CN102600965A - Method for recycling phosphorus from phosphate tailings with high magnesium content - Google Patents
Method for recycling phosphorus from phosphate tailings with high magnesium content Download PDFInfo
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- CN102600965A CN102600965A CN2012100859105A CN201210085910A CN102600965A CN 102600965 A CN102600965 A CN 102600965A CN 2012100859105 A CN2012100859105 A CN 2012100859105A CN 201210085910 A CN201210085910 A CN 201210085910A CN 102600965 A CN102600965 A CN 102600965A
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- phosphorus
- mine tailing
- high magnesium
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Abstract
The invention discloses a method for recycling phosphorus from phosphate tailings with high magnesium content. The method includes following steps: (1) calcining the phosphate tailings with high magnesium content into calcined dolomite at the temperature ranging from 900 DEG C to 1200 DEG C; (2) mixing the calcined dolomite with water according to mass ratio of 1:4-40, and stirring mixture at the temperature ranging from 20 DEG C to 90 DEG C for 10 minutes to 100 minutes to obtain digestive liquor; (3) replenishing water into the digestive liquor so that mass fraction of solid content of the digestive liquor ranges from 2% to 15%, leading gas with carbon dioxide into the digestive liquor, performing carbonization reaction at the temperature ranging from 20 DEG C to 35 DEG C to obtain carbonized liquid, and stopping reaction when the pH (potential of hydrogen) value of the carbonized liquid lowers to 6.5-8.0; and (4) separating to obtain bottom precipitate of the carbonized liquid after the reaction is stopped. The bottom precipitate is hydrous phosphorite, and a ground phosphate rock product is obtained after the hydrous phosphorite is dried. The method can recycle phosphorus resources in the phosphate tailings with high magnesium content, phosphate recycling rate is high, the grade of obtained phosphorus products is high, and an economic benefit and an environmental benefit are remarkable.
Description
Technical field
The present invention relates to chemical technology field, specifically is a kind of method that from discarded object height magnesium phosphorus mine tailing, reclaims phosphorus.
Background technology
Phosphorus ore is a kind of important mineral resources, is mainly used in to produce phosphoric acid and phosphate fertilizer and phosphate product.Because the phosphorus ore great majority of China are mid low grade phosphate rock, generally need become commodity phosphorus concentrate through chemical flotation beneficiation and enrichment.To be rock phosphate in powder obtain the byproduct behind the phosphorus concentrate through floating and enriching to high magnesium phosphorus mine tailing, and its mineral thing is mainly dolomite and fluor-apatite mutually, its P
2O
5Content is 4%～8.5%, and MgO content is 15%～21%, belongs to high magnesium low-grade phosphorus ore.For the ore dressing plant of producing 3000000 tons of phosphorus concentrate per year, annually produce about 1,000,000 tons high magnesium phosphorus mine tailing, contain 5～70,000 tons the P of having an appointment
2O
5, be equivalent to the phosphorus content of about 200,000 tons phosphorus concentrate.For a long time, because this mine tailing is phosphorous lower, is used as discarded object by enterprise usually and adopts the mode of storing up to handle, the phosphor resource in this mine tailing is wasted, and does not realize the maximization of the utilization of resources.Reclaim the phosphor resource in the high magnesium phosphorus mine tailing, significant to the comprehensive utilization ratio that improves resource.
The application part that in the Chinese patent database, relates to the phosphorite tailings utilization has " the phosphorous mine tailing after utilizing flotation of phosphate rock is produced the method for phosphoric acid and byproduct building brick " for example No. 200610018780.8; Number 200810058958.0 " utilizing phosphate rock floating by-product mine tailing directly to prepare the method for phosphor magnesium fertilizer "; Number 200810124040.1 " a kind of integrated conduct method of phosphorite tailings sand "; Number 200910218353.8 " a kind of method of utilizing phosphate rock floating mine tailing blast furnace process to prepare calcium magnesium phosphate " or the like.Though these methods differ from one another, however these methods all do not have a high-recovery from the phosphorus mine tailing, reclaim phosphor resource with phosphorus concentrate form.
Summary of the invention
The objective of the invention is to overcome above-mentioned shortcoming and a kind of method that from industrial waste object height magnesium phosphorus mine tailing, reclaims phosphorus is provided, this technology has the advantages that technological process is short, reaction is easy to operate, phosphorous recovery is high.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is: a kind of method that from high magnesium phosphorus mine tailing, reclaims phosphorus may further comprise the steps composition:
(1) with high magnesium phosphorus mine tailing 900～1200 ℃ of down calcinings, burn till forge white;
(2) the said Bai Yushui that forges is mixed by mass ratio 1:4～40, stirred 10～100 minutes down for 20～90 ℃, obtain digestive juice in temperature;
(3) supplementing water makes the digestive juice solid content at mass fraction 2%～15% in said digestive juice; In digestive juice, feed the gas contain carbon dioxide again and under 20～35 ℃, carry out carburizing reagent and obtain carbodiimide solution, reduce in the pH of carbodiimide solution value and stopped in 6.5～8.0 o'clock reacting;
(4) stop reaction after, form suspension and bottom precipitation thing two parts in the carbodiimide solution, after sedimentation separation or spinning liquid separation, obtain this bottom precipitation thing, this sediment is moisture phosphorus ore, this moisture phosphorus ore obtains the ground phosphate rock product after drying.
The above-mentioned method that from high magnesium phosphorus mine tailing, reclaims phosphorus, wherein said high magnesium phosphorus mine tailing is that phosphorus ore obtains the mineral that contain low-grade phosphorus pentoxide that discharge behind the phosphorus concentrate of high-grade phosphorus pentoxide in ore dressing process, contains P
2O
5Be 2%～10%, MgO is 15%～21%, and CaO is 28%～42%.
The above-mentioned method that from high magnesium phosphorus mine tailing, reclaims phosphorus, the wherein said gas that contains carbon dioxide is the carbon dioxide of volume fraction 20%～100%, the carbon dioxide that produces in the time of can being high magnesium phosphorus mine tailing calcining.
The above-mentioned method that from high magnesium phosphorus mine tailing, reclaims phosphorus, wherein said ground phosphate rock product is in butt P
2O
5Content is 25%～35%.
Above-mentioned a kind of method that from high magnesium phosphorus mine tailing, reclaims phosphorus, the phosphorus total amount is with respect to phosphorus total amount in the high magnesium phosphorus mine tailing in the ground phosphate rock product, and the rate of recovery of phosphorus reaches 50%～90%.
The present invention has following characteristics:
1, the present invention is turned waste into wealth, and has recycled the phosphor resource in the mine tailing, has realized the utilization maximization of phosphor resource, is applicable to rock phosphate in powder exploitation and ore dressing enterprise.
2, compared with prior art, the present invention adopts chemistry and physical method from high magnesium phosphorus mine tailing, to reclaim phosphor resource with the form of high-grade phosphorus ore, and the phosphorus mineral product that obtains can be used to produce phosphoric acid and phosphate fertilizer, and is of many uses.
3, the present invention reclaims phosphor resource from high magnesium phosphorus mine tailing; The rate of recovery is higher; The phosphorus mineral product grade that reclaims is higher; Carbodiimide solution behind the Separation and Recovery phosphorus ore contains a large amount of calcium magnesium resources and can be used to prepare calcium, magnesium Related product and be used for flue gas desulfurization etc., and technology of the present invention can be applied a large amount of processing of high magnesium phosphorus mine tailing.
4, the present invention technology does not have the three wastes basically and produces, and the utilization of realization resource maximizes, and has good economic benefit and important environment protection significance.
The specific embodiment
Practical implementation process of the present invention is following:
A kind of method that from high magnesium phosphorus mine tailing, reclaims phosphorus, it may further comprise the steps:
1) calcining: with chemical composition is P
2O
52%～10%, the high magnesium phosphorus mine tailing of MgO15%～21%, CaO28%～42% under 900～1200 ℃, be sintered into forge white;
2) digestion: the said Bai Yushui that forges is mixed by weight 1:4～40, stirred 10～100 minutes down for 20～90 ℃, obtain digestive juice in temperature;
3) carbonization: supplementing water makes the digestive juice solid content at mass fraction 2%～15% in said digestive juice; In digestive juice, feed volume fraction again and be 20%～100% carbon dioxide; Under 20～35 ℃, carry out carburizing reagent and obtain carbodiimide solution; Reduce in the pH of carbodiimide solution value and to stop reaction at 6.5～8.0 o'clock, the carbon dioxide that the gas of feeding produces in the time of can using the calcining of high magnesium phosphorus mine tailing;
4) separate: after stopping reaction; Form suspension and bottom precipitation thing two parts in the carbodiimide solution, after sedimentation separation or spinning liquid separation, obtain this bottom precipitation thing, this sediment is moisture phosphorus ore; This moisture phosphorus ore obtains the ground phosphate rock product after drying, the ground phosphate rock product that obtains is in butt P
2O
5Content is 25%～35%, and the phosphorus total amount is with respect to phosphorus total amount in the high magnesium phosphorus mine tailing in the ground phosphate rock product, and the rate of recovery of phosphorus reaches 50%～90%.
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 following embodiment.
Embodiment 1
High magnesium phosphorus mine tailing chemical composition: P
2O
57.03%, MgO16.87%, CaO37.47%
Take by weighing tail magnesium phosphorus mine tailing 100g 980 ℃ of down calcinings, obtain forging white 61.4g, forge and whitely stirred 40 minutes down at 80 ℃, obtain digestive juice with 700g water.In digestive juice, replenish 800g water, in digestive juice, feed volume fraction again and be 35% carbon dioxide, under 20 ℃, carry out carburizing reagent and obtain carbodiimide solution, reduce in the pH of carbodiimide solution value and stopped in 6.7 o'clock reacting.After stopping reaction, form suspension and bottom sand shape sediment two parts in the carbodiimide solution, after spinning liquid separates, obtain this bottom sand shape sediment, obtain ground phosphate rock product 24.1g, P behind the oven dry moisture
2O
5Content is 26.2%, and the phosphorus total amount is with respect to phosphorus total amount in the high magnesium phosphorus mine tailing in the ground phosphate rock product, and the rate of recovery of phosphorus reaches 90%.
Embodiment 2
High magnesium phosphorus mine tailing chemical composition: P
2O
55.99%, MgO18.26%, CaO36.81%
Take by weighing tail magnesium phosphorus mine tailing 100g 950 ℃ of down calcinings, obtain forging white 59.8g, forge and whitely stirred 30 minutes down at 80 ℃, obtain digestive juice with 500g water.In digestive juice, replenish 600g water, in digestive juice, feed volume fraction again and be 30% carbon dioxide, under 25 ℃, carry out carburizing reagent and obtain carbodiimide solution, reduce in the pH of carbodiimide solution value and stopped in 6.9 o'clock reacting.After stopping reaction, form suspension and bottom sand shape sediment two parts in the carbodiimide solution, after spinning liquid separates, obtain this bottom sand shape sediment, obtain ground phosphate rock product 13.8g, P behind the oven dry moisture
2O
5Content is 32.5%, and the phosphorus total amount is with respect to phosphorus total amount in the high magnesium phosphorus mine tailing in the ground phosphate rock product, and the rate of recovery of phosphorus reaches 75%.
Embodiment 3
High magnesium phosphorus mine tailing chemical composition: P
2O
56.36%, MgO18.58%, CaO37.02%
Take by weighing tail magnesium phosphorus mine tailing 100g 960 ℃ of down calcinings, obtain forging white 60.5g, forge and whitely stirred 30 minutes down at 85 ℃, obtain digestive juice with 430g water.In digestive juice, replenish 900g water, in digestive juice, feed volume fraction again and be 27% carbon dioxide, under 30 ℃, carry out carburizing reagent and obtain carbodiimide solution, reduce in the pH of carbodiimide solution value and stopped in 6.8 o'clock reacting.After stopping reaction, form suspension and bottom sand shape sediment two parts in the carbodiimide solution, after spinning liquid separates, obtain this bottom sand shape sediment, obtain ground phosphate rock product 12.8g, P behind the oven dry moisture
2O
5Content is 34.7%, and the phosphorus total amount is with respect to phosphorus total amount in the high magnesium phosphorus mine tailing in the ground phosphate rock product, and the rate of recovery of phosphorus reaches 65%.
Embodiment 4
High magnesium phosphorus mine tailing chemical composition: P
2O
59.83%, MgO15.04%, CaO41.77%
Take by weighing tail magnesium phosphorus mine tailing 100g 1200 ℃ of down calcinings, obtain forging white 65.3g, forge and whitely stirred 100 minutes down at 90 ℃, obtain digestive juice with 262g water.In digestive juice, replenish 110g water, in digestive juice, feed volume fraction again and be 20% carbon dioxide, under 35 ℃, carry out carburizing reagent and obtain carbodiimide solution, reduce in the pH of carbodiimide solution value and stopped in about 8.0 o'clock reacting.After stopping reaction, form suspension and bottom sand shape sediment two parts in the carbodiimide solution, after spinning liquid separates, obtain this bottom sand shape sediment, obtain ground phosphate rock product 19.4g, P behind the oven dry moisture
2O
5Content is 25.4%, and the phosphorus total amount is with respect to phosphorus total amount in the high magnesium phosphorus mine tailing in the ground phosphate rock product, and the rate of recovery of phosphorus reaches 50%.
Embodiment 5
High magnesium phosphorus mine tailing chemical composition: P
2O
52.16%, MgO20.93%, CaO28.17%
Take by weighing tail magnesium phosphorus mine tailing 100g 900 ℃ of down calcinings, obtain forging white 56.4g, forge and whitely stirred 10 minutes down at 20 ℃, obtain digestive juice with 2256g water.In digestive juice, replenish 508g water, in digestive juice, feed volume fraction again and be 99% carbon dioxide, under 22 ℃, carry out carburizing reagent and obtain carbodiimide solution, reduce in the pH of carbodiimide solution value and stopped in about 6.5 o'clock reacting.After stopping reaction, form suspension and bottom sand shape sediment two parts in the carbodiimide solution, after spinning liquid separates, obtain this bottom sand shape sediment, obtain ground phosphate rock product 5.3g, P behind the oven dry moisture
2O
5Content is 28.7%, and the phosphorus total amount is with respect to phosphorus total amount in the high magnesium phosphorus mine tailing in the ground phosphate rock product, and the rate of recovery of phosphorus reaches 70%.
Claims (5)
1. method that from high magnesium phosphorus mine tailing, reclaims phosphorus is characterized in that it is made up of following steps:
(1) with high magnesium phosphorus mine tailing 900～1200 ℃ of down calcinings, burn till forge white;
(2) the said Bai Yushui that forges is mixed by mass ratio 1:4～40, stirred 10～100 minutes down for 20～90 ℃, obtain digestive juice in temperature;
(3) supplementing water makes the digestive juice solid content at mass fraction 2%～15% in said digestive juice; In digestive juice, feed the gas contain carbon dioxide again and under 20～35 ℃, carry out carburizing reagent and obtain carbodiimide solution, reduce in the pH of carbodiimide solution value and stopped in 6.5～8.0 o'clock reacting;
(4) stop reaction after, form suspension and bottom precipitation thing two parts in the carbodiimide solution, after sedimentation separation or spinning liquid separation, obtain this bottom precipitation thing, this sediment is moisture phosphorus ore, this moisture phosphorus ore obtains the ground phosphate rock product after drying.
2. according to the said method that from high magnesium phosphorus mine tailing, reclaims phosphorus of claim 1, it is characterized in that described high magnesium phosphorus mine tailing is that phosphorus ore obtains the mineral that contain low-grade phosphorus pentoxide that discharge behind the phosphorus concentrate of high-grade phosphorus pentoxide in ore dressing process, contains P
2O
5Be 2%～10%, MgO is 15%～21%, and CaO is 28%～42%.
3. according to the said method that from high magnesium phosphorus mine tailing, reclaims phosphorus of claim 1, it is characterized in that the described gas that contains carbon dioxide is the gas of 20%～100% carbon dioxide volume fraction, the carbon dioxide that produces in the time of can being high magnesium phosphorus mine tailing calcining.
4. according to the said method that from high magnesium phosphorus mine tailing, reclaims phosphorus of claim 1, it is characterized in that described ground phosphate rock product is in butt P
2O
5Content is 25%～35%.
5. according to the said method that from high magnesium phosphorus mine tailing, reclaims phosphorus of claim 1, it is characterized in that the phosphorus total amount is with respect to phosphorus total amount in the high magnesium phosphorus mine tailing in the described ground phosphate rock product, the rate of recovery of phosphorus reaches 50%～90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100859105A CN102600965A (en) | 2012-03-28 | 2012-03-28 | Method for recycling phosphorus from phosphate tailings with high magnesium content |
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|---|---|---|---|
| CN2012100859105A CN102600965A (en) | 2012-03-28 | 2012-03-28 | Method for recycling phosphorus from phosphate tailings with high magnesium content |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103569984A (en) * | 2013-11-26 | 2014-02-12 | 武汉工程大学 | Method for comprehensively utilizing reverse-flotation phosphorite tailings |
| CN104387121A (en) * | 2014-11-10 | 2015-03-04 | 瓮福（集团）有限责任公司 | Method for preparing phosphorus-magnesium fertilizer |
| CN109351481A (en) * | 2018-11-29 | 2019-02-19 | 长沙矿冶研究院有限责任公司 | A kind of phosphorus ore calcining-digestion-reverse flotation separating technology |
| CN110479481A (en) * | 2019-08-16 | 2019-11-22 | 武汉工程大学 | A kind of floatingization coupling low emission beneficiation method |
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| US4265770A (en) * | 1979-11-09 | 1981-05-05 | Amstar Corporation | Separation of suspended solids from phosphate tailings |
| CN101318674A (en) * | 2008-05-29 | 2008-12-10 | 赵景台 | Synthetic processing method for tail ore of phosphorus ore |
| CN101759165A (en) * | 2009-11-17 | 2010-06-30 | 瓮福（集团）有限责任公司 | Method for recovering P2O5 in phosphorus ore dressing mill tailings |
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2012
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| US4265770A (en) * | 1979-11-09 | 1981-05-05 | Amstar Corporation | Separation of suspended solids from phosphate tailings |
| CN101318674A (en) * | 2008-05-29 | 2008-12-10 | 赵景台 | Synthetic processing method for tail ore of phosphorus ore |
| CN101759165A (en) * | 2009-11-17 | 2010-06-30 | 瓮福（集团）有限责任公司 | Method for recovering P2O5 in phosphorus ore dressing mill tailings |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103569984A (en) * | 2013-11-26 | 2014-02-12 | 武汉工程大学 | Method for comprehensively utilizing reverse-flotation phosphorite tailings |
| CN103569984B (en) * | 2013-11-26 | 2015-08-19 | 武汉工程大学 | A kind of method fully utilizing reverse flotation phosphorite tailings |
| CN104387121A (en) * | 2014-11-10 | 2015-03-04 | 瓮福（集团）有限责任公司 | Method for preparing phosphorus-magnesium fertilizer |
| CN104387121B (en) * | 2014-11-10 | 2017-03-08 | 瓮福（集团）有限责任公司 | A kind of method preparing phosphorus fertiliser containing magnesium |
| CN109351481A (en) * | 2018-11-29 | 2019-02-19 | 长沙矿冶研究院有限责任公司 | A kind of phosphorus ore calcining-digestion-reverse flotation separating technology |
| CN110479481A (en) * | 2019-08-16 | 2019-11-22 | 武汉工程大学 | A kind of floatingization coupling low emission beneficiation method |
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Application publication date: 20120725 |