CN102923739A - Method for utilizing high-magnesium phosphate tailings to produce magnesium fluoride and by-product calcium carbonate - Google Patents
Method for utilizing high-magnesium phosphate tailings to produce magnesium fluoride and by-product calcium carbonate Download PDFInfo
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- CN102923739A CN102923739A CN2012104461652A CN201210446165A CN102923739A CN 102923739 A CN102923739 A CN 102923739A CN 2012104461652 A CN2012104461652 A CN 2012104461652A CN 201210446165 A CN201210446165 A CN 201210446165A CN 102923739 A CN102923739 A CN 102923739A
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Abstract
The invention discloses a method for utilizing high-magnesium phosphate tailings to produce magnesium fluoride and by-product calcium carbonate. The method comprises the following steps: calcinating the high-magnesium phosphate tailings at high temperature to form calcined dolomite, adding water to the calcined dolomite to perform digestion to obtain digestion solution, supplementing water to the digestion solution and then leading carbon dioxide to perform a carbonization reaction to obtain carbonized liquid, separating bottom phosphate ore sediments of the carbonized liquid after the reaction stops, filtering, and obtaining filtrate which is magnesium bicarbonate aqueous solution, and obtaining a calcium carbonate product after drying a filter cake; adding hydrofluoric acid in the obtained magnesium bicarbonate aqueous solution, filtering after the reaction, washing, and obtaining a magnesium fluoride product after drying the filter cake, The industrial waste high-magnesium phosphate tailings serve as raw materials, waste is turned into wealth, abundant magnesium calcium resources in the high-magnesium phosphate tailings are fully utilized to produce the magnesium fluoride and the by-product calcium carbonate, and the method has the advantages of being simple in process, low in production cost and basically free of three wastes.
Description
Technical field
The present invention relates to fluorochemical, specifically a kind of method of utilizing discarded object height magnesium phosphorus mine tailing production magnesium fluoride and by-product calcium carbonate.
Background technology
Magnesium fluoride is colourless crystallization or white powder, it is a kind of important Inorganic Chemicals, of many uses, can be used as the raw material of making pottery, glass, hot pressing crystal, fusing assistant as metal smelting aluminium and magnesium, as welding compound, as the agent that is being coated with of pigment, also can be used for preparing precise parts such as fluorescent material in various eyeglasses in the opticinstrument and filter coating, the negative ray screen etc. in the welding.
The conventional production methods of magnesium fluoride is to adopt different magnesium salts and hydrofluoric acid reaction, mainly contains magnesiumcarbonate method, magnesium oxide method and sal epsom method etc.Because magnesium salts purity directly affects the magnesium fluoride quality, thereby affect the use range of magnesium fluoride, and highly purified magnesium salts can directly raise the price of magnesium fluoride, just seems and extremely is necessary so seek a kind of new purity is high, cost is low magnesium salts, has important practical significance.
To be Rock Phosphate (72Min BPL) obtain byproduct behind the phosphorus concentrate, its P by the ore-dressing technique enrichment to high magnesium phosphorus mine tailing
2O
5Content is that 2%～8.5%, MgO content is that 15%～21%, CaO content is 28%～38%, belongs to high magnesium low-grade phosphorus ore, and magnesium resource is abundant.For the dressing-works of producing 3000000 tons of phosphorus concentrate per year, annually produce about 1,000,000 tons high magnesium phosphorus mine tailing, contain 180,000 tons the MgO of having an appointment.For a long time, because this mine tailing is phosphorous lower, utilize approach few, usually be used as waste by enterprise and adopt the mode of storing up to process, the magnesium resource in this mine tailing is wasted, go back land occupation, pollute surrounding enviroment.Through retrieval, there is no up to now and utilize the patent application that magnesium resource is produced magnesium fluoride and by-product calcium carbonate in the high magnesium phosphorus mine tailing, there is not relevant report yet.
Summary of the invention
The object of the invention is to overcome above-mentioned shortcoming and a kind of method of utilizing discarded object height magnesium phosphorus mine tailing to produce magnesium fluoride and by-product calcium carbonate is provided, magnesium calcium resource in the high magnesium phosphorus of the method energy effective recycling mine tailing has the advantages that technique is simple, production cost is low, substantially produce without the three wastes.
For achieving the above object, the technical solution used in the present invention is: a kind of method of utilizing high magnesium phosphorus mine tailing to produce magnesium fluoride and by-product calcium carbonate may further comprise the steps:
(1) with high magnesium phosphorus mine tailing 850～1180 ℃ of lower calcinings, burn till forge white;
(2) the described Bai Yushui that forges is mixed 1:4～40 in mass ratio, digested 10～100 minutes 20～90 ℃ of lower stirrings of temperature, obtain Digestive system;
(3) in described Digestive system make up water to make the Digestive system solid content be massfraction 2%～15%, passing into the gas that contains carbonic acid gas in the Digestive system carries out carburizing reagent and obtains carbodiimide solution again under 10～35 ℃, be down to 6.6～8.0 o'clock stopped reaction in the pH of carbodiimide solution value, carbodiimide solution is separated rear filtration of bottom Rock Phosphate (72Min BPL) precipitation, filtrate is heavy magnesium water, and the filter cake drying namely gets calcium carbonate product;
(4) add hydrofluoric acid in the heavy magnesium water that obtains, in 10～90 ℃ of lower mix and blend reactions of temperature, the reaction times is no less than 30 minutes, Mg in the mixed reaction solution
2+, F
-The stoichiometry mol ratio be Mg
2+: F
-Filter after the reaction=1:1.8～2.2, washing, and filtrate is recycled, and the filter cake drying namely gets the magnesium fluoride product.
Above-mentioned high magnesium phosphorus mine tailing is that phosphorus ore obtains the mineral that contain low-grade Vanadium Pentoxide in FLAKES that discharge behind the phosphorus concentrate of higher-grade Vanadium Pentoxide in FLAKES in ore dressing process, contains P
2O
5Be that 2%～10%, MgO is that 15%～21%, CaO is 28%～42%.
The above-mentioned gas that contains carbonic acid gas is the gas of 20%～100% carbonic acid gas volume fraction.
Principle of the present invention: high magnesium phosphorus mine tailing mainly is by rhombspar (CaMg (CO
3)
2) and a small amount of fluorapatite composition, the white main component of forging after high-temperature calcination is CaO, MgO and fluorapatite, adds water digestion, and fluorapatite does not react, and CaO, MgO mainly generate calcium hydroxide and magnesium hydroxide, pass into CO
2Gas carries out carbonization, and calcium hydroxide generates the light calcium carbonate suspended substance, and magnesium hydroxide then generates Magnesium hydrogen carbonate and enters liquid phase, after carbonization finishes, carbodiimide solution is separated rear filtration of bottom Rock Phosphate (72Min BPL) precipitation, and filtrate is heavy magnesium water (being magnesium bicarbonate solution), and filter cake is calcium carbonate.Add hydrofluoric acid and namely react the generation magnesium fluoride in the filtrate heavy magnesium water, its reaction formula is as follows:
Mg(HCO
3)
2?+?2HF?=?MgF
2?+?2CO
2↑?+?2H
2O
Because heavy magnesium water is the less magnesium bicarbonate solution of foreign matter content, so the purity of the magnesium fluoride that makes is higher, quality is better.
The present invention is take industrial waste object height magnesium phosphorus mine tailing as raw material, and utilization of waste material takes full advantage of magnesium calcium resource abundant in the high magnesium phosphorus mine tailing and produces magnesium fluoride and by-product calcium carbonate, and technique is simple, and production cost is low.The present invention produces without the three wastes substantially, meet to clean manufacturing technique requirent, has solved the problem of the high magnesium phosphorus of raw material mine tailing land occupation resource, contaminate environment, turns waste into wealth, and has good economic benefit and important environment protection significance.The technology of the present invention can be applied to a large amount of processing of high magnesium phosphorus mine tailing, processes high magnesium phosphorus mine tailing for the Rock Phosphate (72Min BPL) exploitation with Mineral Processing Enterprises a kind of effective ways are provided.
Embodiment
Specific implementation process of the present invention is as follows:
A kind of method of utilizing high magnesium phosphorus mine tailing to produce magnesium fluoride and by-product calcium carbonate, it may further comprise the steps:
1) be P with chemical ingredients
2O
52%～10%, the high magnesium phosphorus mine tailing of MgO15%～21%, CaO28%～42% under 850～1180 ℃, be sintered into forge white;
2) the described Bai Yushui that forges is mixed 1:4～40 in mass ratio, digested 10～100 minutes 20～90 ℃ of lower stirrings of temperature, obtain Digestive system;
3) in described Digestive system make up water to make the Digestive system solid content be massfraction 2%～15%, passing into the gas that contains carbonic acid gas in the Digestive system carries out carburizing reagent and obtains carbodiimide solution again under 10～35 ℃, be down to 6.6～8.0 o'clock stopped reaction in the pH of carbodiimide solution value, carbodiimide solution is separated rear filtration of bottom Rock Phosphate (72Min BPL) precipitation, filtrate is heavy magnesium water, and the filter cake drying namely gets calcium carbonate product;
4) add hydrofluoric acid in the heavy magnesium water that obtains, in 10～90 ℃ of lower mix and blend reactions of temperature, the reaction times is no less than 30 minutes, Mg in the mixed reaction solution
2+, F
-The stoichiometry mol ratio be Mg
2+: F
-Filter after the reaction=1:1.8～2.2, washing, and filtrate is recycled, and the filter cake drying namely gets the magnesium fluoride product.
For the ease of understanding the present invention, below examples of implementation set forth content of the present invention, content of the present invention is not limited only to the following examples.
Embodiment 1
High magnesium phosphorus mine tailing chemical ingredients: P
2O
57.04%, MgO16.86%, CaO37.48%
Take by weighing tail magnesium phosphorus mine tailing 100g 980 ℃ of lower calcinings, obtain forging white 61.4g.Forge white and 700g water 80 ℃ of lower stirrings 40 minutes, obtain Digestive system.In Digestive system, replenish 800g water, the gas that passes into again 35% carbonic acid gas volume fraction in the Digestive system carries out carburizing reagent and obtains carbodiimide solution under 20 ℃, be down to 6.7 o'clock stopped reaction in the pH of carbodiimide solution value, carbodiimide solution is separated rear filtration of bottom Rock Phosphate (72Min BPL) precipitation, filtrate is heavy magnesium water, and the filter cake drying namely gets calcium carbonate product; In the heavy magnesium water that obtains, add hydrofluoric acid, mix and blend reaction under temperature 50 C, 50 minutes reaction times, Mg in the mixed reaction solution
2+, F
-The stoichiometry mol ratio be Mg
2+: F
-=1:2 filters after the reaction, washing, and filtrate is recycled, and the filter cake drying namely gets the magnesium fluoride product.
Embodiment 2
High magnesium phosphorus mine tailing chemical ingredients: P
2O
56.00%, MgO18.25%, CaO36.82%
Take by weighing tail magnesium phosphorus mine tailing 100g 950 ℃ of lower calcinings, obtain forging white 59.8g, forge white and 500g water 80 ℃ of lower stirrings 30 minutes, obtain Digestive system.In Digestive system, replenish 600g water, the gas that passes into again 30% carbonic acid gas volume fraction in the Digestive system carries out carburizing reagent and obtains carbodiimide solution under 25 ℃, be down to 6.9 o'clock stopped reaction in the pH of carbodiimide solution value, carbodiimide solution is separated rear filtration of bottom Rock Phosphate (72Min BPL) precipitation, filtrate is heavy magnesium water, and the filter cake drying namely gets calcium carbonate product; In the heavy magnesium water that obtains, add hydrofluoric acid, at 10 ℃ of lower mix and blend reactions of temperature, 120 minutes reaction times, Mg in the mixed reaction solution
2+, F
-The stoichiometry mol ratio be Mg
2+: F
-=1:1.8 filters after the reaction, washing, and filtrate is recycled, and the filter cake drying namely gets the magnesium fluoride product.
Embodiment 3
High magnesium phosphorus mine tailing chemical ingredients: P
2O
56.35%, MgO18.59%, CaO37.01%
Take by weighing tail magnesium phosphorus mine tailing 100g 960 ℃ of lower calcinings, obtain forging white 60.5g, forge white and 430g water 85 ℃ of lower stirrings 30 minutes, obtain Digestive system.In Digestive system, replenish 900g water, the gas that passes into again 27% carbonic acid gas volume fraction in the Digestive system carries out carburizing reagent and obtains carbodiimide solution under 30 ℃, be down to 6.8 o'clock stopped reaction in the pH of carbodiimide solution value, carbodiimide solution is separated rear filtration of bottom Rock Phosphate (72Min BPL) precipitation, filtrate is heavy magnesium water, and the filter cake drying namely gets calcium carbonate product; In the heavy magnesium water that obtains, add hydrofluoric acid, at 90 ℃ of lower mix and blend reactions of temperature, 30 minutes reaction times, Mg in the mixed reaction solution
2+, F
-The stoichiometry mol ratio be Mg
2+: F
-=1:2.2 filters after the reaction, washing, and filtrate is recycled, and the filter cake drying namely gets the magnesium fluoride product.
Embodiment 4
High magnesium phosphorus mine tailing chemical ingredients: P
2O
59.84%, MgO15.03%, CaO41.79%
Take by weighing tail magnesium phosphorus mine tailing 100g 1180 ℃ of lower calcinings, obtain forging white 65.3g, forge white and 262g water 90 ℃ of lower stirrings 100 minutes, obtain Digestive system.In Digestive system, replenish 110g water, the gas that passes into again 20% carbonic acid gas volume fraction in the Digestive system carries out carburizing reagent and obtains carbodiimide solution under 10 ℃, be down to about 8.0 o'clock stopped reaction in the pH of carbodiimide solution value, carbodiimide solution is separated rear filtration of bottom Rock Phosphate (72Min BPL) precipitation, filtrate is heavy magnesium water, and the filter cake drying namely gets calcium carbonate product; In the heavy magnesium water that obtains, add hydrofluoric acid, at 30 ℃ of lower mix and blend reactions of temperature, 70 minutes reaction times, Mg in the mixed reaction solution
2+, F
-The stoichiometry mol ratio be Mg
2+: F
-=1:1.9 filters after the reaction, washing, and filtrate is recycled, and the filter cake drying namely gets the magnesium fluoride product.
Embodiment 5
High magnesium phosphorus mine tailing chemical ingredients: P
2O
52.15%, MgO20.93%, CaO28.15%
Take by weighing tail magnesium phosphorus mine tailing 100g 850 ℃ of lower calcinings, obtain forging white 56.4g, forge white and 2256g water 20 ℃ of lower stirrings 10 minutes, obtain Digestive system.In Digestive system, replenish 508g water, the gas that passes into again 99% carbonic acid gas volume fraction in the Digestive system carries out carburizing reagent and obtains carbodiimide solution under 22 ℃, be down to about 6.6 o'clock stopped reaction in the pH of carbodiimide solution value, carbodiimide solution is separated rear filtration of bottom Rock Phosphate (72Min BPL) precipitation, filtrate is heavy magnesium water, and the filter cake drying namely gets calcium carbonate product; In the heavy magnesium water that obtains, add hydrofluoric acid, at 40 ℃ of lower mix and blend reactions of temperature, 60 minutes reaction times, Mg in the mixed reaction solution
2+, F
-The stoichiometry mol ratio be Mg
2+: F
-=1:2.1 filters after the reaction, washing, and filtrate is recycled, and the filter cake drying namely gets the magnesium fluoride product.
Claims (3)
1. method of utilizing high magnesium phosphorus mine tailing to produce magnesium fluoride and by-product calcium carbonate is characterized in that it is comprised of following steps:
(1) with high magnesium phosphorus mine tailing 850～1180 ℃ of lower calcinings, burn till forge white;
(2) the described Bai Yushui that forges is mixed 1:4～40 in mass ratio, digested 10～100 minutes 20～90 ℃ of lower stirrings of temperature, obtain Digestive system;
(3) in described Digestive system make up water to make the Digestive system solid content be massfraction 2%～15%, passing into the gas that contains carbonic acid gas in the Digestive system carries out carburizing reagent and obtains carbodiimide solution again under 10～35 ℃, be down to 6.6～8.0 o'clock stopped reaction in the pH of carbodiimide solution value, carbodiimide solution is separated rear filtration of bottom Rock Phosphate (72Min BPL) precipitation, filtrate is heavy magnesium water, and the filter cake drying namely gets calcium carbonate product;
(4) add hydrofluoric acid in the heavy magnesium water that obtains, in 10～90 ℃ of lower mix and blend reactions of temperature, the reaction times is no less than 30 minutes, Mg in the mixed reaction solution
2+, F
-The stoichiometry mol ratio be Mg
2+: F
-Filter after the reaction=1:1.8～2.2, washing, and filtrate is recycled, and the filter cake drying namely gets the magnesium fluoride product.
2. the described method of utilizing high magnesium phosphorus mine tailing to produce magnesium fluoride and by-product calcium carbonate according to claim 1, it is characterized in that described high magnesium phosphorus mine tailing is that phosphorus ore obtains the mineral that contain low-grade Vanadium Pentoxide in FLAKES that discharge behind the phosphorus concentrate of higher-grade Vanadium Pentoxide in FLAKES in ore dressing process, contains P
2O
5Be that 2%～10%, MgO is that 15%～21%, CaO is 28%～42%.
3. the described method of utilizing high magnesium phosphorus mine tailing to produce magnesium fluoride and by-product calcium carbonate according to claim 1 is characterized in that the described gas that contains carbonic acid gas is the gas of 20%～100% carbonic acid gas volume fraction.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN109133018A (en) * | 2018-08-29 | 2019-01-04 | 石门县金子山新材料科技有限公司 | A kind of technique that difficulty selects low grade collophanite to comprehensively utilize |
| CN109354000A (en) * | 2018-10-09 | 2019-02-19 | 湖南化工职业技术学院（湖南工业高级技工学校） | A kind of method of High-Mg phosphate tailings enrichment co-production precipitated calcium carbonate and magnesium hydroxide |
| CN113087496A (en) * | 2021-03-01 | 2021-07-09 | 武汉科技大学 | Magnesium-calcium material taking phosphate tailings as main raw material and preparation method thereof |
| CN115141941A (en) * | 2022-06-27 | 2022-10-04 | 中铝郑州有色金属研究院有限公司 | Comprehensive utilization method of dolomite |
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| CN102653408A (en) * | 2012-05-20 | 2012-09-05 | 瓮福（集团）有限责任公司 | Method for producing light-weight magnesium carbonate by using phosphate tailings with high magnesium content |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN109133018A (en) * | 2018-08-29 | 2019-01-04 | 石门县金子山新材料科技有限公司 | A kind of technique that difficulty selects low grade collophanite to comprehensively utilize |
| CN109354000A (en) * | 2018-10-09 | 2019-02-19 | 湖南化工职业技术学院（湖南工业高级技工学校） | A kind of method of High-Mg phosphate tailings enrichment co-production precipitated calcium carbonate and magnesium hydroxide |
| CN113087496A (en) * | 2021-03-01 | 2021-07-09 | 武汉科技大学 | Magnesium-calcium material taking phosphate tailings as main raw material and preparation method thereof |
| CN115141941A (en) * | 2022-06-27 | 2022-10-04 | 中铝郑州有色金属研究院有限公司 | Comprehensive utilization method of dolomite |
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Application publication date: 20130213 |