: performing liquid-solid separation on mixed material solution discharged from a pressure cooking kettle through a press filter, pumping the filtrate into a three-effect evaporation crystallizer through a pump, firstly preheating the filtrate in a first preheating pipe, then conveying the filtrate into a first-effect evaporation crystallizer, using the secondary vapor generated by first-effect evaporation concentration as a heat source of second-effect evaporation concentration, and conveying sodium tungstate crystals separated out from a second-effect evaporation crystallizer into a plate-and-frame filter press to perform solid-liquid separation; conveying the concentrated solution into a third-effect concentrator, and performing solid-liquid separation on the sodium tungstate crystals separated out from a crystallization kettle of the third-effect evaporation crystallizer; performing solid-liquid separation on the crystals separated out by the second-effect evaporation crystallizer and the third-effect evaporation crystallizer in the plate-and-frame filter press; and conveying the filtrate into a storage tank to return to the pressure cooking procedure to prepare alkali, and discharging the filter residues in a dissolving tank. The method disclosed by the invention is mature in technique and equipment, high in automation degree, high in utilization rate of effective resources, good in energy-saving effect and high in recycled economic benefit, and the method is an important comprehensive recycling component in tungsten smelting.
Description
Technical field
The invention belongs to the tungsten hydrometallurgy, specifically relate to the method that a kind of sodium tungstate solution from tungsten is smelted reclaims remaining alkali.
Background technology
China is tungsten resource big country, and tungsten resource mainly exists with wolframite and sheelite form, and along with successively decreasing of wolframite stock number, exploitation sheelite resource has become the main mineral of tungsten resource.In the past, sheelite is the difficult raw material of adopting difficult smelting during tungsten is smelted, the sheelite resource also rests in the resource reserve, along with the smelting technology of sheelite obtains breaking through, after reaching with the pressure digestion technique of high excess base, sheelite is smelted production capacity and scale is promoted energetically, and technical matters is also further ripe.Owing to adopted excess base technique, although consumed very most of alkali in the leaching process, after reaction finished, the remaining alkali number in the leach liquor was still very high, and remaining alkali naoh concentration does not wait from 40～150g/L.Remaining alkali number too much can bring impact to subsequent technique: the one, and the main technical process that modern tungsten is smelted is ion exchange method, and too high alkali produces unfavorable effect to the absorption of ion-exchange, and the wolframate radical polymeric adsorbent is influenced; The 2nd, these excessive alkali have finally been stayed in the rear liquid of exchange, and the rear liquid of exchange is the main source of tungsten smelting discharging of waste liquid normally, and excessive alkali will make discharging of waste liquid up to standard, must consume a large amount of acid and neutralize to reach emission request.Therefore, excessive more alkali not only affects exchange process simultaneously but also wastes resource, so that the tungsten smelting industry is progressively paid attention to the recovery to remaining alkali.
The recovery of remaining alkali was the alkali recovery in sodium wolframate and sodium hydroxide mixed solution system during tungsten was smelted, the two has such rule in solution: the changes in solubility of sodium wolframate under different naoh concentrations is large, along with the rising of naoh concentration, the solubleness of sodium wolframate is successively decreased.For example sodium hydroxide and the starting point concentration of concentration of sodium tungstate in solution are 100g/L in such feed liquid, pass through evaporation concentration, naoh concentration can reach more than the 500g/L not can crystallization, and sodium wolframate is most of crystallization, and residual concentration can be down to below 20 g/L; Therefore, utilize this rule just can well sodium wolframate and sodium hydroxide be separated from each other.After the separation, the sodium wolframate that crystallizes out continues lower one exchange adsorption operation with water dissolution, and the sodium hydroxide after concentrating then returns presses the digestion operation to carry out recycle, has so just realized the recycling of remaining alkali.
It is the concentrated and crystallisation process of solution evaporation that remaining alkali reclaims, it mainly is energy consumption, but because under the situation that current energy prices constantly rise, what enterprise paid attention to is the relation that reclaims income and cost, when being lower than certain remaining alkali concn, alkali reclaims income and energy consumption consumption quite or during negative, most tungsten smelting enterprise can not consider remaining alkali is reclaimed.And the remaining alkali of current real enforcement reclaims, mainly be for the enterprise that processes the assorted material of low-grade tungsten or adopt high excess base extract technology, usually alkali concn is more than 100 g/L more than in the solution, and these alkali reclaiming methods mainly are to adopt single pot of traditional step evaporation concentration equipment, many outstanding problems such as this method energy consumption is large, level of automation is low, and marginal income is low.
Summary of the invention
The object of the present invention is to provide a kind of technical process simple, the energy-conservation sodium tungstate solution from tungsten is smelted reclaims the method for remaining alkali.
Technical scheme of the present invention is: boil still mixed liquor out by the filtrate after the liquid-solid separation of pressure filter from pressure, with being pumped into the triple effect evaporation crystallizer, at first enter and carry out preheating in the first preheating tube, then enter the first effect evaporative crystallizer, give birth to the vapor pressure scope at 0.4～1.0MPa, the secondary steam of one effect evaporation concentration output is as the thermal source of two effect evaporation concentration, the sodium wolframate crystalline substance that two effect evaporative crystallizer condensing crystals are separated out send plate-and-frame filter press to carry out solid-liquid separation, concentrated solution continues in the triple effect evaporation crystallizer, and the sodium wolframate crystal of separating out from triple effect evaporation crystallizer crystallization kettle is sent into plate-and-frame filter press and carried out solid-liquid separation; The crystal that two effect evaporative crystallizers and triple effect evaporation crystallizer are separated out together enters the sheet frame pressure filter 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 the dissolving tank.
Water vapour in the necessary a large amount of evaporating solnss of the sodium tungstate solution that hangs down remaining alkali concn, after further concentrating, after alkali concn promoted, the solubleness of sodium wolframate when high-alkali descended rapidly, crystal occurs and separates out.Continue along with concentrated, soltion viscosity increases, therefore in the design arrangement of triple effect evaporation crystallizer, two triple effect crystallizations all can vacuumize operation, can effectively reduce like this boiling temperature of solution, although the situation that an effect regeneration steam decreases than living vapor temperature also can realize the further concentrated purpose to solution.Because raising with alkali concn, the solubleness of sodium wolframate reduces, therefore, two, all be provided with independently crystal discharge port in the triple effect evaporation crystallizer, stop like this in two effect crystallizers and to separate out fouling because of a large amount of crystal and hinder the pipe problem.
The present invention reclaims utilizing the triple effect evaporation crystallizer that the sodium hydroxide in the sodium tungstate solution is implemented remaining alkali, realize the lifting of alkali concn by concentrated solution, simultaneously when alkali concn raises, crystal appears in the decline of sodium wolframate solubleness separates out, and just turns back to by alkali after the liquid-solid separation and presses boiling procedure to recycle.This invention has the following advantage.
1. the triple effect evaporation crystallizer has energy utilization rate high, energy-conservation than the concentration and evaporation pan of a traditional effect formula; In the triple effect evaporation flow process, only use living steam in the first effect, effectively utilized the heat in the secondary steam, so saved the usage quantity of living steam, reduced by contrast production cost, improved economic benefit.So the remaining alkali of lower concentration is implemented to reclaim the possibility that becomes tungsten smelting industry wide popularization and application.
2. after remaining alkali being reclaimed, can reduce liquid processing cost after the subsequent exchange, reduce measuring with acid of waste water dis posal procedure regulation pH value, greatly reduce the expenditure with cost of expending of resource; The method level of automation is high, and is easy to operate, than intermittence absorption method energy-conservation and labour intensity is low.
3. the process of remaining alkali recovery also is the process that sodium tungstate solution has been implemented step purification removal of impurities.Most of sodium wolframate condensing crystal, the impurity of overwhelming majority lower concentration is stayed in the solution, although impurity in the remaining alkali concentrated solution is by enrichment, but in returning the pressure boiling procedure, the accumulation situation does not appear in the impurity in the leach liquor, therefore remaining alkali reclaims the process of indirectly having carried out a removal of impurities to whole flow process, is conducive to the purity of follow-up ion exchange process and product.
Smelt the alkali recovery for tungsten and generally also adopt single pot of thickening equipment, the large alkali of a lot of enterprises that stoped of crystallization energy consumption reclaims enforcement, therefore, the method has adopted the triple effect evaporation crystallizer to implement remaining alkali and has reclaimed, it is a kind of energy-saving recovery method, the remaining alkali of the lower concentration that tungsten is smelted reclaims and becomes possibility, and it is obvious to reclaim benefit, is a kind of processing method of the energy-saving and emission-reduction that can apply in the tungsten smelting industry.
The present invention has used for reference the ripe Multi-effect evaporation crystallizer of using in other industry, by in conjunction with the enriched material physical chemistry characteristic in sodium wolframate and the sodium hydroxide mixed solution system, Multi-effect evaporation crystallizer to maturation carries out targetedly design arrangement, take full advantage of thermal source, realize energy-conservation concentrated purpose.As long as concentrated energy consumption descends, the total energy consumption cost then can the remaining alkali of decrease reclaims the lower limit limit of concentration, allows alkali reclaim and can obtain reasonable comprehensive recovery benefit; The present invention is in conjunction with the feature of sodium tungstate solution system, adopts the triple effect evaporation crystallizer, and an effect evaporation, two, triple effect not only concentrated but also improved method that go out crystal are implemented remaining alkali and reclaimed.
Description of drawings
Fig. 1 is concrete technology schema of the present invention.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing.
Embodiment one:
Boil still sodium wolframate feed liquid out from pressure and contain tungstic oxide 100g/L, naoh concentration 40 g/L, liquor capacity is 5000mL, after the liquid-solid separation of pressure filter, with being pumped into the triple effect evaporation crystallizer, one effect evaporative crystallizer entrance is given birth to vapor pressure 0.4MPa, 155 ℃ of temperature, the sodium wolframate crystal that two effect evaporative crystallizers and triple effect evaporation crystallizer are separated out send plate-and-frame filter press to carry out solid-liquid separation, and filtrate is returned the pressure boiling procedure, ion-exchange process is sent in the filter residue dissolving, water of condensation is as main flow diluting water, filtrate naoh concentration 355g/L, tungstic oxide 35.6g/L, the tungsten direct yield is 96%, alkali recovery 97.5%.
Embodiment two:
Boil still sodium wolframate feed liquid out from pressure and contain tungstic oxide 100g/L, naoh concentration 45 g/L, liquor capacity is 5000mL, after the liquid-solid separation of pressure filter, with being pumped into the triple effect evaporation crystallizer, one effect evaporative crystallizer entrance is given birth to vapor pressure 0.4MPa, 155 ℃ of temperature, the sodium wolframate crystal that two effect evaporative crystallizers and triple effect evaporation crystallizer are separated out send plate-and-frame filter press to carry out solid-liquid separation, filtrate is returned the pressure boiling procedure, and ion-exchange process is sent in the filter residue dissolving, and water of condensation is as the main flow diluting water, filtrate naoh concentration 385 g/L, tungstic oxide 25.5g/L.The tungsten direct yield is 97%, alkali recovery 96.8%.
Embodiment three:
Boil still sodium wolframate feed liquid out from pressure and contain tungstic oxide 100g/L, naoh concentration 50 g/L, liquor capacity is 5000mL, after the liquid-solid separation of pressure filter, with being pumped into the triple effect evaporation crystallizer, one effect evaporative crystallizer entrance is given birth to vapor pressure 0.4MPa, 155 ℃ of temperature, the sodium wolframate crystal that two effect evaporative crystallizers and triple effect evaporation crystallizer are separated out send plate-and-frame filter press to carry out solid-liquid separation, filtrate is returned the pressure boiling procedure, and ion-exchange process is sent in the filter residue dissolving, and water of condensation is as the main flow diluting water, filtrate naoh concentration 390.5 g/L, tungstic oxide 23.6g/L.The tungsten direct yield is 97%, alkali recovery 97.1%.
Embodiment four:
Boil still sodium wolframate feed liquid out from pressure and contain tungstic oxide 100g/L, naoh concentration 60 g/L, liquor capacity is 5000mL, after the liquid-solid separation of pressure filter, with being pumped into the triple effect evaporation crystallizer, one effect evaporative crystallizer entrance is given birth to vapor pressure 0.4MPa, 155 ℃ of temperature, the sodium wolframate crystal that two effect evaporative crystallizers and triple effect evaporation crystallizer are separated out send plate-and-frame filter press to carry out solid-liquid separation, filtrate is returned the pressure boiling procedure, and ion-exchange process is sent in the filter residue dissolving, and water of condensation is as the main flow diluting water, filtrate naoh concentration 401.3 g/L, tungstic oxide 21.2g/L.The tungsten direct yield is 96.8%, alkali recovery 97.8%.
Embodiment five:
Boil still sodium wolframate feed liquid out from pressure and contain tungstic oxide 100g/L, naoh concentration 70 g/L, liquor capacity is 5000mL, after the liquid-solid separation of pressure filter, with being pumped into the triple effect evaporation crystallizer, one effect evaporative crystallizer entrance is given birth to vapor pressure 0.4MPa, 155 ℃ of temperature, the sodium wolframate crystal that two effect evaporative crystallizers and triple effect evaporation crystallizer are separated out send plate-and-frame filter press to carry out solid-liquid separation, filtrate is returned the pressure boiling procedure, and ion-exchange process is sent in the filter residue dissolving, and water of condensation is as the main flow diluting water, filtrate naoh concentration 410.4 g/L, tungstic oxide 19.2g/L.The tungsten direct yield is 96.7%, alkali recovery 96.5%.
Embodiment six:
Boil still sodium wolframate feed liquid out from pressure and contain tungstic oxide 100g/L, naoh concentration 100 g/L, liquor capacity is 5000mL, after the liquid-solid separation of pressure filter, with being pumped into the triple effect evaporation crystallizer, one effect evaporative crystallizer entrance is given birth to vapor pressure 0.4MPa, 155 ℃ of temperature, the sodium wolframate crystal that two effect evaporative crystallizers and triple effect evaporation crystallizer are separated out send plate-and-frame filter press to carry out solid-liquid separation, filtrate is returned the pressure boiling procedure, and ion-exchange process is sent in the filter residue dissolving, and water of condensation is as the main flow diluting water, filtrate naoh concentration 420.8 g/L, tungstic oxide 18.5g/L.The tungsten direct yield is 95.6%, alkali recovery 97.3%.
Single-effect evaporation pot and the contrast of triple effect evaporation crystallizer consumption quantity of steam
Claims (1)
1. the method for alkali more than the sodium tungstate solution from tungsten is smelted reclaims, it is characterized in that: boil still mixed liquor out by the filtrate after the liquid-solid separation of pressure filter from pressure, with being pumped into the triple effect evaporation crystallizer, at first enter and carry out preheating in the first preheating tube, then enter an effect evaporative crystallizer, give birth to the vapor pressure scope at 0.4～1.0MPa, the secondary steam of one effect evaporation concentration output is as the thermal source of two effect evaporation concentration, and the sodium wolframate crystal that two effect evaporative crystallizer condensing crystals are separated out send plate-and-frame filter press to carry out solid-liquid separation; Concentrated solution continues in the Three-effect concentration device, and the sodium wolframate crystal plate-and-frame filter press that triple effect evaporation crystallizer crystallization kettle is separated out carries out solid-liquid separation; The crystal that two effect evaporative crystallizers and triple effect evaporation crystallizer are separated out together enters the sheet frame pressure filter 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 the dissolving tank.
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Cited By (7)
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| CN103274403A (en) * | 2013-06-08 | 2013-09-04 | 中国科学院山西煤炭化学研究所 | Method for recycling strong alkali in preparation process of active carbon having high specific surface area |
| CN103523800A (en) * | 2013-09-24 | 2014-01-22 | 中国有色集团（广西）平桂飞碟股份有限公司 | Method for recovering excess sodium hydroxide in tungsten smelting crude sodium tungstate solution |
| CN104140114A (en) * | 2014-08-01 | 2014-11-12 | 张家港化工机械股份有限公司 | Method for recycling residual alkali liquor in caustic soda and caustic soda flake concentration device |
| CN109824064A (en) * | 2019-03-25 | 2019-05-31 | 中南大学 | The method of sodium carbonate is recycled from sodium tungstate leachate |
| CN112458317A (en) * | 2020-11-20 | 2021-03-09 | 安化县安仁粉末冶金有限公司 | Method for extracting tungsten and cobalt from tungsten-cobalt-containing waste and filter pressing device |
| 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 |
| CN115507296A (en) * | 2022-08-26 | 2022-12-23 | 中国电建集团华东勘测设计研究院有限公司 | Liquid hydrogen refueling station system for recycling BOG |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274403A (en) * | 2013-06-08 | 2013-09-04 | 中国科学院山西煤炭化学研究所 | Method for recycling strong alkali in preparation process of active carbon having high specific surface area |
| CN103523800A (en) * | 2013-09-24 | 2014-01-22 | 中国有色集团（广西）平桂飞碟股份有限公司 | Method for recovering excess sodium hydroxide in tungsten smelting crude sodium tungstate solution |
| CN104140114A (en) * | 2014-08-01 | 2014-11-12 | 张家港化工机械股份有限公司 | Method for recycling residual alkali liquor in caustic soda and caustic soda flake concentration device |
| CN104140114B (en) * | 2014-08-01 | 2016-01-13 | 苏州天沃科技股份有限公司 | The recovery method of residual alkali lye in caustic soda, sheet alkali concentrate apparatus |
| CN109824064A (en) * | 2019-03-25 | 2019-05-31 | 中南大学 | The method of sodium carbonate is recycled from sodium tungstate leachate |
| CN112458317A (en) * | 2020-11-20 | 2021-03-09 | 安化县安仁粉末冶金有限公司 | Method for extracting tungsten and cobalt from tungsten-cobalt-containing waste and filter pressing device |
| CN115507296A (en) * | 2022-08-26 | 2022-12-23 | 中国电建集团华东勘测设计研究院有限公司 | Liquid hydrogen refueling station system for recycling BOG |
| CN115507296B (en) * | 2022-08-26 | 2023-11-07 | 中国电建集团华东勘测设计研究院有限公司 | Liquid hydrogen hydrogenation station system for recycling BOG |
| 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 |
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Application publication date: 20130313 |