CN105562213A - Preparation method for phosphorus ore reverse flotation depressing agent sulfuric acid and reverse flotation method - Google Patents

Preparation method for phosphorus ore reverse flotation depressing agent sulfuric acid and reverse flotation method Download PDF

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Publication number
CN105562213A
CN105562213A CN201510977778.2A CN201510977778A CN105562213A CN 105562213 A CN105562213 A CN 105562213A CN 201510977778 A CN201510977778 A CN 201510977778A CN 105562213 A CN105562213 A CN 105562213A
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China
Prior art keywords
sulfuric acid
reverse flotation
phosphorus ore
phosphate reverse
compound method
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CN201510977778.2A
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Chinese (zh)
Inventor
曹效权
宋文义
李丰
刘云涛
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Bluestar Lehigh Engineering Institute
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Bluestar Lehigh Engineering Institute
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Priority to CN201510977778.2A priority Critical patent/CN105562213A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/002Inorganic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/06Depressants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00Specified materials treated by the flotation agents; specified applications
    • B03D2203/02Ores
    • B03D2203/04Non-sulfide ores
    • B03D2203/06Phosphate ores

Abstract

A preparation method for phosphorus ore reverse flotation depressing agent sulfuric acid includes the following steps that phosphorus ore is obtained and crushed to the proper particle size; water is added into a sulfuric acid dispensing stirring tank, then the crushed phosphorus ore is added into the sulfuric acid dispensing stirring tank for stirring and slurry mixing, and the slurry mixing concentration is 2%-80%; concentrated sulfuric acid with the mass concentration being 85%-98% is added and evenly stirred; and an appropriate amount of water is added, the volume is set according to the weight of the added concentrated sulfuric acid, and a phosphorus ore reverse flotation depressing agent sulfuric acid solution is obtained. The invention further discloses a method for carrying out phosphorus ore reverse flotation through the depressing agent sulfuric acid. When the sulfuric acid prepared through the method is applied, the number of times of reverse flotation roughing operation can be reduced by 1-2, multiple chemical adding points are provided, the flotation time is shortened by about 30%, the quantity of the sulfuric acid is reduced by about 50%, and a reverse flotation collecting agent is saved by about 20%; the flotation process is stable, product quality is good, and good economic and social benefits are achieved. Moreover, local materials can be used, so that cost is lowered.

Description

A kind of compound method of phosphate reverse flotation inhibitor sulfuric acid and reverse flotation method
Technical field
The present invention relates to a kind of compound method of inhibitor, the compound method of inhibitor sulfuric acid particularly used in a kind of phosphate reverse flotation process; The invention still further relates to the method that the inhibitor sulfuric acid utilizing preceding method to prepare carries out phosphate reverse flotation.
Background technology
Phosphorus ore, mainly for the production of various phosphate fertilizer, is again important chemical industry raw mineral materials simultaneously.The feature of China's phosphate rock resource is that rich ore is few, and lean ore is many, and in lean ore, how genus difficulty selects phosphorus ore again.Through exploitation for many years, China's abundant ore source is exhausted, and mid low grade phosphate rock stone becomes topmost exploitation object.The enrichment means of mid low grade phosphate rock routine are flotation, and flotation is divided into again direct flotation, reverse flotation and technique that both are combined into.Phosphate reverse flotation technique because of production technology simple, cost is lower, is most widely used at present.
Phosphate reverse flotation technique, collecting agent is mainly aliphatic acid, and conventional inhibitor is inorganic acid, be mainly phosphoric acid, sulfuric acid and both mixing nitration mixture.Phosphoric acid cost is high, and limits by the place of production, and sulphuric acid cost is low, and source is relatively wide, and therefore, phosphorus ore manufacturing enterprise often adopts nitration mixture or sulfuric acid as the inhibitor of phosphate reverse flotation.The dissimilar phosphorus ore nature difference in different regions is larger, therefore part phosphorus ore adopts nitration mixture to be that reverse flotation inhibitor production target is better, and adopt sulfuric acid to be that the technological process of reverse flotation inhibitor is complicated, operation number and chemical feeding points many, sulfuric acid dosage is larger, production cost is higher, and operation controls difficult, and equipment pipe fouling is serious.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, thering is provided in a kind of phosphate reverse flotation process take sulfuric acid as the compound method of inhibitor, successfully solving part phosphorus ore directly adopts sulfuric acid to be inhibitor Problems existing, reach and adopt nitration mixture to be the test index of inhibitor, reagent cost is the reagent cost of inhibitor lower than employing nitration mixture, can be enterprise and brings considerable economic benefit.
Another technical problem to be solved by this invention there is provided the method that the inhibitor sulfuric acid utilizing preceding method to obtain carries out phosphate reverse flotation.
Technical problem to be solved by this invention is realized by following technical scheme.The present invention is a kind of compound method of phosphate reverse flotation inhibitor sulfuric acid, and be characterized in, its step is as follows:
(1) get phosphorus ore and be crushed to suitable particle size;
(2) in sulfuric acid makes up a prescription tank diameter, add water, then carry out stirring size mixing to adding the phosphorus ore after fragmentation during sulfuric acid makes up a prescription tank diameter, concentration of sizing mixing is 2 ~ 80%;
(3) add the concentrated sulfuric acid that mass concentration is 85 ~ 98%, stir;
(4) appropriate water is added, by the concentrated sulfuric acid weight constant volume added, obtained phosphate reverse flotation inhibitor sulfuric acid solution.
The compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid of the present invention, its further preferred technical scheme is: the mixing time described in step (3) is 5 ~ 40 minutes, and preferably mixing time is 25 ~ 40 minutes further.
The compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid of the present invention, its further preferred technical scheme is: the phosphorus ore described in step (1) is broken preferably to-100 orders, further preferably to-150 orders.
The compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid of the present invention, its further preferred technical scheme is: the stirring intensity described in step (3) does not precipitate with ore pulp in tank diameter and is as the criterion.
The compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid of the present invention, its further preferred technical scheme is: removed by partial solid phase thing contained in the phosphate reverse flotation inhibitor sulfuric acid solution prepared.
The compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid of the present invention, its further preferred technical scheme is: the weight proportion of phosphorus ore and the concentrated sulfuric acid is preferably 1:1 ~ 3, more preferably 1:2.
The compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid of the present invention, its further preferred technical scheme be: the temperature to the water added during sulfuric acid makes up a prescription tank diameter described in step (2) is preferably 10 ~ 30 DEG C.Concentration of sizing mixing described in step (2) is preferably 5 ~ 25%, and more preferably 10 ~ 20%.
Technical problem to be solved by this invention can also be realized further by following technical scheme.The invention also discloses a kind of phosphate reverse flotation method, be characterized in, the sulfuric acid solution that the method uses above method described in the main case of any one technology obtained is inhibitor.
In the inventive method, containing partial solid phase thing in the sulfuric acid solution prepared, preformed precipitate pond or the removing of other method can be added, also can not remove, add in phosphate reverse flotation technological process as inhibitor together with sulfuric acid solution, affect less on phosphate rock floating process and end product quality.
Compared with the sulfuric acid that the sulfuric acid prepared by this compound method and conventional method are prepared is applied in phosphate reverse flotation, reverse flotation can be reduced and roughly select operations number 1-2 time, chemical feeding points is multiple, shorten flotation time about 30%, sulfuric acid dosage saves about 50%, and collecting agent in reverse floatation saves about 20%, and floatation process is stablized, product quality is better, has preferably through agent benefit and social benefit.And the present invention can realize gathering materials on the spot, phosphorus ore used or high-grade phosphorus ore are that phosphorus ore manufacturing enterprise has phosphorus ore by oneself, without the need to outsourcing.The concentrated sulfuric acid is that phosphorus ore manufacturing enterprise buys by oneself or the self-produced concentrated sulfuric acid.
Detailed description of the invention
Further technical scheme of the present invention is described below, makes those skilled in the art of the present technique understand the present invention further.
Embodiment 1, a kind of compound method of phosphate reverse flotation inhibitor sulfuric acid, its step is as follows:
(1) get phosphorus ore and be crushed to suitable particle size;
(2) in sulfuric acid makes up a prescription tank diameter, add water, then carry out stirring size mixing to adding the phosphorus ore after fragmentation during sulfuric acid makes up a prescription tank diameter, concentration of sizing mixing is 80%;
(3) add the concentrated sulfuric acid that mass concentration is 85%, stir;
(4) appropriate water is added, by the concentrated sulfuric acid weight constant volume added, obtained phosphate reverse flotation inhibitor sulfuric acid solution.
Embodiment 2, a kind of compound method of phosphate reverse flotation inhibitor sulfuric acid, its step is as follows:
(1) get phosphorus ore and be crushed to suitable particle size;
(2) in sulfuric acid makes up a prescription tank diameter, add water, then carry out stirring size mixing to adding the phosphorus ore after fragmentation during sulfuric acid makes up a prescription tank diameter, concentration of sizing mixing is 2%;
(3) add the concentrated sulfuric acid that mass concentration is 98%, stir;
(4) appropriate water is added, by the concentrated sulfuric acid weight constant volume added, obtained phosphate reverse flotation inhibitor sulfuric acid solution.
Embodiment 3, a kind of compound method of phosphate reverse flotation inhibitor sulfuric acid, its step is as follows:
(1) get phosphorus ore and be crushed to suitable particle size;
(2) to the water adding 5 DEG C during sulfuric acid makes up a prescription tank diameter, then carry out stirring size mixing to adding the phosphorus ore after fragmentation during sulfuric acid makes up a prescription tank diameter, concentration of sizing mixing is 10%;
(3) add the concentrated sulfuric acid that mass concentration is 90%, stir;
(4) appropriate water is added, by the concentrated sulfuric acid weight constant volume added, obtained phosphate reverse flotation inhibitor sulfuric acid solution.
Embodiment 4, a kind of compound method of phosphate reverse flotation inhibitor sulfuric acid, its step is as follows:
(1) get phosphorus ore and be crushed to suitable particle size;
(2) to the water adding 25 DEG C during sulfuric acid makes up a prescription tank diameter, then carry out stirring size mixing to adding the phosphorus ore after fragmentation during sulfuric acid makes up a prescription tank diameter, concentration of sizing mixing is 20%;
(3) add the concentrated sulfuric acid that mass concentration is 95%, stir;
(4) appropriate water is added, by the concentrated sulfuric acid weight constant volume added, obtained phosphate reverse flotation inhibitor sulfuric acid solution.
Embodiment 5, a kind of compound method of phosphate reverse flotation inhibitor sulfuric acid, its step is as follows:
(1) get phosphorus ore and be crushed to suitable particle size;
(2) to the water adding 20 DEG C during sulfuric acid makes up a prescription tank diameter, then carry out stirring size mixing to adding the phosphorus ore after fragmentation during sulfuric acid makes up a prescription tank diameter, concentration of sizing mixing is 40%;
(3) add the concentrated sulfuric acid that mass concentration is 93%, stir;
(4) appropriate water is added, by the concentrated sulfuric acid weight constant volume added, obtained phosphate reverse flotation inhibitor sulfuric acid solution.
Embodiment 6, in the compound method of the phosphate reverse flotation inhibitor sulfuric acid of embodiment 1-5 described in any one: the mixing time described in step (3) is 5 ~ 40 minutes.
Embodiment 7, in the compound method of the phosphate reverse flotation inhibitor sulfuric acid of embodiment 1-5 described in any one: the mixing time described in step (3) is 25 ~ 40 minutes.
Embodiment 8, in the compound method of the phosphate reverse flotation inhibitor sulfuric acid of embodiment 1-6 described in any one: the phosphorus ore described in step (1) is crushed to-150 orders.
Embodiment 9, in the compound method of the phosphate reverse flotation inhibitor sulfuric acid of embodiment 1-7 described in any one: the stirring intensity described in step (3) does not precipitate with ore pulp in tank diameter and is as the criterion.
Embodiment 10, in the compound method of the phosphate reverse flotation inhibitor sulfuric acid of embodiment 1-8 described in any one: removed by partial solid phase thing contained in the phosphate reverse flotation inhibitor sulfuric acid solution prepared.
Embodiment 11, in the compound method of the phosphate reverse flotation inhibitor sulfuric acid of embodiment 1-9 described in any one: the weight proportion of phosphorus ore and the concentrated sulfuric acid is 1:1.
Embodiment 12, in the compound method of the phosphate reverse flotation inhibitor sulfuric acid of embodiment 1-9 described in any one: the weight proportion of phosphorus ore and the concentrated sulfuric acid is 1:3.
Embodiment 13, in the compound method of the phosphate reverse flotation inhibitor sulfuric acid of embodiment 1-9 described in any one: the weight proportion of phosphorus ore and the concentrated sulfuric acid is 1:2.
Embodiment 14, a kind of phosphate reverse flotation method, the sulfuric acid solution that the method uses the method for embodiment 1-12 described in any one obtained is inhibitor.
Embodiment 15, a kind of compound method experiment one of phosphate reverse flotation inhibitor sulfuric acid, its step is as follows: rock phosphate in powder is crushed to-150 orders; Concentrated sulfuric acid concentration is 92%; Phosphorus ore grade is P 2o 5content 32%, the concentrated sulfuric acid and phosphorus ore weight proportion are 2:1, and first in sulfuric acid makes up a prescription tank diameter, add 45 DEG C of hot water, then add phosphorus ore, add the concentrated sulfuric acid after stirring, mixing time of making up a prescription is 30 minutes, adds water, by sulfuric acid amount constant volume 10% weight concentration added.
The sulfuric acid solution prepared is added in phosphate reverse flotation technological process, as raw ore P 2o 5grade is 22.15%, and content of MgO is 7.24%, when ore grinding to-200 order content account for 60.36%, adopts a thick technological process again and again, can obtain concentrate yield 61.46%, P 2o 5grade is 33.00%, and content of MgO is 1.21%, P 2o 5the rate of recovery is the result of the test of 91.75%.
Embodiment 16, a kind of compound method experiment two of phosphate reverse flotation inhibitor sulfuric acid, its step is as follows: rock phosphate in powder is crushed to-180 orders.Concentrated sulfuric acid concentration is 95%.Phosphorus ore grade is P 2o 5content 34%, the concentrated sulfuric acid and phosphorus ore weight proportion are 2:1, and first in sulfuric acid makes up a prescription tank diameter, add 45 DEG C of hot water, then add phosphorus ore, add the concentrated sulfuric acid after stirring, mixing time of making up a prescription is 25 minutes, adds water, by sulfuric acid amount constant volume 10% weight concentration added.
The sulfuric acid solution prepared is added in phosphate reverse flotation technological process, as raw ore P 2o 5grade 20.96%, content of MgO 8.44%, mog for-200 order content account for 67.30% time, adopt a thick technological process again and again, comprehensive concentrate yield 55.59%, P can be obtained 2o 5grade 34.41%, content of MgO 1.12%, P 2o 5the result of the test of the rate of recovery 90.00%.
Embodiment 17, a kind of compound method experiment three of phosphate reverse flotation inhibitor sulfuric acid, its step is as follows: rock phosphate in powder is crushed to-200 orders.Concentrated sulfuric acid concentration is 97%.Phosphorus ore grade is P 2o 5content 28%, the concentrated sulfuric acid and phosphorus ore weight proportion are 1.5:1, first in sulfuric acid makes up a prescription tank diameter, add 55 DEG C of hot water, add phosphorus ore again, add the concentrated sulfuric acid after stirring, mixing time of making up a prescription is 20 minutes, add water, by sulfuric acid amount constant volume 10% weight concentration added.
The sulfuric acid solution prepared is added in phosphate reverse flotation technological process, as raw ore P 2o 5grade is 21.12%, and content of MgO is 8.06%, when ore grinding to-200 order content account for 65.36%, adopts a thick technological process again and again, can obtain concentrate yield 56.02%, P 2o 5grade is 33.36%, and content of MgO is 1.32%, P 2o 5the rate of recovery is the result of the test of 89.45%.
Embodiment 18, a kind of compound method experiment four of phosphate reverse flotation inhibitor sulfuric acid, its step is as follows: rock phosphate in powder is crushed to-200 orders.Concentrated sulfuric acid concentration is 98%.Phosphorus ore grade is P 2o 5content 25%, the concentrated sulfuric acid and phosphorus ore weight proportion are 1.3:1, first in sulfuric acid makes up a prescription tank diameter, add 65 DEG C of hot water, add phosphorus ore again, add the concentrated sulfuric acid after stirring, mixing time of making up a prescription is 25 minutes, add water, by sulfuric acid amount constant volume 10% weight concentration added.The sulfuric acid solution prepared is added in phosphate reverse flotation technological process, as raw ore P 2o 5grade is 22.15%, and content of MgO is 7.24%, when ore grinding to-200 order content account for 60.36%, adopts a thick technological process again and again, can obtain concentrate yield 61.46%, P 2o 5grade is 33.00%, and content of MgO is 1.21%, P 2o 5the rate of recovery is the result of the test of 89.45%.
Embodiment 19, a kind of compound method experiment five of phosphate reverse flotation inhibitor sulfuric acid, its step is as follows: rock phosphate in powder is crushed to-200 orders.Concentrated sulfuric acid concentration is 98%.Phosphorus ore grade is P 2o 5content 35%, the concentrated sulfuric acid and phosphorus ore weight proportion are 3:1, and first in sulfuric acid makes up a prescription tank diameter, add 53 DEG C of hot water, then add phosphorus ore, add the concentrated sulfuric acid after stirring, mixing time of making up a prescription is 15 minutes, adds water, by sulfuric acid amount constant volume 10% weight concentration added.The sulfuric acid solution prepared is added in phosphate reverse flotation technological process, as raw ore P 2o 5grade is 23.87%, and content of MgO is 6.04%, when ore grinding to-200 order content account for 64.86%, adopts a thick technological process again and again, can obtain concentrate yield 61.79%, P 2o 5grade is 34.33%, and content of MgO is 1.12%, P 2o 5the rate of recovery is the result of the test of 88.88%.

Claims (10)

1. a compound method for phosphate reverse flotation inhibitor sulfuric acid, is characterized in that, its step is as follows:
(1) get phosphorus ore and be crushed to suitable particle size;
(2) in sulfuric acid makes up a prescription tank diameter, add water, then carry out stirring size mixing to adding the phosphorus ore after fragmentation during sulfuric acid makes up a prescription tank diameter, concentration of sizing mixing is 2 ~ 80%;
(3) add the concentrated sulfuric acid that mass concentration is 85 ~ 98%, stir;
(4) appropriate water is added, by the concentrated sulfuric acid weight constant volume added, obtained phosphate reverse flotation inhibitor sulfuric acid solution.
2. the compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid according to claim 1, is characterized in that: the mixing time described in step (3) is 5 ~ 40 minutes.
3. the compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid according to claim 1, is characterized in that: the phosphorus ore described in step (1) is crushed to-150 orders.
4. the compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid according to claim 1, is characterized in that: the stirring intensity described in step (3) does not precipitate with ore pulp in tank diameter and is as the criterion.
5. the compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid according to claim 1, is characterized in that: removed by partial solid phase thing contained in the phosphate reverse flotation inhibitor sulfuric acid solution prepared.
6. the compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid according to claim 1, is characterized in that: the weight proportion of phosphorus ore and the concentrated sulfuric acid is 1:1 ~ 3.
7. the compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid according to claim 6, is characterized in that: the weight proportion of phosphorus ore and the concentrated sulfuric acid is 1:2.
8. the compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid according to claim 1, is characterized in that: the temperature to the water added during sulfuric acid makes up a prescription tank diameter described in step (2) is 10 ~ 30 DEG C.
9. the compound method of a kind of phosphate reverse flotation inhibitor sulfuric acid according to claim 1, is characterized in that: the concentration of sizing mixing described in step (2) is 5 ~ 25%.
10. a phosphate reverse flotation method, is characterized in that, the sulfuric acid solution that the method uses the method for claim 1-9 described in any one obtained is inhibitor.
CN201510977778.2A 2015-12-23 2015-12-23 Preparation method for phosphorus ore reverse flotation depressing agent sulfuric acid and reverse flotation method Pending CN105562213A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4364824A (en) * 1981-06-02 1982-12-21 International Minerals & Chemical Corp. Flotation of phosphate ores containing dolomite
CN1443607A (en) * 2003-04-22 2003-09-24 武汉化工学院 Phosphate mineral inhibitor, its application in reverse floatation of phosphorus ore and preparation method
CN102744151A (en) * 2012-07-06 2012-10-24 中蓝连海设计研究院 Branch flotation technology for silicon calcium collophanite
CN103212484A (en) * 2013-04-18 2013-07-24 武汉工程大学 Phosphorite reverse flotation process
CN103551257A (en) * 2013-11-25 2014-02-05 四川省地质矿产勘查开发局成都综合岩矿测试中心 Phosphorite reverse flotation process
CN103909018A (en) * 2014-04-18 2014-07-09 武汉工程大学 Collophanite reverse flotation depressing agent and application thereof
CN104624379A (en) * 2014-12-29 2015-05-20 中蓝连海设计研究院 Obverse and reverse flotation method of low-grade silica-calcia bearing collophane

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4364824A (en) * 1981-06-02 1982-12-21 International Minerals & Chemical Corp. Flotation of phosphate ores containing dolomite
CN1443607A (en) * 2003-04-22 2003-09-24 武汉化工学院 Phosphate mineral inhibitor, its application in reverse floatation of phosphorus ore and preparation method
CN102744151A (en) * 2012-07-06 2012-10-24 中蓝连海设计研究院 Branch flotation technology for silicon calcium collophanite
CN103212484A (en) * 2013-04-18 2013-07-24 武汉工程大学 Phosphorite reverse flotation process
CN103551257A (en) * 2013-11-25 2014-02-05 四川省地质矿产勘查开发局成都综合岩矿测试中心 Phosphorite reverse flotation process
CN103909018A (en) * 2014-04-18 2014-07-09 武汉工程大学 Collophanite reverse flotation depressing agent and application thereof
CN104624379A (en) * 2014-12-29 2015-05-20 中蓝连海设计研究院 Obverse and reverse flotation method of low-grade silica-calcia bearing collophane

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