CN104445300A - Method of preparing magnesium hydroxide and calcium carbonate and separating out phosphorus ores by taking phosphate tailings as raw materials through ammonia circulation process - Google Patents
Method of preparing magnesium hydroxide and calcium carbonate and separating out phosphorus ores by taking phosphate tailings as raw materials through ammonia circulation process Download PDFInfo
- Publication number
- CN104445300A CN104445300A CN201410744065.7A CN201410744065A CN104445300A CN 104445300 A CN104445300 A CN 104445300A CN 201410744065 A CN201410744065 A CN 201410744065A CN 104445300 A CN104445300 A CN 104445300A
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- China
- Prior art keywords
- phosphorus
- calcium carbonate
- magnesium
- mine tailing
- calcium
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/20—Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/01—Treating phosphate ores or other raw phosphate materials to obtain phosphorus or phosphorus compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
Abstract
The invention provides a method of preparing magnesium hydroxide and calcium carbonate and separating out phosphorus ores by taking phosphate tailings as raw materials through an ammonia circulation process. The method can be used for preparing three products, namely magnesium hydroxide, calcium carbonate and phosphorus ores by sufficiently utilizing residual tailings after raw phosphorus ore separating through circulation of ammonia. The method has the characteristics of low cost, simple process and good product quality, and is used for providing an effective utilization way for utilizing the industrial waste phosphate tailings.
Description
Art
The invention belongs to chemical field, is a kind ofly effectively be separated the calcium in waste phosphorus mine tailing, magnesium, phosphoric and produce the method for the product such as magnesium hydroxide, calcium carbonate.
Background technology
Phosphorus mine tailing is a kind of trade waste of discharging after carrying out flotation to phosphorus ore raw ore, i.e. waste residue.Along with the produced quantity of phosphorus ore increases, the quantity of mine tailing also shockingly increases (if every 700,000 tons of raw ores are after selected, producing 20 ~ 300,000 tons of phosphorus mine tailings).
Because P2O5 content is low in phosphorus mine tailing, the detrimental impurity such as magnesium, calcium content is higher, and utility value is very low, and pile up like a mountain to can not get effective phosphorus mine tailing processed for a long time, causes serious pollution to environment, is again the one waste of resource.
Meanwhile, containing abundant magnesium in phosphorus mine tailing, content of magnesia up to about 18%, and containing a certain amount of Vanadium Pentoxide in FLAKES (content 5 ~ 9%), in addition containing elements such as calcium, manganese, antimony, copper, iron, aluminium, fluorine, is a kind of rare rich magnesium resource.To the comprehensive utilization of mine tailing, can turn waste into wealth on the one hand, magnesium, phosphor resource can be reclaimed, three waste discharge can be reduced on the other hand, reduce the pollution to environment, avoid mine tailing to pile up land occupation simultaneously, to the second stage employ and the recycling economy target that realize resource, there is important society and economic implications.
Magnesium hydroxide is a kind of Chemicals with extensive use, large with its resiliency, active large, high adsorption capacity, the advantage such as nontoxic, remove agent, stack desulfurization agent, soil treatment with simulated acid rain and pH value regulator as heavy metal in the neutralizing agent of field of Environment Protection industry acid-bearing wastewater, industrial and mining enterprises and mine discharge.And magnesium hydroxide is high due to heat decomposition temperature, has and better press down the effects such as cigarette, waste water neutralize, desulfurization, progressively replace the inorganic anti-flaming material such as aluminium hydroxide and weisspiessglanz and be applied in refractory materials, pottery, high performance corrosion-proof coating.
The preparation of magnesium hydroxide, bittern, seawater, rhombspar, magnesite etc. can be adopted as magnesium source, by high-temperature calcination, and use alkaline matter to carry out chemical precipitation, as obtained products such as ammonia precipitation, lime precipitation, caustic soda precipitations, generally need consume a large amount of heat energy and rely on sufficient magnesium source.
To the utilization of phosphorus mine tailing, means process phosphorus mine tailings such as adopting calcining, digestion, carbonization, pyrolysis is had to make magnesium oxide " CN102674407A "; Have and adopt high-temperature calcination phosphorus mine tailing, then add ferrosilicon and fluorite batching, finally reduction obtains MAGNESIUM METAL " CN102534254A "; Or phosphorus mine tailing is at high temperature calcined, digested, carbon filter, filtrate adds hydrofluoric acid, obtains magnesium fluoride and calcium carbonate product product " CN102923739A ".
Summary of the invention
The present invention will solve the difficulty that comprehensive utilization means are few, processing costs is too high of phosphorus mine tailing, the valuable magnesium source utilized in phosphorus mine tailing is proposed, the magnesium hydroxide products of production high added value and high-purity calcium carbonate also isolate the method for phosphorus ore, the method have cost low, make full use of waste resource and by product, the simple feature of technique.
In order to realize above-mentioned order ground; the technical scheme that the present invention takes is: with phosphorus mine tailing be raw material ammonia circulation method preparing magnesium hydroxide, calcium carbonate isolate the method for phosphorus concentrate; comprise the following steps: (1) calcines: phosphorus mine tailing is at 850 ~ 1050 DEG C of temperature lower calcinations; after calcining, in phosphorus mine tailing, calcium and magnesium are decomposed into calcium oxide and magnesium oxide, and phosphatic rock does not decompose at this temperature; (2) digest: the phosphorus mine tailing after calcining, with ammonium chloride solution digestion, obtain Digestive system.Now calcium oxide and magnesium oxide are changed into as calcium hydroxide and magnesium hydroxide by water digestion; (3) ammonium solution: hot digestion liquid, to boiling, steams ammonia, calcium hydroxide and magnesium hydroxide change calcium chloride and magnesium chloride into simultaneously, deposit in the solution; (4) filter: ammonium solution terminates rear filtering separation, and filter residue is phosphorus concentrate, and filtrate is calcium chloride and magnesium chloride solution; (5) calcium carbonate processed: pass into carbonic acid gas and ammonia or ammoniacal liquor in calcium chloride and magnesium chloride solution, controls PH well, separates out precipitation of calcium carbonate; (6) filter: filtering separation obtains calcium carbonate solid, filtrate is the solution of ammonium chloride, magnesium chloride and a small amount of calcium chloride; (7) hydrogen manufacturing magnesium oxide: be separated the filtrate after calcium carbonate, add ammoniacal liquor or ammonia, separates out magnesium hydrate precipitate; (8) filter: filtering separation obtains magnesium hydroxide solid, filtrate is ammonium chloride solution and still containing magnesium chloride and calcium chloride, continues to recycle; (9) dry and refine: the calcium carbonate obtained and magnesium hydroxide, being finished product through drying, or further refining.
Embodiment 1: get 100 grams of phosphorus mine tailings, calcines after 1.5 hours, adds 500ml water and clear up, then add 90g ammonium chloride, be heated to boil at 1000 DEG C, after ammonia still process completely, treats cold filtration, obtains filter residue and be phosphorus concentrate.Filtrate 400ml adds volatile salt 20g, and obtain calcium carbonate 25g after separating out sedimentation and filtration, filtrate adds ammoniacal liquor again, and filter after precipitation, obtain magnesium hydroxide 10g, mother liquor continues to recycle.
Claims (7)
1. with phosphorus mine tailing be raw material ammonia circulation method preparing magnesium hydroxide, calcium carbonate isolate the method for phosphorus concentrate; it is characterized in that comprising the following steps: (1) calcines: phosphorus mine tailing is at 850 ~ 1050 DEG C of temperature lower calcinations; after calcining, in phosphorus mine tailing, calcium and magnesium are decomposed into calcium oxide and magnesium oxide, and phosphatic rock does not decompose at this temperature; (2) digest: the phosphorus mine tailing after calcining, with ammonium chloride solution digestion, obtain Digestive system, now calcium oxide and magnesium oxide are changed into as calcium hydroxide and magnesium hydroxide by water digestion; (3) ammonium solution: hot digestion liquid, to boiling, steams ammonia, calcium hydroxide and magnesium hydroxide change calcium chloride and magnesium chloride into simultaneously, deposit in the solution; (4) filter: ammonium solution terminates rear filtering separation, and filter residue is phosphorus concentrate, and filtrate is calcium chloride and magnesium chloride solution; (5) calcium carbonate processed: pass into carbonic acid gas and ammonia or ammoniacal liquor in calcium chloride and magnesium chloride solution, controls PH well, separates out precipitation of calcium carbonate; (6) filter: filtering separation obtains calcium carbonate solid, filtrate is the solution of ammonium chloride, magnesium chloride and a small amount of calcium chloride; (7) hydrogen manufacturing magnesium oxide: be separated the filtrate after calcium carbonate, add ammoniacal liquor or ammonia, separates out magnesium hydrate precipitate; (8) filter: filtering separation obtains magnesium hydroxide solid, filtrate is ammonium chloride solution and still containing magnesium chloride and calcium chloride, continues to recycle; (9) dry and refine: the calcium carbonate obtained and magnesium hydroxide, being finished product through drying, or further refining.
2. claim 1 with phosphorus mine tailing be raw material ammonia circulation method preparing magnesium hydroxide, calcium carbonate isolate the method for phosphorus concentrate, it is characterized in that described phosphorus mine tailing is the mine tailing of the low-grade Vanadium Pentoxide in FLAKES discharged after phosphorus ore obtains higher-grade Vanadium Pentoxide in FLAKES concentrate in ore dressing process, this phosphorus mine tailing is in the dry state containing P
2o
5be 2% ~ 10%, MgO be 15% ~ 22%, CaO be 28% ~ 42%.
3. claim 1 with phosphorus mine tailing be raw material ammonia circulation method preparing magnesium hydroxide, calcium carbonate isolate the method for phosphorus concentrate, it is characterized in that institute's ammonia recycles, only must supplement the ammonia of a small amount of loss.
4. claim 3 with phosphorus mine tailing be raw material ammonia circulation method preparing magnesium hydroxide, calcium carbonate isolate the method for phosphorus concentrate, the ammonia that it is characterized in that analysing magnesium and carbonation stage comes from the ammonia that the ammonia still process stage discharges, and the ammonium chloride required for the ammonia still process stage is from mother liquor.
5. claim 1 with phosphorus mine tailing be raw material ammonia circulation method preparing magnesium hydroxide, calcium carbonate isolate the method for phosphorus concentrate, it is characterized in that institute's carbon dioxide recycle uses, only must supplement the carbonic acid gas of a small amount of loss or the balance by maintenance carbonic acid gas of adjusting the product mix.
6. claim 5 with phosphorus mine tailing be raw material ammonia circulation method preparing magnesium hydroxide, calcium carbonate isolate the method for phosphorus concentrate, it is characterized in that the carbonic acid gas that the carbonic acid gas of carbonation stage needs comes from calcination stage and discharges.
7. claim 1 with phosphorus mine tailing be raw material ammonia circulation method preparing magnesium hydroxide, calcium carbonate isolate the method for phosphorus concentrate, it is characterized in that obtaining magnesium hydroxide, calcium carbonate two products obtain phosphorus concentrate simultaneously, realize the synchronous utilization of calcium in mine tailing, magnesium, phosphorus three kinds of elements.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410744065.7A CN104445300A (en) | 2014-11-14 | 2014-12-09 | Method of preparing magnesium hydroxide and calcium carbonate and separating out phosphorus ores by taking phosphate tailings as raw materials through ammonia circulation process |
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| CN201410638301 | 2014-11-14 | ||
| CN2014106383017 | 2014-11-14 | ||
| CN201410744065.7A CN104445300A (en) | 2014-11-14 | 2014-12-09 | Method of preparing magnesium hydroxide and calcium carbonate and separating out phosphorus ores by taking phosphate tailings as raw materials through ammonia circulation process |
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| CN104445300A true CN104445300A (en) | 2015-03-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410722798.0A Pending CN105584998A (en) | 2014-11-13 | 2014-12-04 | Method for preparing disodium hydrogen phosphate by adopting raffinate of melamine purified phosphoric acid |
| CN201410744065.7A Pending CN104445300A (en) | 2014-11-14 | 2014-12-09 | Method of preparing magnesium hydroxide and calcium carbonate and separating out phosphorus ores by taking phosphate tailings as raw materials through ammonia circulation process |
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| CN201410722798.0A Pending CN105584998A (en) | 2014-11-13 | 2014-12-04 | Method for preparing disodium hydrogen phosphate by adopting raffinate of melamine purified phosphoric acid |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828793A (en) * | 2015-05-06 | 2015-08-12 | 贵州省化工研究院 | Method for extracting phosphor concentrate from phosphor tailings and co-producing magnesium-containing calcium carbonate |
| CN104860279A (en) * | 2015-05-06 | 2015-08-26 | 贵州省化工研究院 | Method for extracting phosphate concentrate from phosphate tailings and cooperatively producing calcium ammonium nitrate and magnesium ammonium sulphate |
| CN104860277A (en) * | 2015-05-06 | 2015-08-26 | 贵州省化工研究院 | Medium and low grade phosphorus ore magnesium removal treatment method |
| CN104860334A (en) * | 2015-05-06 | 2015-08-26 | 贵州省化工研究院 | Processing method for improving quality of medium and low grade phosphorus ore and recycling calcium magnesium |
| CN108314584A (en) * | 2018-03-14 | 2018-07-24 | 贵州芭田生态工程有限公司 | A method of the tailing generated using nitrophosphate fertilizer filter residue, calcium ammonium nitrate filter residue, phosphate rock floating prepares soil conditioner |
| CN109264686A (en) * | 2018-10-16 | 2019-01-25 | 贵州盛源新材料股份有限公司 | A kind of technique that calcium carbonate, magnesium hydroxide are recycled simultaneously by mid low grade phosphate rock or phosphorus tailing enrichment phosphorus concentrate |
| CN109354050A (en) * | 2018-10-24 | 2019-02-19 | 沈阳辰兴化工技术有限公司 | A kind of method and device preparing calcium carbonate and magnesium hydroxide using dolomite |
| CN110106370A (en) * | 2019-05-16 | 2019-08-09 | 攀枝花学院 | The method of vanadium-bearing slag of high calcium and high phosphor pretreatment decalcification dephosphorization |
| CN110872105A (en) * | 2018-08-31 | 2020-03-10 | 贵州芭田生态工程有限公司 | Method for efficiently leaching calcium and magnesium ions in phosphorite |
| CN111302372A (en) * | 2019-12-31 | 2020-06-19 | 黔南民族师范学院 | Method for separating and extracting magnesium and calcium from phosphate tailings treated by secondary ammonium salt |
| CN112694115A (en) * | 2021-01-11 | 2021-04-23 | 湖北三宁化工股份有限公司 | Method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings |
| CN114348980A (en) * | 2022-01-20 | 2022-04-15 | 贵州芭田生态工程有限公司 | Method for enriching phosphate concentrate and simultaneously recovering calcium nitrate and magnesium nitrate from phosphate ore |
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| CN103566726B (en) * | 2013-11-05 | 2016-02-03 | 彭振超 | Calcined dolomite in powder denitrating flue gas desulfurization preparing magnesium hydroxide, magnesia and gypsum method |
| CN103738986B (en) * | 2013-12-20 | 2016-03-09 | 周骏宏 | A kind of dolomite calcination water-soluble separating calcium and magnesium produce the method for magnesium hydroxide and calcium carbonate |
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| CN1008353B (en) * | 1987-03-09 | 1990-06-13 | 华东化工学院 | Production method of sodium hydrogen phosphate from sodium chloride |
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| CN102225775A (en) * | 2011-05-13 | 2011-10-26 | 河北科技大学 | Process for producing magnesium hydroxide and calcium carbonate by dolomite conversion method |
| CN103011630A (en) * | 2012-12-26 | 2013-04-03 | 新疆蓝天镁业股份有限公司 | Method of producing high-purity magnesium hydroxide and magnesium oxide by low-grade magnesite |
| CN104071818A (en) * | 2013-10-28 | 2014-10-01 | 黔南民族师范学院 | Method for separating calcium, magnesium and phosphorus elements from phosphate tailings by adopting water leaching and ammonium leaching |
| CN103566726B (en) * | 2013-11-05 | 2016-02-03 | 彭振超 | Calcined dolomite in powder denitrating flue gas desulfurization preparing magnesium hydroxide, magnesia and gypsum method |
| CN103738986B (en) * | 2013-12-20 | 2016-03-09 | 周骏宏 | A kind of dolomite calcination water-soluble separating calcium and magnesium produce the method for magnesium hydroxide and calcium carbonate |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828793A (en) * | 2015-05-06 | 2015-08-12 | 贵州省化工研究院 | Method for extracting phosphor concentrate from phosphor tailings and co-producing magnesium-containing calcium carbonate |
| CN104860279A (en) * | 2015-05-06 | 2015-08-26 | 贵州省化工研究院 | Method for extracting phosphate concentrate from phosphate tailings and cooperatively producing calcium ammonium nitrate and magnesium ammonium sulphate |
| CN104860277A (en) * | 2015-05-06 | 2015-08-26 | 贵州省化工研究院 | Medium and low grade phosphorus ore magnesium removal treatment method |
| CN104860334A (en) * | 2015-05-06 | 2015-08-26 | 贵州省化工研究院 | Processing method for improving quality of medium and low grade phosphorus ore and recycling calcium magnesium |
| CN108314584A (en) * | 2018-03-14 | 2018-07-24 | 贵州芭田生态工程有限公司 | A method of the tailing generated using nitrophosphate fertilizer filter residue, calcium ammonium nitrate filter residue, phosphate rock floating prepares soil conditioner |
| CN110872105A (en) * | 2018-08-31 | 2020-03-10 | 贵州芭田生态工程有限公司 | Method for efficiently leaching calcium and magnesium ions in phosphorite |
| CN109264686A (en) * | 2018-10-16 | 2019-01-25 | 贵州盛源新材料股份有限公司 | A kind of technique that calcium carbonate, magnesium hydroxide are recycled simultaneously by mid low grade phosphate rock or phosphorus tailing enrichment phosphorus concentrate |
| CN109354050A (en) * | 2018-10-24 | 2019-02-19 | 沈阳辰兴化工技术有限公司 | A kind of method and device preparing calcium carbonate and magnesium hydroxide using dolomite |
| CN110106370A (en) * | 2019-05-16 | 2019-08-09 | 攀枝花学院 | The method of vanadium-bearing slag of high calcium and high phosphor pretreatment decalcification dephosphorization |
| CN111302372A (en) * | 2019-12-31 | 2020-06-19 | 黔南民族师范学院 | Method for separating and extracting magnesium and calcium from phosphate tailings treated by secondary ammonium salt |
| CN112694115A (en) * | 2021-01-11 | 2021-04-23 | 湖北三宁化工股份有限公司 | Method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings |
| CN114348980A (en) * | 2022-01-20 | 2022-04-15 | 贵州芭田生态工程有限公司 | Method for enriching phosphate concentrate and simultaneously recovering calcium nitrate and magnesium nitrate from phosphate ore |
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| CN105584998A (en) | 2016-05-18 |
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Application publication date: 20150325 |