CN109701749A - A kind of method of nitric acid pretreatment direct flotation phosphorus concentrate - Google Patents
A kind of method of nitric acid pretreatment direct flotation phosphorus concentrate Download PDFInfo
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- CN109701749A CN109701749A CN201910058081.3A CN201910058081A CN109701749A CN 109701749 A CN109701749 A CN 109701749A CN 201910058081 A CN201910058081 A CN 201910058081A CN 109701749 A CN109701749 A CN 109701749A
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Abstract
The invention discloses a kind of methods of nitric acid pretreatment direct flotation phosphorus concentrate, belong to phosphorous chemical industry and flotation of phosphate rock field.This method carries out phosphorus ore direct flotation to mid low grade phosphate rock first, then using the calcium and magnesium in low concentration nitric acid pretreatment direct flotation phosphorus concentrate, then carries out two sections of neutralizations, phosphorus concentrate is finally obtained, through the pretreated phosphorus concentrate P of the method for the present invention2O5Content reaches 32 ± 1%, MgO lower than 0.50%, realizes the enrichment of phosphorus.And ammonium nitrate magnesium and calcium ammonium nitrate nitro-compound fertilizer are obtained, realizes the resource utilization of calcium, magnesium.The method of the present invention has simple process, and strong applicability is of great significance in terms of comprehensive utilization of resources.
Description
Technical field
The invention belongs to phosphorous chemical industry and flotation of phosphate rock production field, it is related to a kind of nitric acid pretreatment direct flotation phosphorus concentrate
Method.
Background technique
Yunnan collophane key industry type have it is calcareous, siliceous, three kinds of mixed type, complete types, reserves are occupied with mixed type
It is more, siliceous take second place, calcareous type it is minimum, siliceous collophane accounts for about 1/3.Mixed type phosphorus ore reserves are big, and grade is low, at present using n-
Anti- technique enrichment, beneficiation cost is very high, and economic benefit is not significant, and enterprise is difficult to receive.
Nitrate method phosphate ore processing technology proposed that the 1920s, Germany carried out first in 1908 by Russia scholar earliest
Industrialized production, nineteen twenty-eight Norway Ao Da company successfully develop freezing law technology, and many countries and companies are to the technology later
It is improved.Due to the difference of world's different zones Sulphur ressource, the production capacity of nitrate method phosphate ore processing is concentrated mainly on Europe.I
State starts to the research of nitrate method phosphate ore processing technology in the 1950s, Shanghai Chemical Research Inst is to carbonizatin method, mixed acid process etc.
Extensive research is carried out, and part has carried out pilot scale.Nan Hua institute and Chengdu Univ. of Science & Technology (existing Sichuan University) also relatively early carry out
Correlative study.But the production of domestic industry metaplasia starts from Shanxi chemical fertilizer factory in 1987 (existing Shanxi Tianjimei Chemical Group Co., Ltd) and draws
Into Norway's NORSK HYDRO process flow and the 900000 tons/year of Nitro Phosphate Units that are constructed and put into operation.Current China nitrophosphate fertilizer industry
Increasingly mature, product has stepped the gateway of a country, has gone to the world.But nitrate method technique be using high-grade phosphorus ore, and with
The dilution of phosphate rock resource, it is difficult to meet the requirement of nitrate method technique.Patent 201110201294.0 discloses decomposing phosphorite by using nitric acid
The method of ammonium sulfate round-robin method execution high-water solubility nitrophosphate fertilizer.With decomposing phosphorite by using nitric acid, ammonium sulfate recycles deliming, then uses ammonium hydroxide
Removal of impurities is neutralized, evaporating, concentrating and crystallizing obtains high-water solubility nitrophosphate fertilizer and by-product calcium carbonate product.Patent nitric acid extraction phosphorus
Mine obtains nitrophosphate fertilizer, on the one hand be high-grade phosphorus ore, another aspect impurity etc. fully enters phosphate fertilizer with nitric acid extraction
In, influence water-soluble phosphorus equal size.Patent 201510226378.8 discloses a kind of nitric acid decomposing medium and low grade ammonium phosphate
The technique of calcium and magnesium and ammonium nitrate calcium and magnesium.And mid low grade phosphate rock is directly extracted by nitric acid, then in ammonium hydroxide and prepare fertilizer.
The patent is enriched phosphorus, causes the water-soluble phosphorus of fertilizer of production and nitrogen to be difficult to up to standard.
Summary of the invention
The invention discloses a kind of nitric acid pretreatment direct flotation phosphorus concentrate technology, this method has simple process, applicability
Strong advantage, it can be achieved that calcium, magnesium resource full dose resource utilization.
The present invention solves the above problems used technical solution are as follows:
A kind of method of nitric acid pretreatment direct flotation phosphorus concentrate, which comprises the following steps:
(5) phosphorus ore direct flotation: mid low grade phosphate rock being mixed with regulator and is ground, and grinding fineness is that -0.038mm is low
In 70%, one roughing obtains the concentrate selection that top-ups, and obtained concentrate selection content of top-uping is P2O524~27%, MgO 4~7%,
CaO 39~42%；
(6) pre-process: the concentrate selection low concentration nitric acid that will top-up leaches, and the mass concentration of nitric acid is 1-15%, leaches pH
1.8 are maintained, extraction temperature is 20~50 DEG C, and the time is 180~400min, obtains leachate；
(7) neutralize: the leachate that upper step is obtained filters, and filtrate carries out two sections of neutralizations, the pH of one section of neutralization using ammonium hydroxide
Value is 4.0~4.7；The pH value of two sections of neutralizations is 8.3~9.4；
(4) it dries: filtered sample ore is obtained into phosphorus concentrate after 100~140 DEG C of 1~4h of drying.
" % " of the present invention each means mass percentage.
In (1) step of the invention, using waterglass as inhibitor in the process of lapping, with mid low grade phosphate rock quality
For 100% meter, the dosage of the inhibitor is 1~2%.
The regulator is sodium carbonate or sodium bicarbonate, is in terms of 100% by mid low grade phosphate rock quality, the regulator is used
Amount is 2~5%.
The mass fraction for the ammonium hydroxide that of the invention (3) use is 15~28%, preferably 20~25%；
The phosphorus concentrate composition that the present invention obtains after dust technology pre-processes are as follows: P2O5It is lower than up to 32 ± 1%, MgO
0.50%, it is produced for phosphorous chemical industry.
It according to the solubility product difference of ammonium nitrate magnesium and calcium ammonium nitrate is foundation in the present invention, one section of neutralizations slag is ammonium nitrate
Magnesium, it is nitro-compound fertilizer that two sections, which are calcium ammonium nitrate,.
Silicon mixed type collophane high for high magnesium, traditional handicraft use n- anti-process flow, and process flow is long, at high cost,
The rate of recovery is low.Nitric acid pretreatment technology is to be higher than the characteristic of fluorapatite using dolomite activity in phosphorus ore, by controlling solution
PH value decomposes the dolomite with the mutually embedding cloth of direct flotation phosphorus concentrate, so that magnesium, calcium compound is transferred to liquid phase, phosphorus is made after dense
MgO is reduced to 0.5% hereinafter, P in mine2O5It mentions to 32 ± 1%.And calcium-magnesium-containing filtrate is adjusted pH value, be made into nitric acid ammonia calcium,
Fertilizer, the indexs of correlation such as nitric acid ammonia magnesium are met the requirements.
The present invention leaches direct flotation phosphorus concentrate using low concentration nitric acid, and the addition of one side low concentration nitric acid increases
Reaction liquid-solid ratio improves the diffusion rate of hydrogen, magnesium, calcium ion, accelerates reaction rate；On the other hand it can avoid nitric acid volatilization
And reduce the processing cost and environmental problem of nitrogen oxides tail gas.
On the one hand the present invention realizes the enrichment of phosphorus by calcium, magnesium in nitric acid pretreatment direct flotation phosphorus concentrate etc., and realize
The resource utilization of calcium, magnesium.The concentrate selection low concentration nitric acid that top-ups leaches, and filters filtrate and is neutralized with two sections of ammonium hydroxide, a Duan Zhonghe
Slag is ammonium nitrate magnesium, and two sections are calcium ammonium nitrate, and the concentrate selection that top-ups is in P2O524~27%, MgO 4~7%, CaO 39~42%.
It is P through the pretreated phosphorus concentrate content of the present invention2O532% or so, MgO are lower than 0.50%, produce, realize for phosphorous chemical industry
Phosphorus ore full dose resource utilization.
The present invention has the advantage that and innovation:
(1) grinding fineness is reduced, it is energy saving, ore grinding production capacity is improved, realizes mid low grade phosphate rock full dose resource utilization；
(2) 15% or more phosphorus concentrate yield can be improved in the method for the present invention；
(3) the full dose resource utilization of calcium, magnesium resource is realized；
(4) and unlike patent 201110201294.0 and 201510226378.8, the method for the present invention is by locating in advance
The phosphorus content of reason enrichment phosphorus ore is not direct extraction and leads to subsequent production series technique problem；
(5) processing cost that low concentration nitric acid can avoid volatilization and reduce nitrogen oxides tail gas is added.
A kind of method of nitric acid pretreatment direct flotation phosphorus concentrate disclosed by the invention, have simple process, strong applicability,
It is of great significance in terms of comprehensive utilization of resources.
Specific embodiment
Raw ore derives from Yunnan Linhua Group Corp., Ltd., is mid low grade phosphate rock, raw ore chemical constituent is P2O518~
22%, MgO 3~6%, CaO 30~42%, SiO235~45%.
Embodiment 1
Mid low grade phosphate rock is mixed with regulator and is ground, grinding fineness is -0.038mm67.88%；Using water glass
Glass is as inhibitor, dosage 1.3%；Regulator is sodium carbonate, and dosage 3.6%, the concentrate of one roughing is direct flotation essence
Mine.100g direct flotation phosphorus concentrate is taken, 6% dust technology 11.25g is added, extraction temperature is 30 DEG C, time 230min, is filtered
It obtains filtrate and adds two sections of ammonium hydroxide neutralizations, wherein the pH value of one section of neutralization is 4.2；The pH value of two sections of neutralizations is 8.6, drying difference
For ammonium nitrate magnesium, calcium ammonium nitrate.Obtained phosphorus concentrate Main chemical component is P2O532.78%；MgO 0.39%；P2O5It is comprehensive
The rate of recovery is 80.35%.
Comparative example 1
The best way is direct-reverse flotation at present, and mid low grade phosphate rock is mixed with regulator and is ground, grinding fineness
For -0.038mm67.88%；Using waterglass as inhibitor, dosage 1.3%；Regulator is sodium carbonate, and dosage is
3.6%, the concentrate of one roughing is positive flotation concentrate.100g direct flotation phosphorus concentrate, collecting agent in reverse floatation 1.2g are taken, room temperature floats
Choosing, obtained phosphorus concentrate Main chemical component are P2O528.45%；MgO 0.96%, P2O5Comprehensive recovery is 59.45%.
Comparative example 1 and embodiment 1 compare, phosphorus concentrate P2O5Grade is lower, MgO high, it is difficult to produce high-concentration water-soluble fertilizer
Material.
Embodiment 2
Mid low grade phosphate rock is mixed with regulator and is ground, grinding fineness is that -0.038mm is lower than 70%；Using water
Glass is as inhibitor, dosage 1.4%；Regulator is sodium carbonate, dosage 3.5%；The concentrate of one roughing is direct flotation
Concentrate.100g direct flotation phosphorus concentrate is taken, 9% dust technology 7.48g is added, extraction temperature is 29 DEG C, time 360min, is filtered
It obtains filtrate and adds two sections of ammonium hydroxide neutralizations, wherein the pH value of one section of neutralization is 4.5；The pH value of two sections of neutralizations is 8.3, drying difference
For ammonium nitrate magnesium, calcium ammonium nitrate.Obtained phosphorus concentrate Main chemical component is P2O531.87%；MgO 0.47%；P2O5It is comprehensive
The rate of recovery is 80.76%.
Comparative example 2
The best way is direct-reverse flotation at present, and mid low grade phosphate rock is mixed with regulator and is ground, grinding fineness
For -0.038mm68.99%；Using waterglass as inhibitor, dosage 1.4%；Regulator is sodium carbonate, and dosage is
3.5%, the concentrate of one roughing is positive flotation concentrate.100g direct flotation phosphorus concentrate, collecting agent in reverse floatation 1.4g are taken, room temperature floats
Choosing, obtained phosphorus concentrate Main chemical component are P2O528.74%；MgO 0.95%, P2O5Comprehensive recovery is 60.21%.
Comparative example 2 and embodiment 2 compare, phosphorus concentrate P2O5Grade is lower, MgO high, it is difficult to produce high-concentration water-soluble fertilizer
Material.
Embodiment 3
Mid low grade phosphate rock is mixed with regulator and is ground, grinding fineness is that -0.038mm is lower than 70%；Using water
Glass is as inhibitor, dosage 1.6%；Regulator is sodium bicarbonate, dosage 3.2%；The concentrate of one roughing is to top-up
Concentrate selection.100g direct flotation phosphorus concentrate is taken, 12% dust technology 4.87g is added, extraction temperature is 40 DEG C, time 350min,
Suction filtration obtains filtrate and adds two sections of ammonium hydroxide neutralizations, wherein the pH value of one section of neutralization is 4.6；The pH value of two sections of neutralizations is 9.2, drying
Respectively ammonium nitrate magnesium, calcium ammonium nitrate.Obtained phosphorus concentrate Main chemical component is P2O532.14%；MgO 0.40%；P2O5
Comprehensive recovery is 81.10%.
Comparative example 3
The best way is direct-reverse flotation at present, and mid low grade phosphate rock is mixed with regulator and is ground, grinding fineness
For -0.038mm69.54%；Using waterglass as inhibitor, dosage 1.5%；Regulator is sodium bicarbonate, and dosage is
3.2%；The concentrate of one roughing is positive flotation concentrate.100g direct flotation phosphorus concentrate, collecting agent in reverse floatation 1.3g are taken, room temperature floats
Choosing, obtained phosphorus concentrate Main chemical component are P2O528.50%；MgO 0.89%, P2O5Comprehensive recovery is 59.87%.
Comparative example 3 and embodiment 3 compare, phosphorus concentrate P2O5Grade is lower, MgO high, it is difficult to produce high-concentration water-soluble fertilizer.
Claims (8)
1. a kind of method of nitric acid pretreatment direct flotation phosphorus concentrate, which comprises the following steps:
(1) phosphorus ore direct flotation: mid low grade phosphate rock being mixed with regulator and is ground, and one roughing obtains the concentrate selection that top-ups,
Obtained concentrate selection content of top-uping is P2O524-27%, MgO 4-7%, CaO 39-42%；
(2) pre-process: the concentrate selection low concentration nitric acid that will top-up leaches, and the mass concentration of nitric acid is 1-15%, leaches pH and maintains
1.8, extraction temperature is 20~50 DEG C, and the time is 180~400min, obtains leachate；
(3) neutralize: the leachate that upper step is obtained filters, and filtrate carries out two sections of neutralizations using ammonium hydroxide；
(4) it dries: filtered sample ore is obtained into phosphorus concentrate after 100~140 DEG C of 1~4h of drying.
2. the method for nitric acid pretreatment direct flotation phosphorus concentrate according to claim 1, which is characterized in that in step (3), institute
The grinding fineness for stating grinding is -0.038mm lower than 70%.
3. the method for nitric acid pretreatment direct flotation phosphorus concentrate according to claim 1, which is characterized in that in step (1), institute
It states in process of lapping using waterglass as inhibitor, is the dosage of the inhibitor in terms of 100% by mid low grade phosphate rock quality
It is 1~2%.
4. the method for nitric acid pretreatment direct flotation phosphorus concentrate according to claim 1, which is characterized in that in step (1), institute
State regulator be sodium carbonate or sodium bicarbonate, by mid low grade phosphate rock quality be 100% in terms of, the regulator dosage be 2~
5%.
5. the method for nitric acid pretreatment direct flotation phosphorus concentrate according to claim 1, which is characterized in that in step (3), institute
The mass fraction for stating ammonium hydroxide is 15~28%.
6. the method for nitric acid pretreatment direct flotation phosphorus concentrate according to claim 1 or 5, which is characterized in that the ammonium hydroxide
Mass fraction be 20~25%.
7. the method for nitric acid pretreatment direct flotation phosphorus concentrate according to claim 1, which is characterized in that two sections of neutralizations
In, the pH value of one section of neutralization is 4.0~4.7, and the pH value of two sections of neutralizations is 8.3~9.4.
8. the method for nitric acid pretreatment direct flotation phosphorus concentrate according to claim 1, which is characterized in that step (4) is medium
The phosphorus concentrate composition arrived are as follows: P2O532 ± 1%, MgO are lower than 0.50%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240136A (en) * | 2019-06-21 | 2019-09-17 | 宜都兴发化工有限公司 | Potassium, sodium enter the inhibitor of phosphoric acid in a kind of control phosphorus concentrate |
| CN111036413A (en) * | 2019-11-27 | 2020-04-21 | 东北大学 | Application of inhibitor AA/AMPS in positive flotation and magnesium removal of phosphate ore |
| CN111036412A (en) * | 2019-11-27 | 2020-04-21 | 东北大学 | Application of high-efficiency inhibitor HPMA in positive flotation and magnesium removal of phosphate ore |
| CN112047348A (en) * | 2020-09-17 | 2020-12-08 | 云南磷化集团有限公司 | Method for full resource utilization of high-silicon low-magnesium low-grade phosphate ore |
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| CN104909841A (en) * | 2015-05-06 | 2015-09-16 | 贵州省化工研究院 | Process for preparing calcium magnesium ammonium phosphate and calcium magnesium ammonium nitrate through nitric acid decomposition of low-medium graded phosphate ore |
| CN105256135A (en) * | 2014-06-13 | 2016-01-20 | 北京科技大学 | Method for recovering phosphorus resource in high-phosphorus iron ore through ball-milling acid leaching-biological adsorption |
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| CN107879363A (en) * | 2017-11-06 | 2018-04-06 | 湖北三宁化工股份有限公司 | A kind of method that nitric acid decomposes phosphorus mine tailing extracting sulfuric acid calcium pyroborate by-product magnesium hydroxide and ammonium nitrate magnesium |
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2019
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| US5147528A (en) * | 1990-04-12 | 1992-09-15 | Falconbridge Limited | Phosphate beneficiation process |
| CN1730161A (en) * | 2005-07-30 | 2006-02-08 | 中蓝连海设计研究院 | Collophanite direct flotation and reverse flotation technique |
| CN105256135A (en) * | 2014-06-13 | 2016-01-20 | 北京科技大学 | Method for recovering phosphorus resource in high-phosphorus iron ore through ball-milling acid leaching-biological adsorption |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110240136A (en) * | 2019-06-21 | 2019-09-17 | 宜都兴发化工有限公司 | Potassium, sodium enter the inhibitor of phosphoric acid in a kind of control phosphorus concentrate |
| CN111036413A (en) * | 2019-11-27 | 2020-04-21 | 东北大学 | Application of inhibitor AA/AMPS in positive flotation and magnesium removal of phosphate ore |
| CN111036412A (en) * | 2019-11-27 | 2020-04-21 | 东北大学 | Application of high-efficiency inhibitor HPMA in positive flotation and magnesium removal of phosphate ore |
| CN112047348A (en) * | 2020-09-17 | 2020-12-08 | 云南磷化集团有限公司 | Method for full resource utilization of high-silicon low-magnesium low-grade phosphate ore |
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