CN111438002A - Method for treating silicon-calcium collophanite by 'floating-chemical' coupling - Google Patents
Method for treating silicon-calcium collophanite by 'floating-chemical' coupling Download PDFInfo
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- CN111438002A CN111438002A CN202010310984.9A CN202010310984A CN111438002A CN 111438002 A CN111438002 A CN 111438002A CN 202010310984 A CN202010310984 A CN 202010310984A CN 111438002 A CN111438002 A CN 111438002A
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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
- B03D1/02—Froth-flotation processes
- B03D1/021—Froth-flotation processes for treatment of phosphate ores
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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
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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
- B03D1/12—Agent recovery
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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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
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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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
- 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 provides a method for treating silico-calcium collophanite by 'floating-chemical' coupling, which comprises the steps of firstly carrying out direct flotation on silico-calcium collophanite to obtain flotation concentrate and high-silicon tailings, then carrying out demagging treatment on the flotation concentrate to obtain phosphate concentrate, and carrying out calcium separation treatment on demagging mother liquor obtained by the demagging treatment to obtain gypsum whiskers and phosphoric acid solution. The invention removes silicon-containing minerals in the collophanite through direct flotation, reduces the content of magnesium in the collophanite through a chemical method, and improves the phosphorus taste in the collophanite, so that the obtained phosphate concentrate meets the requirement of wet-process phosphoric acid.
Description
Technical Field
The invention relates to the technical field of waste resource utilization, in particular to a method for treating silico-calcium collophanite by 'floating-chemical' coupling.
Background
The phosphorite resources in China are rich, the reserves are the second place in the world, but the rich ore is less, the lean ore is more, most of the phosphorite is the middle-low grade calcium collophanite, the content of harmful substances in the ore is generally higher, the phosphorus mineral and the gangue mineral are closely symbiotic, the disseminated granularity is fine, and the phosphorite belongs to the difficultly-selected phosphorite. Therefore, the development and utilization of the medium-low grade collophanite become the problem which is urgently to be solved for guaranteeing the sustainable development of resources.
Hand selection has been the main beneficiation means until the beginning of the 19 th century, and later, with the rise of labor cost and the improvement of other beneficiation methods, manual selection is rapidly declined. At present, the types of the ore dressing process of the phosphate ore are extremely various, but the common ore dressing process is a flotation process, a roasting-digestion process, a heavy medium ore dressing process, a scrubbing and desliming process and a combined ore dressing process, wherein the flotation process is the most direct and effective method for enriching the phosphate ore at the present stage and is also much concerned by ore dressing researchers. While collophanite is often mixed with carbonate (containing MgO and CaO) mineral and calcium silicate (containing SiO)2CaO), minerals, argillaceous substances (containing Al)2O3、SiO2) Minerals and the like various gangue minerals coexist. Therefore, different flotation processes need to be selected according to different gangue minerals during mineral separation. In summary, the beneficiation processes are roughly as follows: the method comprises a single positive flotation desiliconization test, a single reverse flotation desiliconization test, a positive-reverse flotation desiliconization-first-then-demagnetisation test, a reverse-positive flotation desiliconization-first-second test and a double reverse flotation desiliconization-first-demagnetisation-second test.
The single direct flotation of phosphorite is to sort out apatite in collophanite to obtain phosphate concentrate directly. It is suitable for medium grade phosphate ore with simple structure. Grinding the phosphorite to a certain fineness, adding a series of regulators, and bubbling to obtain qualified phosphate concentrate.
Magnesium is a main harmful impurity in the process of treating phosphorite by an acid method, the decomposition rate of the phosphorite is reduced, the consumption of acid is increased, and the difficulty in filtration and the high moisture absorption of downstream products are caused. In order to smoothly carry out the production of phosphorus chemical industry and improve the quality of phosphorus chemical industry products, the high-magnesium phosphorite needs to be subjected to magnesium removal treatment. The low-grade phosphorite can generate a large amount of leaching waste liquid containing metal ions in the process of magnesium removal, if the leaching waste liquid is directly discharged, the leaching waste liquid can cause serious harm to the environment, and magnesium resources are wasted. In order to realize tail-free discharge in the phosphorite magnesium removal process and achieve the purpose of resource utilization, the treatment of magnesium removal waste liquid is an urgent problem to be solved in the industry of phosphorization industry.
The recycling of the magnesium-removed waste phosphorite liquid is mainly used for extracting magnesium from the leaching waste liquid, and the method mainly comprises the following steps: emulsion membrane process, solvent extraction process, ion exchange process, chemical precipitation process. Although the solvent extraction method can extract part of magnesium ions, the cost of the extractant is high; the ion exchange method has better magnesium extraction effect, but the resin consumption is large, and the method is not suitable for industrial production. The chemical precipitation method utilizes a precipitator and magnesium ions in the magnesium removal waste liquid to form precipitates so as to achieve the effect of separating magnesium. When the chemical precipitation method is widely applied, gypsum whiskers are mainly obtained, are novel materials with excellent performance and wide market prospect, and have extremely wide development prospect in the aspects of filling materials, reinforcing materials, friction materials, filtering materials, asphalt modification and the like.
In the prior art, some researches on the comprehensive utilization of silicon-calcium collophanite have been carried out, and a Chinese patent with publication number of CN 108927294A discloses a flotation method of silicon-calcium collophanite, which firstly selects a fatty acid anion collecting agent to carry out reverse flotation on quartz and silicate minerals, effectively reduces the contents of MgO and SiO2 in the collophanite, and has the advantages of simple and novel process, stable flow and low beneficiation cost. The invention discloses a siliceous collophanite direct flotation collecting agent and a preparation method thereof, wherein 6-9 parts of triethanolamine sodium oleate, 1-2 parts of anionic surfactant and 1-3 parts of mixed fatty alcohol are uniformly stirred and mixed at normal temperature to prepare the siliceous collophanite direct flotation collecting agent. The Chinese patent with publication number CN 110813543A discloses a silico-calcium collophanite double reverse flotation process for recovering tailing resources through acid leaching, which returns mixed acid produced by phosphate tailings to the reverse flotation magnesium removal operation of phosphate, greatly reduces the discharge of the phosphate tailings, reduces the consumption of concentrated sulfuric acid, and has great application prospect in the aspects of energy conservation and emission reduction. The chinese patent publication No. CN 107309075 a discloses a collophanite beneficiation method, which separates coarse fraction ore pulp and fine fraction ore pulp by controlling the ore grinding particle size of the collophanite, wherein the coarse fraction ore pulp is not subjected to flotation treatment, and only the fine fraction ore pulp is subjected to flotation, thereby saving the usage amount of flotation reagents, reducing the flotation flow, and lowering the flotation cost.
This patent has improved the phosphorus taste of flotation concentrate through combining flotation and chemical demagging technology, utilizes the demagging waste liquid after the chemical demagging simultaneously, changes it into the gypsum whisker, has increased the added value of phosphorite, has also reduced the waste of resource.
Disclosure of Invention
In view of the above, the invention aims to provide a method for treating calcium silicon collophanite by floating-chemical coupling, so as to solve the problem that the resource utilization rate of the existing low-and-medium-grade collophanite is low due to difficult treatment.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a method for treating silicon-calcium collophanite by 'floating-chemical' coupling comprises the following steps:
1) placing the silicon-calcium collophanite in a flotation machine, adding water, and stirring to obtain ore pulp;
2) sequentially adding sodium carbonate, sodium silicate and a sulfofatty acid collecting agent into the ore pulp, and performing direct flotation to obtain flotation concentrate and high-silicon tailings;
3) mixing the flotation concentrate with phosphoric acid, performing a demagging reaction, and after the demagging reaction is finished, performing suction filtration to obtain a phosphate concentrate and a demagging mother liquor;
4) and adding a precipitator into the magnesium-removing mother liquor to perform calcium precipitation reaction, and obtaining gypsum whiskers and a phosphoric acid solution after the calcium precipitation reaction is finished.
Optionally, the concentration of the ore pulp in the step 1) is 20-40%.
Optionally, the adding amount of the sodium carbonate, the sodium silicate and the sulfofatty acid collector in the ore pulp of the step 2) is 2-10kg/t, 0.5-5kg/t and 0.4-3kg/t respectively.
Optionally, the reaction time of the direct flotation in the step 2) is 3-10min, and the aeration and bubble scraping time is 5-15 min.
Optionally, the mass fraction of the phosphoric acid in the step 3) is 20-60%.
Optionally, the reaction temperature of the magnesium removal reaction in the step 3) is 50-100 ℃, and the reaction time is 2-5 h.
Optionally, the precipitating agent in step 4) is sulfuric acid or ammonium sulfate.
Optionally, the adding amount of the precipitant in the step 4) is 1-1.5 times of the amount of the calcium substance in the magnesium-removing mother liquor.
Compared with the prior art, the method for treating the silicon-calcium collophanite by the floating-chemical coupling treatment has the following advantages:
1. the invention removes silicon-containing minerals in the collophanite through direct flotation, reduces the content of magnesium in the collophanite through a chemical method, and improves the phosphorus taste in the collophanite, so that the obtained phosphate concentrate meets the requirement of wet-process phosphoric acid.
2. The raw materials used in the method are relatively difficult to treat collophanite, the process is relatively simple and short, the operation is convenient, and a theoretical basis is provided for the burden reduction and income increase of enterprises.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a process flow diagram of the floating-chemical coupling method for treating silica-calcium collophanite according to the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention will be described in detail below with reference to the drawings and examples.
Example 1
Referring to fig. 1, the method for processing silico-calcic collophanite by "floating-chemical" coupling of this embodiment specifically includes the following steps:
1) 500g of silico-calcium collophanite is taken and placed in a flotation machine, 1220ml of water is added, and the mixture is fully and evenly stirred to prepare ore pulp;
2) adding 3kg/t of sodium carbonate, 2kg/t of sodium silicate and 2kg/t of sulfofatty acid collecting agent into the ore pulp in sequence, stirring for 5min after the adding is finished, then ventilating and scraping for 5min, carrying out positive flotation, and then, draining the concentrate product and the tailing product to obtain flotation concentrate and high-silicon tailing;
3) placing the flotation concentrate obtained in the step 2) into a 1000ml three-neck flask, heating the flotation concentrate to 75 ℃ in an oil bath, slowly adding 50ml of 40% phosphoric acid for mixing, performing demagging reaction for 3.5 hours, and performing suction filtration to obtain phosphate concentrate and demagging mother liquor;
4) and (3) transferring the demagging mother liquor obtained in the step 3) into a beaker, adding 60ml of 98% sulfuric acid, performing calcium precipitation reaction, after the calcium precipitation reaction is finished, performing suction filtration to obtain gypsum whiskers and a phosphoric acid solution, wherein the phosphoric acid solution is used for demagging the phosphate concentrate in the next flotation.
Example 2
Referring to fig. 1, the method for processing silico-calcic collophanite by "floating-chemical" coupling of this embodiment specifically includes the following steps:
1) 500g of silico-calcium collophanite is taken and placed in a flotation machine, 1100ml of water is added, and the mixture is fully and evenly stirred to prepare ore pulp;
2) adding 5kg/t of sodium carbonate, 3.5kg/t of sodium silicate and 1.8kg/t of sulfo fatty acid collecting agent into the ore pulp in sequence, stirring for 6min after the adding is finished, then ventilating and scraping for 8min, carrying out positive flotation, and then, drying a concentrate product and a tailing product to obtain flotation concentrate and high-silicon tailing;
3) placing the flotation concentrate obtained in the step 2) into a 1000ml three-neck flask, heating the flotation concentrate to 80 ℃ in an oil bath, slowly adding 60ml of 50% phosphoric acid for mixing, performing demagging reaction for 4.5 hours, and performing suction filtration to obtain phosphate concentrate and demagging mother liquor;
4) and (3) transferring the demagging mother liquor obtained in the step 3) into a beaker, adding 65ml of 98% sulfuric acid, performing calcium precipitation reaction, after the calcium precipitation reaction is finished, performing suction filtration to obtain gypsum whiskers and a phosphoric acid solution, wherein the phosphoric acid solution is used for demagging the phosphate concentrate in the next flotation.
Example 3
Referring to fig. 1, the method for processing silico-calcic collophanite by "floating-chemical" coupling of this embodiment specifically includes the following steps:
1) 500g of silico-calcium collophanite is taken and placed in a flotation machine, 1010ml of water is added, and the mixture is fully and evenly stirred to prepare ore pulp;
2) adding 5.5kg/t of sodium carbonate, 3.2kg/t of sodium silicate and 3.2kg/t of sulfo fatty acid collecting agent into the ore pulp in sequence, stirring for 6min after the adding is finished, then ventilating and scraping for 12min, performing direct flotation, and then, draining the concentrate product and the tailing product to obtain flotation concentrate and high-silicon tailing.
3) Placing the flotation concentrate obtained in the step 2) into a 1000ml three-neck flask, heating the flotation concentrate to 65 ℃ in an oil bath, slowly adding 32ml of 55% phosphoric acid, mixing, performing demagging reaction for 4.5 hours, and performing suction filtration to obtain phosphate concentrate and demagging mother liquor;
4) and (3) transferring the demagging mother liquor obtained in the step 3) into a beaker, adding 60ml of 98% sulfuric acid, performing calcium precipitation reaction, after the calcium precipitation reaction is finished, performing suction filtration to obtain gypsum whiskers and a phosphoric acid solution, wherein the phosphoric acid solution is used for demagging the phosphate concentrate in the next flotation.
Example 4
Referring to fig. 1, the method for processing silico-calcic collophanite by "floating-chemical" coupling of this embodiment specifically includes the following steps:
1) 500g of silico-calcium collophanite is taken and placed in a flotation machine, 950ml of water is added, and the mixture is fully and evenly stirred to prepare ore pulp;
2) adding 6.5kg/t of sodium carbonate, 3.1kg/t of sodium silicate and 1.5kg/t of sulfo fatty acid collecting agent into the ore pulp in sequence, stirring for 9min after the adding is finished, then ventilating and scraping for 14min, performing direct flotation, and then, drying a concentrate product and a tailing product to obtain flotation concentrate and high-silicon tailing;
3) placing the flotation concentrate obtained in the step 2) into a 1000ml three-neck flask, heating the flotation concentrate to 80 ℃ in an oil bath, slowly adding 30ml of 58% phosphoric acid for mixing, performing demagging reaction for 2.5 hours, and performing suction filtration to obtain phosphate concentrate and demagging mother liquor;
4) and (3) transferring the demagging mother liquor obtained in the step 3) into a beaker, adding 55ml of 98% sulfuric acid, performing calcium precipitation reaction, after the calcium precipitation reaction is finished, performing suction filtration to obtain gypsum whiskers and a phosphoric acid solution, wherein the phosphoric acid solution is used for demagging the phosphate concentrate in the next flotation.
Example 5
Referring to fig. 1, the method for processing silico-calcic collophanite by "floating-chemical" coupling of this embodiment specifically includes the following steps:
1) 500g of silico-calcium collophanite is taken and placed in a flotation machine, 860ml of water is added, and the mixture is fully and evenly stirred to prepare ore pulp;
2) adding 8.5kg/t of sodium carbonate, 5.0kg/t of sodium silicate and 3.8kg/t of sulfo fatty acid collecting agent into the ore pulp in sequence, stirring for 10min after the adding is finished, then ventilating and scraping for 15min, carrying out positive flotation, and then, drying a concentrate product and a tailing product to obtain flotation concentrate and high-silicon tailing;
3) placing the flotation concentrate obtained in the step 2) into a 1000ml three-neck flask, heating the flotation concentrate to 85 ℃ in an oil bath, slowly adding 55ml of 35% phosphoric acid for mixing, performing demagging reaction for 3.0h, and performing suction filtration to obtain phosphate concentrate and demagging mother liquor;
4) and (3) transferring the demagging mother liquor obtained in the step 3) into a beaker, adding 65ml of 98% sulfuric acid, performing calcium precipitation reaction, after the calcium precipitation reaction is finished, performing suction filtration to obtain gypsum whiskers and a phosphoric acid solution, wherein the phosphoric acid solution is used for demagging the phosphate concentrate in the next flotation.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for treating calcium silicon collophanite by 'floating-chemical' coupling is characterized by comprising the following steps:
1) placing the silicon-calcium collophanite in a flotation machine, adding water, and stirring to obtain ore pulp;
2) sequentially adding sodium carbonate, sodium silicate and a sulfofatty acid collecting agent into the ore pulp, and performing direct flotation to obtain flotation concentrate and high-silicon tailings;
3) mixing the flotation concentrate with phosphoric acid, performing a demagging reaction, and after the demagging reaction is finished, performing suction filtration to obtain a phosphate concentrate and a demagging mother liquor;
4) and adding a precipitator into the magnesium-removing mother liquor to perform calcium precipitation reaction, and obtaining gypsum whiskers and a phosphoric acid solution after the calcium precipitation reaction is finished.
2. The process of claim 1, wherein the concentration of the ore slurry in step 1) is 20-40%.
3. The method for the coupled treatment of silico-calcareous collophanite according to claim 1, characterized in that the addition amount of the sodium carbonate, the sodium silicate and the sulfofatty acid collector in the ore pulp of the step 2) is 2-10kg/t, 0.5-5kg/t and 0.4-3kg/t respectively.
4. The method for the coupled floating-chemical treatment of silicon-calcium collophanite according to claim 1, characterized in that the reaction time of the positive flotation in the step 2) is 3-10min, and the aeration froth-scraping time is 5-15 min.
5. The process for coupled floating-gasification silico-calcic collophanite according to claim 1, wherein the mass fraction of phosphoric acid in step 3) is 20-60%.
6. The method for coupled floating-chemical treatment of silicon-calcium collophanite according to claim 1, wherein the reaction temperature of the demagging reaction in the step 3) is 50-100 ℃ and the reaction time is 2-5 h.
7. The process of claim 1, wherein the precipitating agent in step 4) is sulfuric acid or ammonium sulfate.
8. The process of claim 1, wherein the amount of the precipitant added in the step 4) is 1-1.5 times of the amount of the calcium in the magnesium-removed mother liquor.
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