CN113182077B - Reverse flotation process for synchronously removing magnesium and aluminum in phosphate ore - Google Patents

Reverse flotation process for synchronously removing magnesium and aluminum in phosphate ore Download PDF

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CN113182077B
CN113182077B CN202110377838.2A CN202110377838A CN113182077B CN 113182077 B CN113182077 B CN 113182077B CN 202110377838 A CN202110377838 A CN 202110377838A CN 113182077 B CN113182077 B CN 113182077B
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CN113182077A (en
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刘鑫
郑光明
陈慧
王旭东
李防
孙桦林
刘兵兵
刘海方
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Yidu Xingfa Chemical Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/02—Froth-flotation processes
    • B03D1/021—Froth-flotation processes for treatment of phosphate ores
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/007—Modifying reagents for adjusting pH or conductivity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/02—Collectors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; specified applications
    • B03D2203/02—Ores
    • B03D2203/04—Non-sulfide ores
    • B03D2203/06—Phosphate ores

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Abstract

The invention relates to a reverse flotation process for synchronously removing magnesium and aluminum in phosphorite. The technical scheme is as follows: introducing the phosphorite slurry into a synchronous reverse flotation process; firstly, adding a regulator into phosphorite slurry, then synchronously adding a fatty acid collecting agent and an amine collecting agent into the phosphorite slurry, carrying out pre-flotation operation to obtain a product I and a foam product I in a tank, wherein the foam product I is phosphate tailings I, the product I in the tank is subjected to rough concentration operation and rough concentration to obtain a product II and a foam product II in the tank, the product II in the tank is phosphate concentrate, the foam product II is subjected to first scavenging operation and scavenging operation to obtain a product III and a foam product III in the tank, the product III in the tank returns to the previous step to enter the rough concentration operation together with the product I in the tank, the foam product III returns to the next step to enter the first scavenging operation together with the product II, the foam product IV is phosphate tailings II. The invention has the characteristics of strong ore adaptability, small consumption of flotation reagents and low beneficiation cost.

Description

Reverse flotation process for synchronously removing magnesium and aluminum in phosphate ore
Technical Field
The invention belongs to the technical field of phosphorite separation, and particularly relates to a reverse flotation process for synchronously removing magnesium and aluminum in phosphorite.
Background
The top three of the world ranks of phosphorite resources in China, but the rich ore is less, the lean ore is more, and P is 2 O 5 The rich ore with grade higher than 30 percent only accounts for about 8 percent of the total reserve volume and is largePart of the phosphate ore must be enriched to be utilized by high added value. Flotation is widely adopted in phosphorite separation, and aiming at phosphorite with many kinds of impurities and high impurity content, the impurities can be effectively removed only by adopting positive-negative (reverse-positive) flotation or double-negative flotation, and the two mainstream flotation processes have the defects that the positive-negative flotation process is high in cost and the double-negative flotation process is poor in stability in practical application. The flotation process which is most widely applied in the existing phosphorite beneficiation is a single reverse flotation process, and the single reverse flotation process has the obvious advantages of good flow stability and low operation cost, but the single reverse flotation process only can remove impurities containing magnesium and basically has no removal effect on impurities containing aluminum. If the synchronous removal of aluminum-containing impurities and magnesium-containing impurities can be realized through medicament system innovation on the basis of single reverse flotation, the method has important significance for the technical progress of phosphorite mineral separation.
Plum-winter lotus and the like (plum-winter lotus, zhouze, plum-Honghong, and the like. Collophanite synchronous reverse flotation test research [ J ] mineral product protection and utilization, 2019,39 (02): 29-33+ 38.) in order to solve the problems of large dosage of pH regulator and complex flotation process in collophanite, a phosphate reagent with the code number of Gz92 and an ammonia reagent with the code number of AE35 are respectively used as reverse flotation collectors of dolomite and quartz, and flotation tests of pure minerals and artificial mixed minerals are carried out under the condition of neutral pulp pH, so that the synchronous reverse flotation has feasibility, and a new way is provided for collophanite beneficiation. However, in actual ore flotation, because the ore pulp system is much more complicated than the pure ore system, the synchronous reverse flotation process has many technical problems to be solved, such as: under the condition of neutral pH value, the flotation process is longer and the phosphorus loss rate is higher due to the lower flotation efficiency of synchronous reverse flotation; under acidic pH conditions, the flotation froth is sticky, leading to poor flow stability, etc.
The patent technology of 'a low-magnesium high-sesqui collophanite synchronous reverse flotation process' (CN 111617885A) discloses a synchronous reverse flotation process for actual phosphorite, which adopts two regulators, namely phosphoric acid and a mixed solution of aluminum chloride, sodium chloride and polyacrylamide in a mass ratio of 0.5-1.5. Compared with a double-reverse flotation process, the method has the advantages that the process structure is more simplified, the flotation cost can be obviously reduced, but the process only has one phosphorus tailing discharge port, organic matters and dolomite with good floatability in raw ores cannot be discharged in time, the organic matters and the dolomite circulate in the process, and great negative influence is brought to the separation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a sorting method with a simple and efficient flow structure and good stability.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following specific steps:
(1) Will P 2 O 5 Grade of 24.0-29.0%, mgO content of 0.8-2.5%, al 2 O 3 2.0 to 4.5 percent of phosphorite slurry with the grain diameter of less than 0.074mm accounting for 60 to 80 percent and the concentration of 20 to 35 weight percent is introduced into a synchronous reverse flotation process; firstly, adding a regulator into phosphorite pulp, then synchronously adding a fatty acid collecting agent and an amine collecting agent into the phosphorite pulp, and performing pre-flotation to obtain a product I and a foam product I in a cell, wherein the foam product I is phosphorus tailings I;
(2) Introducing rough concentration operation into the product I in the tank, adding a fatty acid collecting agent and an amine collecting agent into the product I in the tank, and performing rough concentration to obtain a product II in the tank and a foam product II, wherein the product II in the tank is phosphate concentrate;
(3) Introducing a first scavenging operation into the foam product II, scavenging to obtain a product III in the tank and a foam product III, and returning the product III in the tank to the previous step to enter a roughing operation together with the product I in the tank;
(4) And introducing a second scavenging operation into the foam product III for scavenging to obtain a product IV in the tank and a foam product IV, returning the product IV in the tank to the previous step, and entering the first scavenging operation together with the foam product II, wherein the foam product IV is the phosphate tailings II.
The regulator is prepared by mixing sulfuric acid and aluminum sulfate in a molar ratio of 4.0-7.0: 1.0, and the addition amount of the regulator is 4.0-10.0 kg/t based on the dry basis of the phosphorite slurry.
The reverse flotation process for synchronously removing magnesium and aluminum in phosphorite is characterized in that the mass ratio of the fatty acid collecting agent to the amine collecting agent is 3.0-4.5: 1.0, taking the dry base of the phosphorite slurry as a reference, and respectively adding the total amount of the collecting agents in the pre-flotation operation and the roughing operation to 0.3-0.7 kg/t and 0.4-1.6 kg/t.
The fatty acid collecting agent is sodium salt of oleic acid, linoleic acid, palmitic acid and stearic acid, and the mass ratio of the sodium salt to the fatty acid is 10-18:5-15:10-16:60-65 (preferably 14; the amine collecting agent is acetate of dodecylamine.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
1. compared with a single reverse flotation process, the method provided by the invention has stronger adaptability to phosphate ores, and can be used for treating both carbonate phosphate ores and mixed phosphate ores.
2. The invention adopts the mixture of aluminum sulfate and sulfuric acid as the regulator, can adjust the pH value of the ore pulp to 4.0-5.5 suitable for reverse flotation and demagging, and can also adjust the foam toughness, so that the fluidity of flotation foam is improved, the conveying is facilitated, the problems of difficult foam accumulation and difficult conveying are avoided, and the amine collecting agent can be applied to reverse flotation. The action mechanism of the regulator for regulating the foam toughness can be roughly divided into the following two points, namely, the pH value of ore pulp is reduced by adding sulfuric acid, the surface electronegativity of micro-fine grade mineral particles is weakened, aluminum sulfate is added into the ore pulp, aluminum hydroxide floccules can be generated, a large number of micro-fine grade mineral particles are adsorbed, the electronegativity of the micro-fine grade particles in an ore pulp system is greatly weakened due to the synergistic effect of the sulfuric acid and the aluminum sulfate, the action of the micro-fine grade particles and an amine collecting agent is weakened, the electronegative particles in the foam are reduced, the foam toughness is poor, and the flowability is good.
3. The invention adopts the adding mode of the regulator and the collecting agent, can realize the effect of synchronously removing magnesium and aluminum, and avoids the situations of overlong flotation process and complex backwater system which are difficult to control due to mutual interference between the negative and positive ion collecting agents when adopting a double reverse flotation process.
4. The phosphorus concentrate product P obtained by the invention 2 O 5 Grade greater than 33.0%, mgO content less than 0.8%, al 2 O 3 Content is less than 2.0%, P 2 O 5 The recovery rate is more than 80 percent.
Therefore, the method has the characteristics of strong ore adaptability, simple and compact flow structure, easy control and easy realization of industrialization.
Drawings
FIG. 1 is a flow chart of a reverse flotation process for synchronously removing magnesium and aluminum in phosphorite.
Detailed Description
For better understanding of the present invention, the following description of the present invention is provided in conjunction with the following embodiments and the accompanying drawings, but the present invention is not limited to the following embodiments.
Example 1
A reverse flotation process for synchronously removing magnesium and aluminum in phosphorite. The method of the embodiment comprises the following specific steps:
(1) Will P 2 O 5 Grade 29.0%, mgO content 1.6%, al 2 O 3 The phosphorite pulp with the content of 3.0 percent, the grain diameter of less than 0.074mm accounting for 64.0 percent and the pulp concentration of 30.0 weight percent is introduced into a synchronous reverse flotation process; adding a regulator (a mixture of sulfuric acid and aluminum sulfate in a molar ratio of 7.0; then, synchronously adding a fatty acid collecting agent (a mixture of sodium salts of oleic acid, linoleic acid, palmitic acid and stearic acid in a mass ratio of 4.5 to 1.0, namely 14;
(2) Introducing a product I in a rough concentration operation, synchronously adding a fatty acid collecting agent (a saponified compound consisting of oleic acid, linoleic acid, palmitic acid and stearic acid in a mass ratio of 14 to 14) and an amine collecting agent (laurylamine) into the product I in the tank according to the mass ratio of 3.3;
(3) Introducing a first scavenging operation into the foam product II, scavenging to obtain a product III in the tank and a foam product III, and returning the product III in the tank to the previous step to enter a roughing operation together with the product I in the tank;
(4) And introducing a second scavenging operation into the foam product III for scavenging to obtain a product IV in the tank and a foam product IV, returning the product IV in the tank to the previous step, and entering the first scavenging operation together with the foam product II, wherein the foam product IV is the phosphate tailings II.
P of the phosphate concentrate obtained in this example 2 O 5 Grade 34.17%, mgO content 0.47%, al 2 O 3 Content 1.80%, P 2 O 5 The recovery rate is 90.30%.
In addition, this embodiment also compares the influence of the scavenging times on the mineral separation index, that is, the mineral separation index of the scavenging process including the primary scavenging operation, the secondary scavenging operation, and the tertiary scavenging operation is compared, and the specific table is as follows:
Figure BDA0003011943350000041
as can be seen from the data in the table above, the scavenging process including two scavenging operations is most suitable, and the comparison shows that: when the scavenging process only comprises one scavenging operation, P in the phosphorus tailings II 2 O 5 The grade is higher by 16.20 percent, the reject grade is higher, and the phosphorus concentrate P is caused 2 O 5 The recovery rate is low; when three times of scavenging operation are included, the grade of the phosphate tailings II is not changed greatly, which indicates that no obvious gain is generated when the scavenging operation frequency is continuously increased.
Example 2
A reverse flotation process for synchronously removing magnesium and aluminum in phosphate ore. The method of the embodiment comprises the following specific steps:
(1) Will P 2 O 5 Grade 26.2%, mgO content 1.64%, al 2 O 3 The content of the components is 3.8 percent,introducing phosphorite slurry with particle size less than 0.074mm accounting for 76.0% and pulp concentration of 25.0wt% into a synchronous reverse flotation process; adding a regulator (a mixture of sulfuric acid and aluminum sulfate in a molar ratio of 6.0; then, synchronously adding a fatty acid collecting agent (a mixture of sodium salts of oleic acid, linoleic acid, palmitic acid and stearic acid in a mass ratio of 4.0 to 1.0, namely 14;
(2) Introducing a product I in a cell into roughing operation, synchronously adding a fatty acid collecting agent (a saponified compound consisting of oleic acid, linoleic acid, palmitic acid and stearic acid in a mass ratio of 14.14;
(3) Introducing a first scavenging operation into the foam product II, scavenging to obtain a product III in the tank and a foam product III, and returning the product III in the tank to the previous step to enter a roughing operation together with the product I in the tank;
(4) And introducing a second scavenging operation into the foam product III for scavenging to obtain a product IV in the tank and a foam product IV, returning the product IV in the tank to the previous step, and entering the first scavenging operation together with the foam product II, wherein the foam product IV is the phosphate tailings II.
P of the phosphate concentrate obtained in this example 2 O 5 Grade 33.00%, mgO content 0.46%, al 2 O 3 Content 1.96%, P 2 O 5 The recovery rate is 85.60%.
In addition, in order to examine the synergistic effect of the collectors, the beneficiation effect when only the fatty acid collector or only the amine collector is added is also examined in the embodiment, as shown in the following table:
Figure BDA0003011943350000051
the data in the table above show that the mineral separation index of synchronously adding the two collecting agents is optimal, compared with the situation that only one collecting agent is added, the two collecting agents are synchronously added, and the purpose of synchronously removing magnesium and aluminum can be achieved by utilizing the synergistic effect between the collecting agents. In addition, when only the amine collecting agent is added, the flotation froth has high viscosity and poor fluidity, and the flow cannot be stably operated. Therefore, the agent system and the agent adding mode adopted by the invention not only can synchronously remove the magnesium and the aluminum in the phosphorite, but also has better stability in the flow structure, and avoids the problems of difficult elimination of foam accumulation and difficult transportation caused by the amine collecting agent, so that the amine collecting agent can be applied to reverse flotation.
Example 3
A reverse flotation process for synchronously removing magnesium and aluminum in phosphorite. The method of the embodiment comprises the following specific steps:
(1) Will P 2 O 5 Grade 24.0%, mgO content 2.29%, al 2 O 3 The phosphorite slurry with the content of 3.76 percent, the grain diameter of less than 0.074mm accounting for 80.0 percent and the ore pulp concentration of 35.0 weight percent is introduced into a synchronous reverse flotation process; adding a regulator (a mixture of sulfuric acid and aluminum sulfate in a molar ratio of 4.0; then, synchronously adding a fatty acid collecting agent (a mixture of sodium salts of oleic acid, linoleic acid, palmitic acid and stearic acid in a mass ratio of 3.5 to 1.0, namely 14;
(2) Introducing a product I in a cell into roughing operation, synchronously adding a fatty acid collecting agent (a saponified compound consisting of oleic acid, linoleic acid, palmitic acid and stearic acid in a mass ratio of 14.14;
(3) Introducing a first scavenging operation into the foam product II, scavenging to obtain a product III in the tank and a foam product III, and returning the product III in the tank to the previous step to enter a roughing operation together with the product I in the tank;
(4) And introducing a second scavenging operation into the foam product III for scavenging to obtain a product IV in the tank and a foam product IV, returning the product IV in the tank to the previous step, and entering the first scavenging operation together with the foam product II, wherein the foam product IV is the phosphate tailings II.
P of the phosphate concentrate obtained in this example 2 O 5 Grade 32.98%, mgO content 0.56%, al 2 O 3 Content 2.12%, P 2 O 5 The recovery rate was 82.83%.
Compared with the prior art, the specific implementation mode has the following positive effects:
1. compared with a single reverse flotation process, the method provided by the invention has stronger adaptability to phosphate ores, and can treat both carbonate phosphate ores and mixed phosphate ores.
2. The mixture of aluminum sulfate and sulfuric acid is used as the regulator, the pH value of the ore pulp can be regulated to 4.0-5.5 suitable for reverse flotation and magnesium removal, the foam toughness can be regulated, the mobility of flotation foam is improved, the conveying is facilitated, the problems that foam accumulation is difficult to eliminate and the conveying is difficult are avoided, and the amine cation collecting agent can be applied to reverse flotation. The action mechanism of the regulator for regulating the foam toughness can be roughly divided into the following two points, namely, the pH value of ore pulp is reduced by adding sulfuric acid, the surface electric property of micro-fine grade mineral particles is weakened, aluminum sulfate is added into the ore pulp, aluminum hydroxide floccules can be generated, a large number of micro-fine grade mineral particles are adsorbed, the electronegativity of the micro-fine grade particles in an ore pulp system is greatly weakened due to the synergistic effect of the sulfuric acid and the aluminum sulfate, the action of the micro-fine grade particles and an amine cation collecting agent is weakened, the electronegative particles in the foam are reduced, the foam toughness is poor, and the flowability is good.
3. The adding mode of the regulator and the collecting agent adopted by the specific embodiment can realize the effect of synchronously removing magnesium and aluminum, and avoids the situations of too long flotation flow and complex backwater system and difficult control caused by mutual interference between the negative and positive ion collecting agents when a double-reverse flotation process is adopted.
4. The phosphate concentrate product P obtained by the present embodiment 2 O 5 Grade greater than 33.0%, mgO content less than 0.8%, al 2 O 3 Content less than 2.0%, P 2 O 5 The recovery rate is more than 80 percent.
Therefore, the specific implementation mode has the characteristics of strong ore adaptability, simple and compact flow structure, easy control and easy realization of industrialization.

Claims (1)

1. The reverse flotation process for synchronously removing magnesium and aluminum in phosphorite is characterized by comprising the following steps:
(1) Will P 2 O 5 Grade 29.0%, mgO content 1.6%, al 2 O 3 The phosphorite pulp with the content of 3.0 percent, the grain diameter of less than 0.074mm accounting for 64.0 percent and the pulp concentration of 30.0 weight percent is introduced into a synchronous reverse flotation process; adding a regulator into the phosphate ore slurry, wherein the regulator is a mixture of sulfuric acid and aluminum sulfate in a molar ratio of 7.0; then, synchronously adding a fatty acid collecting agent and an amine collecting agent into the phosphorus ore pulp according to the mass ratio of 4.5: 10:14:62, an amine collecting agent is lauryl amine acetate, the total adding amount of the collecting agent is 0.3kg/t, and pre-flotation is carried out to obtain a product I in the cell and a foam product I, wherein the foam product I is phosphate tailings I;
(2) Introducing a product I in the cell into roughing operation, synchronously adding a fatty acid collecting agent and an amine collecting agent into the product I in the cell according to a mass ratio of 3.3: 10:14: 62. the amine collecting agent is dodecylamine, the total adding amount of the collecting agent is 0.4kg/t, rough separation is carried out to obtain a product II and a foam product II in the cell, and the product II in the cell is phosphate concentrate;
(3) Introducing a first scavenging operation into the foam product II, scavenging to obtain a product III in the tank and a foam product III, and returning the product III in the tank to the previous step to enter a roughing operation together with the product I in the tank;
(4) And introducing a second scavenging operation into the foam product III for scavenging to obtain a product IV in the tank and a foam product IV, returning the product IV in the tank to the previous step, and entering the first scavenging operation together with the foam product II, wherein the foam product IV is the phosphate tailings II.
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CN113695087A (en) * 2021-08-13 2021-11-26 武汉工程大学 Method and equipment for reclaiming available phosphorus from roughly and scavenged phosphorus tailings through middle-column type recleaning
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