CN102943174A - Method for preparing nickel sulfide concentrate through titanium dioxide waste acids - Google Patents
Method for preparing nickel sulfide concentrate through titanium dioxide waste acids Download PDFInfo
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- CN102943174A CN102943174A CN2012104741507A CN201210474150A CN102943174A CN 102943174 A CN102943174 A CN 102943174A CN 2012104741507 A CN2012104741507 A CN 2012104741507A CN 201210474150 A CN201210474150 A CN 201210474150A CN 102943174 A CN102943174 A CN 102943174A
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- titanium white
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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
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Abstract
The invention provides a method for preparing nickel sulfide concentrate through titanium dioxide waste acids. The specific technical scheme includes that waste acids produced in the nickel sulfide industry are used for immersing nickel laterite ore, assistants are added after warming, agitation and digestion are performed for a certain time, compressed air or oxygen is blown in, filtration is performed after a certain period, a vulcanizing agent is added after the filtration solution is heated to a designated temperature, and filtration is performed again after agitation and heat preservation are performed for a certain period to obtain the nickel sulfide concentrate. The method is an effective way to use titanium dioxide waste acids comprehensively, wastes are turned into treasures, the cost used by a wet process to process metallic nickel can be reduced, air pollution is reduced, and good economic benefits can be produced.
Description
Technical field
The invention provides a kind of method of being produced nickel sulfide concentrate by titanium white waste acid, belong to industrial waste acid comprehensive utilization and hydrometallurgy field.
Background technology
Titanium dioxide is widely used in the fields such as coating, plastics, printing ink, papermaking, makeup, is the outer important a kind of industrial chemicals of Now Domestic.The nearly various schools of thinkers titanium powder plant overwhelming majority of China adopts Production By Sulfuric Acid Process at present, and 1 ton of titanium dioxide of the every production of this production technique will produce the spent acid about 8～10 ton 20% according to statistics.Like this large spent acid of amount, if directly discharging, will serious environment pollution, so must process spent acid and can discharge after up to standard.
At present existing lot of documents and the processing of patent report titanium white waste acid and the method for recycling.Reduce the refining plant of content of inorganic acid in finished acid of waste sulfuric acid concentration system for titanium dioxide such as patent CN202272737U(), a kind of refining plant that reduces content of inorganic acid in finished acid of waste sulfuric acid concentration system for titanium dioxide is disclosed, comprise ripening tank, ripening tank is the ripening tank of two series connection, wherein second ripening tank is for treating filter pocket, the subsider of 3～4 interval type operations is set behind filter pocket, subsider top arranges the transfer lime that clear liquor enters the finished product acid tank, the bottom throw out outlet of subsider communicates with plate-and-frame filter press through pump, and the plate-and-frame filter press purified liquor outlet communicates with subsider.Patent CN101538021(recycles method and the device thereof that titanium dioxide waste acid by sulfuric acid process is produced the vitriol oil), relate to a kind of method and device thereof that the rare spent acid of titanium white is produced the vitriol oil that reclaim, at first, dilute sulphuric acid is carried out pre-concentrate, remove most of impurity that rare spent acid brings by precipitation, the make up water that sulfuric acid after pre-concentrate, removal of impurities is replaced sulfuric acid production system, add in the sulfuric acid circulation groove of sulfuric acid absorption tower, absorb sulphur trioxide through sulfuric acid absorption tower, produce the vitriol oil, thereby reach the purpose that dilute sulphuric acid is reclaimed.Patent CN2897369(efficient titanium pigment waste acid concentrator) provides a kind of efficient titanium pigment waste acid concentrator, be comprised of waste acid concentration pipeline, oily heating circuit, warm air pipeline, described waste acid concentration pipeline is to be made of spent acid groove, primary acids pump, graphite heat exchanger, residual evaporator, secondary acid pump, oil heating vacuum evaporator and freezing and crystallizing groove.The method of this class concentration and recovery spent acid has solved the recycling problem of titanium white waste acid to a certain extent, but the method equipment investment of concentration and recovery spent acid is large, erosion resistance to equipment requires high, and adopt evaporation concentration production high density sulphur energy consumption larger, cause the recycling cost compare high, and reclaim concentration and be difficult to reach requirement, can't fully recovering in production.The neutralization discharging refers to add in spent acid in the neutralizing agents such as lime or calcium carbonate and spent acid, the waste liquor PH value is reached or approaching neutral rear discharging, these class methods produce the gypsum of a large amount of low values, because the gypsum purposes is few, face again the competition with other gypsum manufacturing enterprises, therefore market is the comparison hard problem, and a large amount of gypsum store up and transportation cost higher, can make the production cost of sulfate process titanium dioxide improve 10% ~ 15%.
And adopt titanium white waste acid to process different ores, and produce the method for corresponding noble metal, because production cost is low, the economic benefit of generation is large, will become the main direction of studying that will solve from now on the titanium white waste acid comprehensive utilization.The method of comprehensive utilization of patent CN101824542A(titanium dioxide waste acid by sulfuric acid process), the technical problem that solves of this invention has provided the method for comprehensive utilization of the lower titanium dioxide waste acid by sulfuric acid process of a kind of cost.The method of comprehensive utilization of this invention titanium dioxide waste acid by sulfuric acid process is: adopt the ore blending titanium white waste acid that contains cupric oxide or zinc oxide, filter and obtain copper sulfate and solution of zinc sulfate; Prepare copper sponge with iron powder reducing copper sulfate, the zinc sulfate electrolysis makes metallic zinc, qualified discharge after the waste liquid usefulness lime neutralizing treatment after preparation copper sponge gained waste liquid or the zinc sulfate electrolysis.Patent CN102092793A(processes the method that Waste Sulfuric Acid prepares high purity manganese sulfate and hydrate thereof with rhodochrosite), take full advantage of the Waste Sulfuric Acid that rhodochrosite comes the process for producing titanium dioxide to produce, first that the rhodochrosite pulverizing is rear with hydrochloric acid with its contained manganese lixiviate out, then react with the Waste Sulfuric Acid that the production titanium dioxide produces with soaking body fluid, turn waste into wealth, when having administered environmental pollution Waste Sulfuric Acid is transformed into the manganous sulfate with very high economic worth, create considerable economic worth.Patent CN101787546A(is produced the method for electrolytic metal Mn by titanium white waste acid), the technical problem that this invention solves provided a kind of production cost lower produce the method for electrolytic metal Mn by titanium white waste acid.The method is that manganese ore, sulfurous iron ore and the titanium white waste acid that will contain Manganse Dioxide add in the reaction vessel, and reacting by heating is filtered, and purifies, and electrolysis obtains manganese metal and vitriolated waste electrolyte at last.Above patent can both be successfully applied to titanium white waste acid the smelting of noble metal, create considerable economic worth, but also exist deficiency, must carry out to use behind the purification and impurity removal to titanium white waste acid such as some product, and there is a large amount of ferro elements in the ore, and the copper sulfate that reaction generates through spent acid, zinc sulfate, manganous sulfates etc. are soluble in water equally with ferric sulfate, remove de-iron relatively more difficult, separating-purifying copper sulfate, zinc sulfate, the manganous sulfate expense is very high, and need large number quipments, have high input, subsequent production also can produce Waste Sulfuric Acid, is faced with equally the again processing problem of spent acid.
Summary of the invention
The purpose of this invention is to provide a kind of deficiency that solves existing titanium white waste acid comprehensive utilization technique, specially grind through pains, proposed a kind of method of processing titanium white waste acid, namely adopt titanium white waste acid digestion of laterite nickel minerals, produce nickel sulfide concentrate.The present invention does not need the titanium dioxide waste acid by sulfuric acid process removal of impurities, reduce waste acid concentration, cleaning section, only needed in the production process to add auxiliary agent and pass into air, just can reach the leaching that reduces ferro element, reduce the content of iron in the leach liquor, reach the effect that improves nickel recovery.It is low that the present invention produces the nickel sulfide concentrate cost, and the vulcanizing agent consumption is few, pollutes few.
The present invention was achieved in that and adopts titanium white waste acid to mix with red soil nickel ore, begins the lixiviate that heats up behind the furnishing pulpous state, 60～110 ℃ of lower stirring and leaching 20～120 minutes, add auxiliary agent, regulate pH=0.5～4.5, then be blown into pressurized air or oxygen under the heat-retaining condition, continue reaction and filter after 0.5～5 hour, filtrate is put into reactor, start stirring and be heated to 40～100 ℃, add vulcanizing agent, continue stirring and also be incubated 0.5～5 hour, filter, filter residue is nickel sulfide concentrate.
The titanium white waste acid weight concentration of telling is 10%～30%, and the consumption of spent acid is 2～7 times of red soil nickel ore.
Described lixiviate mode is the normal pressure lixiviate.
Described auxiliary agent is one or more compositions in vitriolate of tartar, Repone K, saltpetre, potassium hydroxide, potassiumphosphate, sodium sulfate, sodium-chlor, SODIUMNITRATE, sodium hydroxide, sodium phosphate, ammonium sulfate, ammonium chloride, ammonium nitrate and the ammonium phosphate, and add-on is 1～15% of red soil nickel ore weight.
Described adjusting pH adopts alkaline matter, and described alkaline matter is a kind of in sodium hydroxide, ammoniacal liquor, yellow soda ash, sodium bicarbonate and the calcium carbonate or their composition.
Described filter type is that direct filtration or cooling are filtered.
Described vulcanizing agent is a kind of in sulfurated lime, magnesium sulfide, barium sulphide, Iron sulfuret, aluminium sulfide, zinc sulphide, cupric sulfide, manganese sulfide, lead sulfide, tin sulfide and ammonium sulfide and their disulphide or the polysulfide or their composition; The weight that adds vulcanizing agent is 0.5～5 times of nickel ion content in the filtrate.
Compared with prior art, the present invention has the following advantages:
1, adopt titanium white waste acid to replace common sulfuric acid digestion of laterite nickel minerals to produce nickel sulfide concentrate, solved the difficult problem of spent acid comprehensive utilization, production cost is low, and equipment used is simple.
2, titanium white waste acid directly fully utilizes, and does not need to be concentrated to finite concentration, does not also need purification and impurity removal, has reduced concentrated, treating plant, has reduced energy consumption.
3, the lixiviate later stage adds auxiliary agent and oxygenant, has greatly reduced iron leaching, has reduced the content of iron in the vat liquor, makes vat liquor need not to carry out in addition deironing and processes, and reduces deferrization process, reduces and produces work intensity.
4, adopt special vulcanizing agent, avoided the release of hydrogen sulfide in the conversion process, both protected workshop and atmospheric environment, reduced again the loss of vulcanizing agent, reduce production costs.
Description of drawings
Fig. 1 is the present invention is produced nickel sulfide concentrate by the titanium white waste liquid process flow sheet.
Embodiment
All acid and the content of nickel are weight content among the embodiment 1(embodiment)
1000Kg laterite nickel, the titanium white waste acid of adding 3500Kg22% is opened and is stirred the furnishing pulpous state, be warmed up to 80 ℃, normal pressure stirring and leaching 45 minutes adds 150Kg sodium sulfate solid, add sodium hydroxide and regulate pH=4.2, be blown into pressurized air, continue reaction 1.5 hours, filter after cooling to 40 ℃, filtrate is put into reactor, is heated to 80 ℃ under stirring, add 280Kg powdery Iron sulfuret, insulation reaction cools to 50 ℃ after 3 hours, filters, filter residue is nickel sulfide concentrate, and nickel content is 11.5%.
Embodiment 2
1000Kg laterite nickel, the titanium white waste acid of adding 5200Kg15% is opened and is stirred the furnishing pulpous state, be warmed up to 80 ℃, normal pressure stirring and leaching 60 minutes adds the 100Kg solid potassium chloride, add sodium hydroxide and regulate pH=3.0, be blown into pressurized air, continue reaction 2 hours, filter, filtrate is put into reactor, is heated to 90 ℃ under stirring, add 300Kg powdery sulfurated lime, insulation reaction cools to 50 ℃ after 3 hours, filters, filter residue is nickel sulfide concentrate, and nickel content is 8.3%.
Embodiment 3
1000Kg laterite nickel, the titanium white waste acid of adding 5200Kg18% is opened and is stirred the furnishing pulpous state, be warmed up to 80 ℃, normal pressure stirring and leaching 60 minutes adds the 100kg ammonium sulfate solids, add sodium hydroxide and regulate pH=3.0, be blown into pressurized air, continue reaction 2 hours, filter, filtrate is put into reactor, is heated to 90 ℃ under stirring, add 300Kg powdery ammonium sulfide and curing ammonium, insulation reaction cools to 50 ℃ after 3 hours, filters, filter residue is nickel sulfide concentrate, and nickel content is 13.1%.
Embodiment 4
1000Kg laterite nickel, the titanium white waste acid of adding 4500Kg20% is opened and is stirred the furnishing pulpous state, be warmed up to 80 ℃, normal pressure stirring and leaching 60 minutes adds 60Kg yellow soda ash and 20kg ammonium phosphate solid, add sodium hydroxide and regulate pH=1.0, be blown into pressurized air, continue reaction 2 hours, filter, filtrate is put into reactor, is heated to 90 ℃ under stirring, add 210Kg powdery zinc sulphide, insulation reaction cools to 50 ℃ after 3 hours, filters, filter residue is nickel sulfide concentrate, and nickel content is 12.6%.
Embodiment 5
1000Kg laterite nickel, the titanium white waste acid that adds 6000Kg17%, open and stir the furnishing pulpous state, be warmed up to 110 ℃, normal pressure stirring and leaching 45 minutes adds 100Kg sodium-chlor and 50kg potassiumphosphate solid, adds sodium hydroxide and regulates pH=4.5, be blown into pressurized air, continue reaction 4 hours, filter, filtrate is put into reactor, be heated to 95 ℃ under stirring, add the mixture of 280Kg powdery ammonium sulfide and zinc sulphide, insulation reaction cools to 50 ℃ after 3 hours, filters, filter residue is nickel sulfide concentrate, and nickel content is 15.8%.
Embodiment 6
1000Kg laterite nickel, the titanium white waste acid of adding 4500Kg15% is opened and is stirred the furnishing pulpous state, be warmed up to 100 ℃, normal pressure stirring and leaching 60 minutes adds 60Kg ammonium sulfate and 40kg sodium sulphite solid, add sodium hydroxide and regulate pH=1.5, be blown into pressurized air, continue reaction 2 hours, filter, filtrate is put into reactor, is heated to 90 ℃ under stirring, add 200Kg powdery zinc sulphide, insulation reaction cools to 50 ℃ after 3 hours, filters, filter residue is nickel sulfide concentrate, and nickel content is 13.6%.
Embodiment 7
1000Kg laterite nickel, the titanium white waste acid that adds 5000Kg21%, open and stir the furnishing pulpous state, be warmed up to 90 ℃, normal pressure stirring and leaching 70 minutes adds 60kg sodium sulfate and 20kg chloride solid, adds sodium hydroxide and regulates pH=4.2, be blown into pressurized air, continue reaction 2.5 hours, filter after cooling to 40 ℃, filtrate is put into reactor, be heated to 80 ℃ under stirring, add the mixture of 250Kg powdery barium sulfate and magnesium sulfide, insulation reaction cools to 50 ℃ after 3 hours, filters, filter residue is nickel sulfide concentrate, and nickel content is 12.5%.
The nickel sulfide concentrate that above-described embodiment obtains can be directly used in extracting metals nickel.
Claims (6)
1. method of being produced nickel sulfide concentrate by titanium white waste acid, it is characterized in that: adopt titanium white waste acid to mix with red soil nickel ore, behind the furnishing pulpous state, 60～110 ℃ of lower lixiviates 20～120 minutes, add auxiliary agent, regulate pH=0.5～4.5, then under heat-retaining condition, be blown into pressurized air or oxygen, continue reaction and filter after 0.5～5 hour, filtrate is put into reactor, starts stirring and is heated to 40～100 ℃, add vulcanizing agent, continue to stir and be incubated 0.5～5 hour, filter, filter residue is nickel sulfide concentrate;
Described titanium white waste acid weight concentration is 10～30%, and consumption is 2～7 times of red soil nickel ore.
2. the method for being produced nickel sulfide concentrate by titanium white waste acid according to claim 1, it is characterized in that: described lixiviate mode is the normal pressure lixiviate.
3. the method for being produced nickel sulfide concentrate by titanium white waste acid according to claim 1, it is characterized in that: described auxiliary agent is one or more compositions in vitriolate of tartar, Repone K, saltpetre, potassium hydroxide, potassiumphosphate, sodium sulfate, sodium-chlor, SODIUMNITRATE, sodium hydroxide, sodium phosphate, ammonium sulfate, ammonium chloride, ammonium nitrate and the ammonium phosphate, and add-on is 1～15% of red soil nickel ore weight.
4. the method for being produced nickel sulfide concentrate by titanium white waste acid according to claim 1, it is characterized in that: described adjusting pH adopts alkaline matter, and described alkaline matter is a kind of in sodium hydroxide, ammoniacal liquor, yellow soda ash, sodium bicarbonate and the calcium carbonate or their composition.
5. the method for being produced nickel sulfide concentrate by titanium white waste acid according to claim 1 is characterized in that: described filter type is that direct filtration or cooling are filtered.
6. the method for being produced nickel sulfide concentrate by titanium white waste acid according to claim 1 is characterized in that: described vulcanizing agent is a kind of in sulfurated lime, magnesium sulfide, barium sulphide, Iron sulfuret, aluminium sulfide, zinc sulphide, cupric sulfide, manganese sulfide, lead sulfide, tin sulfide, ammonium sulfide and their disulphide or the polysulfide or their composition; The weight that adds vulcanizing agent is 0.5～5 times of nickel ion content in the filtrate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012104741507A CN102943174A (en) | 2012-11-21 | 2012-11-21 | Method for preparing nickel sulfide concentrate through titanium dioxide waste acids |
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| CN2012104741507A CN102943174A (en) | 2012-11-21 | 2012-11-21 | Method for preparing nickel sulfide concentrate through titanium dioxide waste acids |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106676274A (en) * | 2016-11-21 | 2017-05-17 | 西北矿冶研究院 | Method for resource utilization of lead and zinc in high-iron and high-phosphorus-containing waste residues in steel wire rope industry |
| CN113073207A (en) * | 2021-03-23 | 2021-07-06 | 中国恩菲工程技术有限公司 | Method for extracting valuable metals from high-magnesium type laterite-nickel ore |
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| CN1329308C (en) * | 2005-07-15 | 2007-08-01 | 曹国华 | Method for obtaining nickel sulfide from pickled liquor of laterite nickel ore |
| CN101338377A (en) * | 2008-08-27 | 2009-01-07 | 中南大学 | High-efficiency leaching process of nickel from laterite-nickel ore |
| CN101541985A (en) * | 2006-09-06 | 2009-09-23 | 艾拉梅公司 | Process for the hydrometallurgical treatment of a lateritic nickel/cobalt ore and process for producing nickel and/or cobalt intermediate concentrates or commercial products using it |
| CN102260791A (en) * | 2011-07-29 | 2011-11-30 | 广西银亿科技矿冶有限公司 | Heap leaching method for red soil nickel ore |
| CN102732724A (en) * | 2012-07-06 | 2012-10-17 | 铜陵化学工业集团有限公司 | Method for removing iron from magnesium-containing pickle liquor obtained by leaching of serpentine with titanium dioxide waste acid |
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2012
- 2012-11-21 CN CN2012104741507A patent/CN102943174A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1329308C (en) * | 2005-07-15 | 2007-08-01 | 曹国华 | Method for obtaining nickel sulfide from pickled liquor of laterite nickel ore |
| CN101541985A (en) * | 2006-09-06 | 2009-09-23 | 艾拉梅公司 | Process for the hydrometallurgical treatment of a lateritic nickel/cobalt ore and process for producing nickel and/or cobalt intermediate concentrates or commercial products using it |
| CN101338377A (en) * | 2008-08-27 | 2009-01-07 | 中南大学 | High-efficiency leaching process of nickel from laterite-nickel ore |
| CN102260791A (en) * | 2011-07-29 | 2011-11-30 | 广西银亿科技矿冶有限公司 | Heap leaching method for red soil nickel ore |
| CN102732724A (en) * | 2012-07-06 | 2012-10-17 | 铜陵化学工业集团有限公司 | Method for removing iron from magnesium-containing pickle liquor obtained by leaching of serpentine with titanium dioxide waste acid |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106676274A (en) * | 2016-11-21 | 2017-05-17 | 西北矿冶研究院 | Method for resource utilization of lead and zinc in high-iron and high-phosphorus-containing waste residues in steel wire rope industry |
| CN106676274B (en) * | 2016-11-21 | 2018-09-28 | 西北矿冶研究院 | Method for resource utilization of lead and zinc in high-iron and high-phosphorus-containing waste residues in steel wire rope industry |
| CN113073207A (en) * | 2021-03-23 | 2021-07-06 | 中国恩菲工程技术有限公司 | Method for extracting valuable metals from high-magnesium type laterite-nickel ore |
| CN113073207B (en) * | 2021-03-23 | 2022-07-22 | 中国恩菲工程技术有限公司 | Method for extracting valuable metals from high-magnesium type laterite-nickel ore |
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Application publication date: 20130227 |