CN117443590A - Method for removing iron and reducing arsenic cooperatively by collophanite reverse flotation - Google Patents

Method for removing iron and reducing arsenic cooperatively by collophanite reverse flotation Download PDF

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Publication number
CN117443590A
CN117443590A CN202311359038.3A CN202311359038A CN117443590A CN 117443590 A CN117443590 A CN 117443590A CN 202311359038 A CN202311359038 A CN 202311359038A CN 117443590 A CN117443590 A CN 117443590A
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China
Prior art keywords
flotation
collophanite
arsenic
dosage
agent
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CN202311359038.3A
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Inventor
胡盘金
郑光明
李防
孙桦林
雍青
邓光政
曾庆林
彭飞
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Yidu Xingfa Chemical Co ltd
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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
    • B03D1/001—Flotation agents
    • B03D1/018—Mixtures of inorganic and organic compounds
    • 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
    • B03D1/14—Flotation machines
    • 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
    • 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
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/04—Frothers
    • 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

Abstract

The invention discloses a method for removing iron and arsenic cooperatively by reverse flotation of collophanite, which is used for preferentially separating arsenopyrite and pyrite before removing magnesium on the premise of not influencing the main process for removing impurities. Firstly, adding water into ground collophanite for pulping, transferring into a flotation machine, sequentially adding a proper amount of activating agent, collecting agent and foaming agent, maintaining stable high entropy mass transfer condition of flotation pulp, and finally, selecting sulfide ore foam with stable property through intensified flotation process control. The reverse flotation obtains rough concentrate with iron content less than 0.30%, arsenic content less than 200mg/kg, and phosphorus recovery rate more than 94%. The invention removes arsenic and iron through reverse flotation in the beneficiation stage, has the advantages of simple flow, easy control, no interference to main flow flotation impurity removal and the like, and has good development prospect in the aspect of collophanite cooperative impurity removal.

Description

Method for removing iron and reducing arsenic cooperatively by collophanite reverse flotation
Technical Field
The invention belongs to the field of mineral processing engineering, and particularly relates to a method for cooperatively removing iron and arsenic by collophanite reverse flotation.
Background
Phosphorus element is one of the essential macroelements for growth and development of animals and plants, and phosphate ore is gradually developed into an important chemical raw material, and is widely used for producing yellow phosphorus, phosphoric acid, phosphate fertilizer and various phosphates. Collophanite is an ore aggregate containing a small amount of elements such as magnesium, aluminum, silicon, iron, arsenic and the like, mainly phosphate. Iron-bearing minerals are classified into oxidized minerals and sulfidic minerals, the sulfidic minerals are mainly pyrite, arsenic is derived from arsenopyrite, and the iron-bearing minerals and the arsenopyrite are similar to each other in terms of similarity, and have similar crystal structures, surface chemistry and solution chemistry. Iron and arsenic elements can enter the finished acid through wet phosphoric acid, and the downstream product quality is affected. Arsenic content in the phosphate fertilizer exceeds standard, and the arsenic can enter a food chain through biological circulation, so that the health of a human body is affected. The national fertilizer and soil conditioner standardization technical committee divides chemical fertilizer into garden, farmland and ecological levels. The garden grade fertilizer can not be applied to edible plants, and the total arsenic content is less than or equal to 50mg/kg; the farmland-grade fertilizer can be suitable for edible plants, and the total arsenic content is less than or equal to 25mg/kg; the ecological fertilizer can be applied to any plants, and the total arsenic content is less than or equal to 10mg/kg. Various phosphates can be used as feed additives, and arsenic content in the phosphate is one of the important factors limiting its development. The national standard GB/T22549-2017 and GB 22548-2017 specify that the arsenic content of calcium hydrophosphate and calcium biphosphate as feed additives is less than or equal to 20mg/kg, and the national standard GB 34470-2017 specifies that the total arsenic content of potassium biphosphate added into the feed is less than or equal to 10mg/kg. The performance of a new energy battery using phosphoric acid as a base material is also limited by the iron and arsenic content of the phosphate. Therefore, a new method for removing iron and reducing arsenic from collophanite is needed to be developed, and elements such as iron and arsenic are removed in the beneficiation process, so that the method has important significance for fine phosphorus chemical industry.
The key point of reverse flotation of sulphide ore from oxidized ore is pulp blending, flotation reagent selection and intensified control of flotation process. Chinese patent CN1544155 uses copper sulfate and amyl xanthate as activators and collectors to flash activate gold-bearing pyrite and arsenopyrite. The Chinese patent CN123019706 can increase the floatation speed of pyrite by adding ferrous sulfate, citric acid and copper sulfate to activate pyrite inhibited by calcium oxide. The single salt has limited activation capability on a small amount of sulfide ores in oxidized ores, and a single xanthate collector cannot have selectivity and collecting capability, so that removal of sulfide ores in a collophanite reverse flotation method is difficult to realize.
Disclosure of Invention
Aiming at the problem that the impurity of the sulfide mineral containing iron and arsenic affects the quality of downstream phosphorus chemical products, the invention aims to provide a method for removing iron and arsenic cooperatively at a collophanite processing source through reverse flotation, in particular to a method for separating pyrite and arsenopyrite through reverse flotation before magnesium removal. Mainly comprises three links of ore particle slurrying, medicament mass transfer and process strengthening control. Flotation gave a coarse concentrate with less than 0.30% iron and less than 200mg/kg arsenic.
The technical scheme adopted by the invention comprises the following steps:
1. pulping ore particles: adding the ground collophanite into acid wastewater for pulping to obtain ore pulp with the concentration of 15-35%, and stirring uniformly and good dispersibility, wherein the acid wastewater can be used as a pyrite and arsenopyrite activator, and can also change the outer layer electrical properties of the double electric layers of apatite and gangue minerals, thereby indirectly influencing the action form between mineral particles and a collector; the raw ore or rough concentrate has a phosphorus grade of 20-29%, contains iron of 0.5-2%, arsenic of 0.01-0.2%, and mineral particles with particle diameters below 74um account for 70-85%, wherein the particle diameters are less than 38um and 45-60%;
2. mass transfer of the medicament: and (2) sequentially adding a plurality of activators, collectors and foaming agents into the uniform ore pulp obtained in the step (1), and transferring the uniform ore pulp into a flotation machine, thereby creating powerful conditions for mass transfer enhancement of flotation agents in a flotation medium.
1) The activating agent in the step 2 comprises inorganic acid and inorganic salt, mainly comprises two or more of sulfuric acid, nitric acid, phosphoric acid, oxalic acid, copper sulfate, lead nitrate, ammonium sulfate, ammonium chloride, ammonium bisulfate and ammonium nitrate, and the dosage is 1kg/t-10kg/t; the proportion of the inorganic acid to the salt is 5:1-20:1, the inorganic acid can adjust the pH value of ore pulp, and the adjusting and controlling range is 4.0-7.0; the inorganic acid has an activating effect, the oxidation-reduction property of ore pulp is changed through H+ mass transfer, the oxidation-reduction potential of pyrite and arsenopyrite in an acidic medium is higher, oxidation of sulfur elements on the surface of the sulfide mineral is facilitated to be a hydrophobic sulfur-rich film, and floatability of pyrite and arsenopyrite is improved; on the other hand, the selective inhibition effect is exerted, the positioning ions of the double-electric-layer structure of the apatite are H+ and OH, the concentration of H+ in ore pulp is increased by adding inorganic acid, the outer layer electrical property of the double-electric-layer structure of the apatite is changed, and the apatite can be effectively inhibited; the ammonium salt can erode the hydrophilic oxide layer on the surface of the sulphide ore to expose the fresh surface and improve the hydrophobicity, and the metal ions in the metal salt can increase the active sites on the surface of the mineral, so that the ammonium salt has synergistic activation effect when being matched with the ammonium salt.
2) The collecting agent in the step 2 is two or more of butyl sodium xanthate, amyl sodium xanthate, isoamyl sodium xanthate, hexyl sodium xanthate, butylammonium black drug and No. 25 black drug, and the dosage is 30-300g/t; the synergistic use of various xanthates and black drugs gives consideration to the collecting capacity and selectivity, and can improve the floating rate of pyrite, arsenopyrite and other sulfide minerals; secondly, the inorganic salt added in the step 1) absorbs and transfers mass to the surface of the mineral, so that the interfacial chemical reaction between the mineral and the collector is enhanced, the active area and the action site of the surface of the mineral are enhanced, part of xanthate molecules and activated ions on the surface of the mineral generate more stable xanthate, and xanthate is strengthened from a single dual xanthate form into a form of combined action of xanthate and dual xanthate through the absorption and the mass transfer of activated ions.
3) The foaming agent in the step 2 comprises two or more of pine oil, methyl isobutyl carbinol, eucalyptus oil and camphor oil, and the dosage is 20-60g/t.
4) In the step 2, the arsenic-containing mineral flotation adopts one-stage dosing or sectional dosing flotation, the initial speed of flotation can be accelerated by one-stage dosing, the selectivity of a collector is reduced, part of apatite enters the dearsenified tailings through mechanical entrainment, the sectional flotation can indirectly control the mineral flotation speed by adjusting the dosage of the reagent, the function of the flotation reagent is effectively exerted, the dosage of the reagent is reduced, the mechanical entrainment can be avoided to a certain extent, the dosage of one-stage reagent in the sectional dosing process is 50% -70%, and the dosage of the second-stage reagent is 30% -50%.
3. And (3) process control: mineral pulp with high entropy mass transfer condition of the minerals and the medicament is selected in an inflatable flotation machine with the rotating speed of 1000-2000 r/min, and the flotation gas is mixed air mixed with part of inert gases such as nitrogen, helium or argon; the inert gas can prevent the excessive oxidation of the arsenopyrite and pyrite, maintain a stable hydrophobic surface and increase the difference of the hydrophilicity and hydrophobicity of the arsenopyrite and pyrite and the oxidized ores such as apatite, dolomite, feldspar and the like. The flotation scraping frequency is controlled to be 4-6 seconds/plate in the process control, and the flotation time is 4-10 minutes. The flotation foam scraping frequency is controlled to be 4-6 seconds/plate in the process control, the foam scraping frequency is strictly controlled, the loss of phosphorus-containing minerals caused by mechanical entrainment is avoided, and the foam scraping time is 4-10 minutes.
Detailed Description
The present invention will be described in further detail with reference to examples. The following examples are only intended to illustrate the present invention and not to limit the scope of the invention.
Example 1
Some calcium type collophanite is composed of apatite, dolomite, calcite, pyrite and a small amount of arsenopyrite, the main iron-containing mineral is pyrite, and a small amount of arsenopyrite is also included. The specific chemical components are as follows: p (P) 2 O 5 28.55%、Fe1.09%、As 0.08%。
Firstly, grinding collophanite with the proportion of 74 mu m to 82-85%, and adjusting the concentration to be 28-30%; sequentially adding an activating agent, a collecting agent and a foaming agent, wherein the activating agent is prepared from inorganic acid and inorganic salt according to a ratio of 14:1, the inorganic acid is added at one time, the using amount of the inorganic acid is 4.2kg/t, the inorganic acid is mainly sulfuric acid, phosphoric acid and oxalic acid, and the using amount of the inorganic salt is 0.3kg/t, and the inorganic salt comprises ammonium sulfate, ammonium bisulfate and ammonium chloride; sodium butylxanthate,Sodium amyl xanthate, sodium isoamyl xanthate, sodium hexyl xanthate and butylammonium black drug are mixed to be used as collecting agents, and the dosage of each agent is 20g/t; then pine oil, methyl isobutyl carbinol and eucalyptus oil are added as foaming agents, and the dosage of the three agents is 10g/t respectively. Finally, mixed air containing 20% helium is introduced as flotation gas, the rotating speed of a flotation machine is adjusted to 1900 r/min, the scraper frequency is 5 seconds/plate, and the flotation time is 7min; roughing to obtain P 2 O 5 29.49%, fe 0.23% and As 80 mg/kg.
Example 2
The main minerals of certain weathered calcareous collophanite are apatite, dolomite, calcite, and small amount of pyrite and arsenopyrite, and the main chemical components are as follows: p (P) 2 O 5 26.34%、Fe1.78%、As 0.11%。
Adding acid backwater into weathered calcareous collophanite through a ball mill to grind until the proportion of-74 μm is 82%. Transferring the ground collophanite into a flotation tank, and regulating the concentration to be 27%; the activator is added according to the proportion of inorganic acid to inorganic salt of 14:1, the total dosage is 6kg/t, the dosage of inorganic acid is 5.6 kg/t, the inorganic acid is mainly sulfuric acid, phosphoric acid and oxalic acid, the dosage of inorganic salt is 0.4 kg/t, the inorganic salt is mainly copper sulfate, lead nitrate, ammonium sulfate, ammonium bisulfate and ammonium chloride, wherein the dosage of the roughing first-stage combined activator is 60% of the total dosage, and the dosage of the roughing second-stage activator is 40%; the sodium butylxanthate, sodium isoamyl xanthate and butylammonium black drug are used as collecting agents, the dosage is 50g/t respectively, and the dosage of the roughing first section and the roughing second section is 50 percent. Then pine oil, methyl isobutyl carbinol and eucalyptus oil are added as foaming agents, and the dosage is 10g/t respectively. Finally, air and helium are introduced as flotation gas, the ratio is 8:2, the rotating speed of a flotation machine is adjusted to 1900 r/min, the scraping plate frequency is 5 seconds/plate, and the scraping time is 5 min; rough concentrate P obtained by two-stage roughing 2 O 5 27.26%, fe0.28% and As content 120mg/kg.
Example 3
The main minerals of certain silica-lime collophanite are apatite, potassium feldspar, albite, quartz, dolomite, calcite, pyrite and arsenopyrite, and the main chemical components are as follows: p (P) 2 O 5 24.58%, fe1.56% and As 0.06%. The method comprisesThe method comprises the steps of grinding the silicon-calcium collophanite by using a ball mill until the ore concentration is 65% and the ore pulp concentration is adjusted to 33%, and adding etheramine and quaternary ammonium under the weak alkaline condition to remove aluminosilicate.
Adding acid backwater into ore pulp after reverse flotation desilication to dilute the ore pulp, and adjusting the concentration to 25%; then sequentially adding inorganic acid and inorganic salt in a specific proportion of 15:1, wherein the total dosage is 8kg/t, the dosage of the inorganic acid is 7.5 kg/t, the inorganic acid is mainly sulfuric acid, phosphoric acid and oxalic acid, the dosage of the inorganic salt is 0.5 kg/t, the inorganic salt is mainly copper sulfate, lead nitrate, ammonium sulfate, ammonium chloride, ammonium bisulfate and ammonium nitrate, and the dosage of roughing one-stage and two-stage activators is 7:3; the consumption of the collecting agent is 150g/t, wherein the consumption of the sodium amyl xanthate and the sodium isoamyl xanthate is 50g/t, the consumption of the sodium hexyl xanthate and the black butyl ammonium is 25g/t, and the consumption of the first-stage roughing and the second-stage roughing is 65 percent and 35 percent respectively. A mixture of pine oil, methyl isobutyl methyl alcohol and eucalyptus oil was added as foaming agent at 10g/t each. Finally, mixed air containing 20% of argon is introduced as flotation gas, the rotating speed of a flotation machine is adjusted to 1900 r/min, the scraper frequency is 5 seconds/plate, and the flotation time is 5 min; obtaining P through two-stage roughing 2 O 5 25.12%, fe0.30%, and As40 mg/kg.
Example 4
The certain arsenic-containing medium-low grade silicon-calcium collophanite is composed of apatite, potassium feldspar, quartz, dolomite, pyrite and arsenopyrite, wherein arsenic-containing minerals are arsenopyrite, and the specific chemical components are as follows: p (P) 2 O 5 22.64%, fe1.88% and As 0.13%. The silica-lime collophanite adopts the sequential impurity removal flow of reverse flotation arsenic removal, reverse flotation magnesium removal and alkaline reverse flotation aluminum removal.
Firstly, grinding and grading collophanite, wherein the grinding fineness is 79 percent of the proportion of-74 mu m, and the concentration of ore pulp is regulated to 30 percent. And sequentially adding a proper amount of activating agent, collecting agent and foaming agent to perform reverse flotation dearsenification. The dosage of the activating agent is 4kg/t, the dosage of the mixed acid consisting of sulfuric acid, phosphoric acid and oxalic acid is 3.8kg/t, and the dosage of inorganic salts such as copper sulfate, lead nitrate, ammonium sulfate, ammonium chloride, ammonium bisulfate, ammonium nitrate and the like is 0.2kg/t; the amount of the collector is 200g/t,wherein, the concentration of sodium amyl xanthate, sodium isoamyl xanthate and sodium hexyl xanthate is 50g/t each, and the concentration of the black drug in # 25 and the concentration of the black drug in butyl ammonium are 25g/t each; the combination of pine and eucalyptus oils was 15g/t each as a foaming agent. The reverse flotation deironing and arsenic reduction, the two sections of processes are respectively and independently dosed, the dosage of the first section of medicament accounts for 70% of the total dosage, and the dosage of the second section of flotation medicament accounts for 30%. The mixed air containing 20% of argon is used as flotation gas, the rotation speed of a flotation machine is adjusted to 1900 r/min, the scraper frequency is 5 seconds/plate, and the flotation time is 4 min. Two-stage flotation to remove arsenic can obtain P 2 O 5 22.89%, fe0.26% and As 70 mg/kg.

Claims (7)

1. The method for removing iron and arsenic cooperatively by collophanite reverse flotation is characterized by comprising the following steps of:
(1) Adding collophanite into acid wastewater for size mixing to obtain evenly dispersed ore pulp;
(2) Sequentially adding an activating agent, a collecting agent and a foaming agent into the uniform ore pulp obtained in the step (1), and then carrying out aerated flotation;
the activating agent is selected from two or more of sulfuric acid, nitric acid, oxalic acid, phosphoric acid, copper sulfate, lead nitrate, ammonium sulfate, ammonium chloride, ammonium bisulfate and ammonium nitrate;
the collector is selected from two or more of sodium butyl xanthate, sodium amyl xanthate, sodium isoamyl xanthate, sodium hexyl xanthate, butylammonium black drug and 25# black drug;
the foaming agent is selected from two or more of pine oil, methyl isobutyl carbinol, eucalyptus oil and camphor oil.
2. The method for synergistic deironing and arsenic reduction by collophanite reverse flotation according to claim 1, wherein the flotation raw ore has a phosphorus grade of 20-29%, iron content of 0.5-2%, arsenic content of 0.01-0.2%, and acid wastewater is added to adjust the concentration of ore pulp to 15-35%.
3. The method for synergistic deironing and arsenic reduction in collophanite reverse flotation according to claim 1, wherein the ore pulp is subjected to flotation in an aerated flotation machine with a rotational speed of 1000-2000 r/min after addition of activator, collector and frother.
4. A method for synergistic iron and arsenic removal by reverse flotation of collophanite as claimed in claim 3, wherein air containing inert atmosphere is introduced during flotation, the flotation scraping frequency is controlled to be 4-6 seconds/plate, and the flotation time is 4-10min.
5. The method for synergistic deironing and arsenic reduction by collophanite reverse flotation according to claim 4, wherein the inert atmosphere is selected from any one of nitrogen, helium or argon.
6. The method for synergistic deironing and arsenic reduction by collophanite reverse flotation according to claim 1, wherein the dosage of the activator is 1-10kg/t;
the dosage of the collecting agent is 30-300g/t;
the dosage of the foaming agent is 20-60g/t.
7. The method for synergistic iron and arsenic removal by reverse flotation of collophanite as claimed in claim 1 or 6, wherein the activator, collector and foaming agent are added by two-stage dosing, wherein the dosage of one stage of agent is 50-70% of the total dosage, and the dosage of the two stages of agent is 30-50%.
CN202311359038.3A 2023-10-19 2023-10-19 Method for removing iron and reducing arsenic cooperatively by collophanite reverse flotation Pending CN117443590A (en)

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