CN1180100C - Method for producing manganese carbonate by utilizing manganese sulfate in waste manganese ore leaching slag - Google Patents
Method for producing manganese carbonate by utilizing manganese sulfate in waste manganese ore leaching slag Download PDFInfo
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- CN1180100C CN1180100C CNB001132970A CN00113297A CN1180100C CN 1180100 C CN1180100 C CN 1180100C CN B001132970 A CNB001132970 A CN B001132970A CN 00113297 A CN00113297 A CN 00113297A CN 1180100 C CN1180100 C CN 1180100C
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- manganese
- carbonate
- waste
- soluble
- slag
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- 239000011572 manganese Substances 0.000 title claims abstract description 42
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 37
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 title claims abstract description 35
- 239000002893 slag Substances 0.000 title claims abstract description 30
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 title claims abstract description 24
- 239000002699 waste material Substances 0.000 title claims abstract description 24
- 239000011702 manganese sulphate Substances 0.000 title claims abstract description 17
- 235000007079 manganese sulphate Nutrition 0.000 title claims abstract description 17
- 239000011656 manganese carbonate Substances 0.000 title claims abstract description 13
- 235000006748 manganese carbonate Nutrition 0.000 title claims abstract description 13
- 229940093474 manganese carbonate Drugs 0.000 title claims abstract description 13
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 title claims abstract description 13
- 238000002386 leaching Methods 0.000 title claims description 13
- 229940099596 manganese sulfate Drugs 0.000 title claims description 13
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 7
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 3
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 12
- 238000003860 storage Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 229910001424 calcium ion Inorganic materials 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 150000004673 fluoride salts Chemical class 0.000 claims 2
- 239000002244 precipitate Substances 0.000 claims 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical group S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 229910052979 sodium sulfide Inorganic materials 0.000 claims 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical group [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims 1
- 150000004763 sulfides Chemical class 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 2
- 235000010755 mineral Nutrition 0.000 abstract description 2
- 239000011707 mineral Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000001117 sulphuric acid Substances 0.000 abstract 3
- 235000011149 sulphuric acid Nutrition 0.000 abstract 3
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 16
- 239000000243 solution Substances 0.000 description 14
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 235000010265 sodium sulphite Nutrition 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 235000021050 feed intake Nutrition 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000000247 postprecipitation Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Processing Of Solid Wastes (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to a method for producing manganese carbonate from recycling manganese sulphate in waste manganese ore extract slag. The present invention solves the problem that environment pollution is caused by soluble manganese sulphate, and sufficiently utilized mineral resources. In the method of the present invention, waste extract slag which is left after manganese ore powder is leached by sulphuric acid for preparing sulphuric acid solution is used as raw material, and manganese sulphate solution in waste manganese ore extract slag which is leached by water is recovered. After impurities are removed, the manganese sulphate solution reacts with soluble carbonate solution (such as ammonium bicarbonate) to produce manganese carbonate, and other corresponding manganese products are prepared by the manganese carbonate. The method is suitable for various manufacturers which produce manganese products with manganese ore powder and sulphuric acid as raw material.
Description
Technical field
The present invention relates to a kind of method of producing manganous carbonate, particularly a kind of waste manganese mud that utilizes soaks the method that the manganous sulfate in the slag is produced manganous carbonate.
Background technology
Manganous sulfate, electrolytic metal Mn, the production of manganese goods such as electrolytic manganese dioxide, all be earlier manganese carbonate ore (rhodochrosite) to be used sulfuric acid to leach, make manganese sulfate solution, behind impurity removal and purification, be used for producing various corresponding manganese goods again, waste manganese mud behind sulfuric acid to leach soaks in the slag, and the manganese sulfate solution that contains weight about 30% own has been drained as refuse together in company with soaking slag.Through measuring and calculating, an electrolytic manganese dioxide factory that produces 10000 tons per year soaks the manganous sulfate that emits the slag from giving up and be converted to pure manganese up to more than 700 tons every year; Produce 3000 tons of electrolytic manganese factories per year for one, annual pure manganese of from soak slag, draining also up to 150 tons about.This has not only greatly wasted valuable Mineral resources, and the useless solubility manganous sulfate that soaks in the slag is returned environment and brought very big pollution.It is few that waste manganese mud soaks the manganese sulfate solution relative quantity of carrying secretly in the slag, though reclaiming with water extraction is most economical way, but because the manganese sulfate solution after reclaiming is very rare, add the manganese sulfate solution that reclaims is also wanted purification refine, the more cost that makes of operation is higher, and is if will reclaim the production that liquid is directly used in electrolytic metal Mn or electrolytic manganese dioxide, then very uneconomical economically, therefore, all manganese goods factories of China all do not recycle the manganous sulfate that waste manganese mud soaks in the slag to be carried secretly.Estimate not following 5000 tons of the annual pure manganese of wasting therefrom.So, if can solve the recycling waste manganese mud effectively and soak the manganous sulfate of carrying secretly in the slag, manganese resource is fully used, and can obtains favorable economic benefit, can also reduce environmental pollution simultaneously, its economy and society meaning is all very great.
Summary of the invention
The object of the present invention is to provide a kind of technology simple, the waste manganese mud that utilizes that production cost is low soaks the method that the manganous sulfate in the slag is produced manganous carbonate.
The objective of the invention is to realize by following approach: utilize waste manganese mud to soak the method that the manganous sulfate in the slag is produced manganous carbonate, it is to adopt following step:
1) will leach the waste manganese mud behind the manganese sulfate solution soaks in the leaching groove jar of slag input belt stirrer, add the 1-4 water doubly soak slag weight, add solubility villiaumite and dissolvable sulfide, make that calcium ions is lower than 20PPM in the solution, metal ion is lower than 10PPM, fully stirs; Described solubility villiaumite is a Neutral ammonium fluoride, and described dissolvable sulfide is a sodium sulphite;
2) stir leaching about 0.5 hour, after the filtration filtrate beaten to the high-order storage tank I standby;
3) with the soluble carbon hydrochlorate with deionized water by weight 180: 2000 or 100: 1500 dissolving, filter the back and beat extremely among the high-order storage tank II standby; Described carbonate is bicarbonate of ammonia;
4) under agitation, manganese sulfate solution among header tank I and the II and carbonate solution are injected reaction kettle for reaction simultaneously with the thread shape, its consumption is 1 by manganous sulfate and carbonate mol ratio: (1-6) feed intake, behind reinforced the finishing, continue stirring reaction about 0.5 hour;
5) with the reactant centrifugation, throw out is changed in the rinse bath, add deionized water, agitator treating is after 10 minutes, centrifuging, post precipitation repeats above-mentioned adding deionized water and stirring washing, centrifuging operation 2-3 time again;
6) will wash good throw out 55-60 ℃ of oven dry down, obtain manganese carbonate product.
The present invention utilizes waste manganese mud to soak manganous sulfate in the slag, and to produce the method technology of manganous carbonate simple, used device is few, employing is with water extraction, adding fluorochemical and sulfide removal of impurities carries out simultaneously, make technical process simple, the manganous sulfate that employing leaches out with soluble carbon acid salt solution precipitation becomes the method for manganese carbonate product, has solved in the infusion manganous sulfate and has crossed rare and difficulty that be difficult to recycle; It is the various purity of raw material production manganous carbonate that the manganese carbonate product that adopts this method to produce can reach with electrolytic metal Mn, and cost has only the latter half.This method be applicable to all various be the raw material production manganous sulfate with sulfuric acid and manganese ore powder, electrolytic metal Mn, the producer of electrolytic manganese dioxide and all relevant manganese goods uses.
Embodiment
With embodiment the present invention is described in further detail below:
Embodiment 1: soaking slag with the waste manganese mud of electrolytic manganese dioxide factory is that raw material is implemented method of the present invention:
The manganous sulfate refined soln concentration of electrolytic manganese dioxide factory is about 140gMn/L, and waste manganese mud soaks the manganous sulfate concentration of carrying secretly in the slag with 100gMn/L, and its proportion d=1.5 calculates.
Get waste manganese mud and soak 3 tons of inputs of slag 8M
3In the leaching can, add 4 tons of entry, start agitator, add 2Kg sodium sulphite, (calcium in the check leaching solution and copper, lead, cadmium, the isoionic content of mercury, as add Neutral ammonium fluoride or sodium sulphite when not reaching requirement), stir after 30 minutes, will leach thing pressure filter press filtration, (not limpid as solution, carry out the press filtration second time or vacuum filtration), refined liquid is squeezed among the high-order storage tank I standby with pump.
Take by weighing bicarbonate of ammonia 180Kg,, beat to the high-order storage tank II solution standby with filtration pump with deionized water 2 tons of dissolvings.
Manganese sulfate solution among the high-order storage tank I is put half (about 2 tons) to volume 8M
3Reactor in, start agitator, under the normal temperature, the ammonium bicarbonate soln among manganese sulfate solution among the high-order storage tank I and the high-order storage tank II is injected reactor simultaneously with constant speed.Feed intake finish after, continued stirring reaction 20 minutes, after the natural subsidence, the venting supernatant liquid, lower sediment changes the whizzer centrifugation over to, changes precipitation over to 1M then
3In the rinse bath, add deionized water 300Kg agitator treating after 10 minutes, centrifuging, precipitation is again with above-mentioned adding deionized water and stirring, centrifugal filtering method washing 2 times, the product that centrifugation obtains is put into enamel or Stainless Steel Disc, 55-60 ℃ of oven dry down, gets about manganese carbonate product 75Kg, quality can reach GB10503-89 I-III type, and the rate of recovery of manganous carbonate is about 75%.
Embodiment 2: raw material still soaks slag for the waste manganese mud with electrolytic manganese dioxide factory
Get waste manganese mud and soak 3 tons of slags, drop into 8M
3In the leaching can, add 4 tons of entry, start agitator and stir after 20 minutes, with pressure filter press filtration (not adding fluorochemical or sulfide).Each step is all identical with embodiment 1 later on.Can get about manganese carbonate product 75Kg, quality is the general industry manganous carbonate, and the rate of recovery of manganous carbonate is about 75%.
Embodiment 3: soaking slag with the waste manganese mud of electrolytic metal Mn factory is raw material
The manganous sulfate refined soln concentration of electrolytic manganese dioxide factory is about 38gMn/L, and waste manganese mud soaks the manganous sulfate concentration of carrying secretly in the slag with 35g/L, and its proportion d=1.3 calculates.
Get waste manganese mud and soak 3 tons of slags, drop into 8M
3In the leaching can, add 4 tons of entry, all the other operations are all carried out (wherein the bicarbonate of ammonia consumption is 100Kg, adds 1.5 tons of dissolvings of water) by embodiment 1.Can get about manganese carbonate product 30Kg GB10503-89 I-III type.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001132970A CN1180100C (en) | 2000-02-28 | 2000-02-28 | Method for producing manganese carbonate by utilizing manganese sulfate in waste manganese ore leaching slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001132970A CN1180100C (en) | 2000-02-28 | 2000-02-28 | Method for producing manganese carbonate by utilizing manganese sulfate in waste manganese ore leaching slag |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1311340A CN1311340A (en) | 2001-09-05 |
| CN1180100C true CN1180100C (en) | 2004-12-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001132970A Expired - Fee Related CN1180100C (en) | 2000-02-28 | 2000-02-28 | Method for producing manganese carbonate by utilizing manganese sulfate in waste manganese ore leaching slag |
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| Country | Link |
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| CN (1) | CN1180100C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260797A (en) * | 2011-07-22 | 2011-11-30 | 湘潭电化集团有限公司 | Production process for reclaiming manganese from manganese-containing waste water and waste slag by using waste gas |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101579685B (en) * | 2009-06-10 | 2010-10-27 | 重庆大学 | A method for processing and utilizing electrolytic manganese waste residue |
| CN101704555A (en) * | 2009-07-20 | 2010-05-12 | 贵州红星发展股份有限公司 | Method for circularly purifying manganese sulfate and manganese carbonate |
| CN101704553B (en) * | 2009-07-20 | 2012-11-07 | 贵州红星发展股份有限公司 | Method for preparing manganese carbonate |
| CN102839286A (en) * | 2012-09-26 | 2012-12-26 | 中信锦州金属股份有限公司 | Method for recycling bivalent manganese in electrolytic manganese leached residues |
| CN102887545B (en) * | 2012-10-15 | 2014-09-24 | 兰州大学 | Method for preparing electronic grade manganese carbonate from manganese copper zinc cobalt calcium chloride solution |
| CN103789542B (en) * | 2014-01-20 | 2015-10-07 | 中南大学 | A kind of wet reducing leaching method of manganese oxide mineral |
| CN105481019B (en) * | 2015-12-18 | 2017-05-24 | 长沙矿冶研究院有限责任公司 | Method for removing alkaline-earth metal and heavy metal impurities in manganese sulfate solution |
| CN108752059B (en) * | 2018-07-04 | 2021-05-11 | 重庆市地质矿产测试中心 | Method for producing forest silicon-calcium-manganese composite mineral fertilizer by using manganese slag |
| CN109097578A (en) * | 2018-07-17 | 2018-12-28 | 重庆上甲电子股份有限公司 | A method of manganese carbonate is produced using aniline reduction electrolytic manganese anode mud |
| CN110127766A (en) * | 2019-07-02 | 2019-08-16 | 贵州中伟资源循环产业发展有限公司 | A kind of preparation process of LITHIUM BATTERY manganese sulfate solution |
-
2000
- 2000-02-28 CN CNB001132970A patent/CN1180100C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260797A (en) * | 2011-07-22 | 2011-11-30 | 湘潭电化集团有限公司 | Production process for reclaiming manganese from manganese-containing waste water and waste slag by using waste gas |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1311340A (en) | 2001-09-05 |
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