CN105624406A - Process method for recovering tungsten from honeycomb type SCR waste catalyst - Google Patents
Process method for recovering tungsten from honeycomb type SCR waste catalyst Download PDFInfo
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- CN105624406A CN105624406A CN201610041873.6A CN201610041873A CN105624406A CN 105624406 A CN105624406 A CN 105624406A CN 201610041873 A CN201610041873 A CN 201610041873A CN 105624406 A CN105624406 A CN 105624406A
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- leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/009—General processes for recovering metals or metallic compounds from spent catalysts
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
- C22B34/365—Obtaining tungsten from spent catalysts
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- 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
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Abstract
The invention relates to a process method for recovering tungsten from a honeycomb type SCR waste catalyst. The waste catalyst is crushed, dust and impurities are washed away by adding water, the waste catalyst is dried and ground into powder and then subjected to high-temperature leaching under pressure, filter residues and a leaching solution are obtained through soil-liquid separation, the filter residues are washed with deionized water, sodium, tungsten and vanadium in the filter residues are washed away, and washing water is recovered; after impurities in the leaching solution are removed, hydrochloric acid is added to the leaching solution and the washing water so as to adjust the pH value, then the leaching solution and the washing water are fed into ion exchange equipment, and a mixed solution containing ammonium paratungstate and ammonium metavanadate is obtained through the ion exchange and desorption procedures; after the pH value of the mixed solution is adjusted, ammonium salt is added, the temperature is adjusted, solid-liquid separation is conducted after precipitation crystallization, filtrate is collected, and the filtrate is evaporated and crystallized to obtain ammonium paratungstate crystal. According to the process method for recovering the tungsten from the honeycomb type SCR waste catalyst, resourceful treatment of the waste catalyst is achieved, environmental pollution is reduced, the recovery rate of the ammonium paratungstate is high, the quality of recovered products is good, neither high temperature nor high pressure is needed, energy consumption is low, cost is low, waste water is reused or discharged after meeting the standard, the environmental risk is small, and the method has high practicality.
Description
Technical field
The present invention relates to catalyst and reclaim field, particularly relate to the recovery process of SCR dead catalyst, particularly relate to a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst.
Background technology
SCR (SCR) flue-gas denitration process is widely adopted in steam power plant of China nitrogen oxides emission reduction work, and at present, the nitrogen oxides of domestic and international more than 90% reduces discharging and adopts SCR flue-gas denitration process. Denitrating catalyst is the important raw and processed materials of SCR flue-gas denitration process, mainly by titanium dioxide (TiO2, content 80%-90%), vanadic anhydride (V2O5, content 1%-5%), Tungstic anhydride. (WO3, content 5%-10%) and composition. While discharged nitrous oxides is significantly cut down, create the substantial amounts of waste flue gas denitration catalyst containing poisonous and harmful substance.
It is generally the service life of denitrating catalyst 3 years, the denitrating catalyst of inactivation is regenerated, can improve or recover the activity of decaying catalyst so that it is can recycle. Maximum renewable 3-4 time of denitrating catalyst, afterwards recyclable various raw material, metal or carry out final disposal.
Waste flue gas denitration catalyst is except titanium dioxide, vanadic anhydride, Tungstic anhydride., possibly together with heavy metals such as chromium, beryllium, arsenic and hydrargyrum. The main hazard characteristic of waste flue gas denitration catalyst is Leaching, wherein beryllium, copper, arsenic leaching concentration be generally higher than the leaching concentration of new denitrating catalyst; Beryllium in Some Enterprises waste flue gas denitration catalyst, arsenic, hydrargyrum leaching concentration exceed the relevant requirement of " hazardous waste judging standard leaching characteristic identification " (GB5085.3-2007). If resource, harmless treatment can not properly be carried out, very easily cause environmental pollution.
Ammonium paratungstate, also known as ammonium metatungstate, is a kind of inorganic chemical industry articles for use, can obtain Tungstic anhydride. through calcining. Tungstic anhydride. can be used for high-melting-point alloy processed and hard alloy, tungsten filament processed and fire proofing material etc., is additionally operable to calcining reduction and produces tungsten powder and tungsten carbide powder, and then be used for producing hart metal product, such as cutter and mould. Simultaneously can be used for manufacturing pure tungsten goods, tungsten rod, tungsten filament, tungsten electrode. Commercial production also has a small amount of coloring agent being used as yellow ware.
Waste flue gas denitration catalyst is reclaimed, is possible not only to effectively solve the handling problems of dead catalyst, and the tungsten in dead catalyst can be reclaimed, it is of value to the recycling treatment of dead catalyst, reduce waste discharge, obtain available effective ingredient simultaneously, meet the demand for development that China is current. It is therefore desirable to found a kind of method safely and effectively reclaiming tungsten from useless denitrating catalyst.
Summary of the invention
It is an object of the invention to provide a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst, reduce disposal amount and the discharge capacity of useless denitrating catalyst, the effective ingredient-tungsten in dead catalyst is reclaimed, achieve the recycling treatment of dead catalyst, reduce environmental pollution, and the response rate of ammonium paratungstate is high, can reach 89%, reclaim good product quality, not needing significantly high temperature and pressure, energy consumption is low, and cost is little, waste water recycling or qualified discharge, environmental risk is little.
The object of the invention to solve the technical problems realizes by the following technical solutions.
According to a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst that the present invention proposes, it comprises the following steps:
(1), SCR dead catalyst is crushed, add water and wash away dust, foreign material, it is milled to 150-180 order after drying, it is then fed in the sodium hydroxide solution that concentration is 200g/L, high temperature leaching with pressure, controlling temperature during leaching and be 110-120 DEG C, leaching pressure is 0.2-0.3MPa, and leaching solid-to-liquid ratio is 2-4m3/ t, after leaching, solid-liquid separation obtains filtering residue and leaching liquid, gained filtering residue deionized water wash, washes away sodium therein, tungsten, vanadium, and wash water reclaims;
(2), be 9.5-10.5 by step (1) gained leaching liquid salt adding acid for adjusting pH value, filter, remove silica gel impurity;
(3), the wash water that the filtrate after step (2) remove impurity and step (1) are reclaimed adds hydrochloric acid adjustment pH value is 3-4, it is then fed into ion-exchange unit, obtains the mixed solution containing ammonium paratungstate and ammonium metavanadate through ion exchange, parsing operation;
(4), by step (3) gained mixed solution regulating pH is 9, adds ammonium salt, then adjusts the temperature to 80 DEG C, naturally cool to room temperature after reacting 1 hour, and solid-liquid separation after precipitated crystal collects filtrate;
(5), the filtrate evaporative crystallization that step (4) is collected is obtained order of ammoniumparatungstate crystal.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Aforesaid a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst, wherein, step (1) extraction time is 2-3 hour.
Aforesaid a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst, wherein, the mixed liquor that step (3) adds 5mol/L ammonium chloride with 2mol/L ammonia resolves, and in the desorbed solution obtained, tungsten, vanadium total content control at more than 60g/L, and the pH value of gained desorbed solution controls at 8-10.
Aforesaid a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst, wherein, the ion-exchange unit described in step (3) adopts steel lining to mould ion exchange column, and the specification of described ion exchange column is diameter 1.4m, high 7m, the quantity of ion exchange column is 4; Ion exchange adopts serial column absroption mode, and resin adopts D314 type, and every post feeds 6 tons, amounts to 24 tons.
Aforesaid a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst, wherein, the ammonium salt described in step (4) is ammonium chloride, and solid-liquid separation method adopts centrifuge to separate.
Aforesaid a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst, wherein, the filtrate in step (5) directly uses reactor evaporative crystallization, then separates with centrifuge, and crystal is dried.
The present invention compared with prior art has clear advantage and beneficial effect, by technique scheme, a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst of the present invention can reach suitable technological progress and practicality, and there is the extensive value in industry, it at least has the advantage that
(1) present invention is enriched with each operation wash water, pipe leakage, workshop are rinsed and all have valency waste water, lose little, and waste water reuse or qualified discharge after environmental protection equipment processes, and environmental pollution is little.
(2) present invention adopts high temperature leaching with pressure, compared with traditional High Temperature High Pressure solvent extraction method, and the temperature and pressure that the present invention need not be significantly high, reduce safety coefficient, leaching solid-to-liquid ratio is little, saves reagent, and cost is little.
(3) method that the present invention adopts wet-cleaning, pulverizing, leaching, decomposition, can at utmost reduce loss, improves the response rate, and the tungsten loss of extract technology is about 3%, and the tungsten loss of ion-exchange step is about 3%, it is ensured that high-recovery.
(4) response rate of ammonium paratungstate of the present invention is up to 89%, the good product quality of recovery, meets social need, and more saves cost, has great economic benefit, social benefit and environmental benefit.
In sum, a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst of the present invention has significant progress technically, and has obvious good effect, is really a new and innovative, progressive, practical new design.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention, and can be practiced according to the content of description, and in order to the above and other purpose of the present invention, feature and advantage can be become apparent, below especially exemplified by preferred embodiment, and coordinate accompanying drawing, describe in detail as follows.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
For further setting forth that the present invention reaches technological means and effect that predetermined goal of the invention is taked, below in conjunction with accompanying drawing and preferred embodiment, to a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst proposed according to the present invention, its detailed description of the invention, structure, feature and effect thereof, describe in detail as after.
The present invention is a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst, including the pretreatment of SCR dead catalyst, fine grinding; High temperature leaching with pressure; Leached mud washing, wash water reclaim; Leachate remove impurity, leachate and wash water enter ion-exchange unit enrichment; Producing of ammonium paratungstate; Wastewater treatment and renovation.
Specifically include following steps:
(1), SCR dead catalyst is crushed, add water and wash away dust, foreign material, it is milled to 150-180 order after drying, it is then fed in the sodium hydroxide solution that concentration is 200g/L, high temperature leaching with pressure, controls temperature and is 110-120 DEG C during leaching, leaching pressure is 0.2-0.3MPa, extraction time is 2-3 hour, and leaching solid-to-liquid ratio is 2-4m3/ t, after leaching, solid-liquid separation obtains filtering residue and leaching liquid, gained filtering residue deionized water wash, washes away sodium therein, tungsten, vanadium, and wash water reclaims;
(2), be 9.5-10.5 by step (1) gained leaching liquid salt adding acid for adjusting pH value, filter, remove silica gel impurity;
(3), the wash water that the filtrate after step (2) remove impurity and step (1) are reclaimed adds hydrochloric acid adjustment pH value is 3-4, it is then fed into ion-exchange unit, obtains the mixed solution containing ammonium paratungstate and ammonium metavanadate through ion exchange, parsing operation;
(4), by step (3) gained mixed solution regulating pH is 9, adds ammonium chloride, then adjusts the temperature to 80 DEG C, naturally cool to room temperature after reacting 1 hour, separates with centrifuge, collect filtrate after precipitated crystal;
(5) filtrate, by step (4) collected directly obtains order of ammoniumparatungstate crystal with reactor evaporative crystallization, then separates with centrifuge, is dried by gained order of ammoniumparatungstate crystal.
Preferably, in above-mentioned process, the mixed liquor that step (3) adds 5mol/L ammonium chloride with 2mol/L ammonia resolves, and in the desorbed solution obtained, tungsten, vanadium total content control at more than 60g/L, and the pH value of gained desorbed solution controls at 8-10.
Preferably, in above-mentioned process, the ion-exchange unit described in step (3) adopts steel lining to mould ion exchange column, and the specification of described ion exchange column is diameter 1.4m, high 7m, and the quantity of ion exchange column is 4; Ion exchange adopts serial column absroption mode, and resin adopts D314 type, and every post feeds 6 tons, amounts to 24 tons.
The waste water entrance ion-exchange unit process of gained tungstenic, vanadium in the recovery process of the present invention, all the other waste water enters environmental protection equipment and processes, and the waste water after process can direct reuse or qualified discharge.
Above-mentioned a kind of process reclaiming tungsten from honeycomb fashion SCR dead catalyst, is respectively provided with many saving graces for technical staff of the same trade now, and really has technological progress.
The above, it it is only presently preferred embodiments of the present invention, not the present invention is done any pro forma restriction, although the present invention is disclosed above with preferred embodiment, but it is not limited to the present invention, any those skilled in the art, without departing within the scope of technical solution of the present invention, when the technology contents of available the disclosure above makes a little change or is modified to the Equivalent embodiments of equivalent variations, in every case it is the content without departing from technical solution of the present invention, according to any simple modification that above example is made by the technical spirit of the present invention, equivalent variations and modification, all still fall within the scope of technical solution of the present invention.
Claims (6)
1. the process reclaiming tungsten from honeycomb fashion SCR dead catalyst, it is characterised in that it comprises the following steps:
(1), SCR dead catalyst is crushed, add water and wash away dust, foreign material, it is milled to 150-180 order after drying, it is then fed in the sodium hydroxide solution that concentration is 200g/L, high temperature leaching with pressure, controlling temperature during leaching and be 110-120 DEG C, leaching pressure is 0.2-0.3MPa, and leaching solid-to-liquid ratio is 2-4m3/ t, after leaching, solid-liquid separation obtains filtering residue and leaching liquid, gained filtering residue deionized water wash, washes away sodium therein, tungsten, vanadium, and wash water reclaims;
(2), be 9.5-10.5 by step (1) gained leaching liquid salt adding acid for adjusting pH value, filter, remove silica gel impurity;
(3), the wash water that the filtrate after step (2) remove impurity and step (1) are reclaimed adds hydrochloric acid adjustment pH value is 3-4, it is then fed into ion-exchange unit, obtains the mixed solution containing ammonium paratungstate and ammonium metavanadate through ion exchange, parsing operation;
(4), by step (3) gained mixed solution regulating pH is 9, adds ammonium salt, then adjusts the temperature to 80 DEG C, naturally cool to room temperature after reacting 1 hour, and solid-liquid separation after precipitated crystal collects filtrate;
(5), the filtrate evaporative crystallization that step (4) is collected is obtained order of ammoniumparatungstate crystal.
2. the process of recovery Pd from honeycomb fashion SCR dead catalyst as claimed in claim 1, it is characterised in that step (1) extraction time is 2-3 hour.
3. the recovery process of honeycomb fashion SCR dead catalyst as claimed in claim 1, it is characterized in that step (3) 2mol/L ammonia adds the mixed liquor parsing of 5mol/L ammonium chloride, in the desorbed solution obtained, tungsten, vanadium total content control at more than 60g/L, and the pH value of gained desorbed solution controls at 8-10.
4. the recovery process of honeycomb fashion SCR dead catalyst as claimed in claim 1, it is characterized in that the ion-exchange unit described in step (3) adopts steel lining to mould ion exchange column, the specification of described ion exchange column is diameter 1.4m, high 7m, and the quantity of ion exchange column is 4; Ion exchange adopts serial column absroption mode, and resin adopts D314 type, and every post feeds 6 tons, amounts to 24 tons.
5. the recovery process of honeycomb fashion SCR dead catalyst as claimed in claim 1, it is characterised in that the ammonium salt described in step (4) is ammonium chloride, solid-liquid separation method adopts centrifuge to separate.
6. the recovery process of honeycomb fashion SCR dead catalyst as claimed in claim 1, it is characterised in that the filtrate in step (5) directly uses reactor evaporative crystallization, then separates with centrifuge, and crystal is dried.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108359799A (en) * | 2018-03-09 | 2018-08-03 | 王永平 | A kind of method of green reclaim titanium containing tungsten vanadium catalyst |
| CN110923459A (en) * | 2019-12-29 | 2020-03-27 | 江苏龙清环境技术有限公司 | Method for recovering titanium-tungsten powder from waste SCR catalyst |
| CN111217394A (en) * | 2020-02-18 | 2020-06-02 | 厦门钨业股份有限公司 | high-Fischer low-apparent-density ammonium paratungstate and production method and equipment thereof |
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| CN102936039A (en) * | 2012-11-15 | 2013-02-20 | 攀枝花市晟天钛业有限公司 | Recovery process of honeycomb type selective catalytic reduction (SCR) waste catalyst containing tungsten, vanadium and titanium |
| CN104232902A (en) * | 2014-09-03 | 2014-12-24 | 陈敏 | Method for recycling tungsten, molybdenum, aluminum and cobalt from waste catalyst through wet process |
| CN104630482A (en) * | 2015-01-13 | 2015-05-20 | 漯河兴茂钛业股份有限公司 | Alkali-leaching ion exchange method for comprehensively utilizing waste denitrification catalyst |
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- 2016-01-21 CN CN201610041873.6A patent/CN105624406A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102936039A (en) * | 2012-11-15 | 2013-02-20 | 攀枝花市晟天钛业有限公司 | Recovery process of honeycomb type selective catalytic reduction (SCR) waste catalyst containing tungsten, vanadium and titanium |
| CN104232902A (en) * | 2014-09-03 | 2014-12-24 | 陈敏 | Method for recycling tungsten, molybdenum, aluminum and cobalt from waste catalyst through wet process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108359799A (en) * | 2018-03-09 | 2018-08-03 | 王永平 | A kind of method of green reclaim titanium containing tungsten vanadium catalyst |
| CN110923459A (en) * | 2019-12-29 | 2020-03-27 | 江苏龙清环境技术有限公司 | Method for recovering titanium-tungsten powder from waste SCR catalyst |
| CN111217394A (en) * | 2020-02-18 | 2020-06-02 | 厦门钨业股份有限公司 | high-Fischer low-apparent-density ammonium paratungstate and production method and equipment thereof |
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Application publication date: 20160601 |