CN110918265A - Method for preparing high-quality phosphate concentrate - Google Patents
Method for preparing high-quality phosphate concentrate Download PDFInfo
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- CN110918265A CN110918265A CN201911254060.5A CN201911254060A CN110918265A CN 110918265 A CN110918265 A CN 110918265A CN 201911254060 A CN201911254060 A CN 201911254060A CN 110918265 A CN110918265 A CN 110918265A
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- flotation
- sesquioxide
- sio
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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
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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
- B03D1/004—Organic compounds
- B03D1/01—Organic compounds containing nitrogen
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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
Abstract
The invention relates to a method for preparing high-quality phosphate concentrate. Reverse flotation for SiO removal in the fine fraction mainly by means of the action of reverse flotation reagents2And sesquioxide, which is different from the currently widely used technology for removing SiO by coarse fraction reverse flotation after classification2And fine fraction direct tailing discarding. The invention overcomes the influence of slime in fine fraction on flotation, and realizes the efficient reverse flotation removal of SiO in micro-fine particles2And a sesquioxide. The phosphate concentrate prepared by the method can reduce the discharge amount of the phosphogypsum in the production process of wet-process phosphoric acid and improve the purity of calcium sulfate dihydrate in the phosphogypsum.
Description
Technical Field
The invention particularly relates to a high P2O5Low SiO content2A preparation method of phosphate concentrate with low sesquioxide content, belonging to the fields of phosphate ore dressing and phosphogypsum emission reduction.
Background
China has abundant phosphorite resource reserves, but most of the phosphorite resources can become qualified raw materials for downstream utilization only by mineral processing.
Because the direct flotation production cost is higher, most phosphate ores are processed by adopting a mineral separation mode of removing carbonate gangue by reverse flotation so as to be supplied to the downstream wet-process phosphoric acid production for use.
With the further depletion of phosphorite resources caused by the continuous development and utilization of phosphorite resources, phosphate concentrate obtained by only using a simple process for removing MgO in phosphorite through reverse flotation can not meet the requirements of ore for downstream wet-process phosphoric acid, and on one hand, P after MgO removal can not meet the requirements of ore for downstream wet-process phosphoric acid2O5The recovery rate is reduced, on the other hand, the content of sesquioxide cannot be effectively reduced in the process, the wet-process phosphoric acid production is influenced, meanwhile, a large amount of silicate enters the wet-process phosphoric acid processing process, the phosphoric acid production efficiency is low, the discharge amount of phosphogypsum is increased, and the content of calcium sulfate dihydrate in the phosphogypsum is reduced.
SiO from phosphate ore2And the embedded grain size characteristics of the sesquioxide, SiO2And the sesquioxide has fine embedded particle size in the phosphate ore, particularly, the content of the sesquioxide in the fine particle grade is higher than that in the coarse particle grade by a plurality of orders of magnitude, aiming at the characteristic, the currently adopted treatment method is to carry out graded desliming on the fine particle grade and directly throw the tail, the method can greatly reduce the recovery rate of the phosphate ore, the technical and economic indexes are extremely poor, and the sesquioxide cannot be adopted generally.
Disclosure of Invention
The invention aims to solve the problems by adopting a reverse flotation method to separate SiO2And sesquioxide are removed from their enriched fine fraction, thereby maximizing P assurance2O5The recovery rate of the calcium sulfate is improved, and the discharge amount of the phosphogypsum in the production process of the wet-process phosphoric acid can be reduced to a certain extent, so that the purity of the calcium sulfate dihydrate in the phosphogypsum is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method of producing a high quality phosphate concentrate comprising the steps of:
(1) crushing and grinding phosphate ore, wherein the particle size of minus 200 meshes is more than 90%, the monomer dissociation degree is more than 85%, and the grinding concentration is 40-50%;
(2) adding sulfuric acid, phosphoric acid and a reverse flotation MgO removal collecting agent into the ore pulp prepared in the step (1) to perform reverse flotation MgO removal operation to obtain a magnesium-removed rough phosphate concentrate, wherein the concentration of the ore pulp in the step is 20-30%, and the pH value of the ore pulp in the step is 3.5-5.9;
(3) grading the magnesium-removed rough phosphate concentrate prepared in the step (2), wherein the coarse fraction is used as 'concentrate 1', and the fine fraction is subjected to reverse flotation to remove SiO2And a sesquioxide;
(4) sequentially adding an inhibitor and reverse flotation SiO removal into the ore pulp with the finer fraction obtained in the step (3)2Removing SiO by reverse flotation with sesquioxide collecting agent2And sesquioxide, wherein the product in the tank is 'concentrate 2', the concentration of the flotation pulp in the step is 10-20%, and the pH value of the flotation pulp is 4.0-5.9;
(5) combining the concentrate 1 in the step (3) and the concentrate 2 in the flotation tank in the step (4) to obtain the high P2O5Low SiO content2And final phosphate concentrate of low sesquioxide.
The phosphate ore in the step (1) is collophanite, the mass percentage of MgO is 3-6%, and SiO is2The mass percentage of the sesquioxide is 12-26%, and the mass percentage of the sesquioxide is 2-4%.
In the step (2), the consumption of sulfuric acid, phosphoric acid and the reverse flotation MgO removal collecting agent is based on the dry basis weight of flotation ore pulp, the consumption of sulfuric acid is 8-16 kg/t, the consumption of phosphoric acid is 0.5-2 kg/t, and the consumption of the reverse flotation MgO removal collecting agent is 1-3 kg/t. The reagents can be prepared into 2-10% of mass concentration for use, wherein the reverse flotation MgO removal collecting agent is prepared by mixing sodium oleate, stearic acid and ether amine according to the mass ratio of 1:0.5: 0.1.
Classifying by using a fine particle classifying device in the step (3), wherein the fine particle classifying device comprises: a swirler, a high-frequency vibrating screen and a dense settling classification.
The coarse and fine particle classification in the step (3) is to divide the ore particle size into two relatively coarse and fine particle fractions, and classification operation is carried out according to actual ore particle size screening analysis data, wherein the classification limit comprises the particle fraction from +/-100 meshes to +/-800 meshes. Preferably, the coarser fraction is +450 mesh and the finer fraction is-450 mesh.
The inhibitor in the step (4) is fully water-soluble humic acid sodium salt or humic acid potassium salt, and the dosage of the inhibitor is 50-300 g/t based on the dry weight of the flotation pulp.
Step (4) reverse flotation SiO removal2And the sesquioxide collecting agent can remove SiO by reverse flotation under the acidic condition2And the efficient collecting agent of the sesquioxide is prepared by mixing dodecyl primary amine hydrochloride, polyether amine and tributyl phosphate according to the mass ratio of 1:0.2:0.1, and the using amount of the efficient collecting agent is 50-300 g/t on the basis of the dry weight of the flotation pulp.
Step (4) realizes the flotation of the ultrafine particles and the removed SiO2And sesquioxide ore particle size < 30 microns.
The ore grinding dissociation degree of the invention is more than 85%;
phosphoric acid and sulfuric acid are used as inhibitors of phosphorite for removing MgO by reverse flotation, and a fatty acid collecting agent is used as a collecting agent for removing MgO by reverse flotation, wherein the collecting agent is formed by mixing sodium oleate, stearic acid and ether amine according to the mass ratio of 1:0.5: 0.1;
the demagging rough phosphate concentrate is used as rough concentrate to carry out grading operation of relative coarse and fine particle grades;
the grading equipment of the invention is micro-fine particle grading equipment such as a swirler, a high-frequency vibrating screen, dense settling grading and the like;
the classification operation is carried out according to the actual ore particle size screening analysis data, and the classification limit comprises the particle size between +/-100 meshes and +/-800 meshes.
The invention uses humic acid sodium salt or humic acid potassium salt as inhibitor to reverse flotation SiO removal aiming at the relatively fine grain size after classification2And the sesquioxide collecting agent can remove SiO by reverse flotation under the acidic condition2And the efficient collecting agent of the sesquioxide is prepared by mixing dodecyl primary amine hydrochloride, polyether amine and tributyl phosphate according to the mass ratio of 1:0.2: 0.1.
The final concentrate of the invention is prepared by removing magnesium and crude phosphorusReverse flotation SiO removal of the coarse part and the fine part of the concentrate classification2And the product after the sesquioxide is combined.
The phosphate concentrate prepared by the method can improve the production efficiency of wet-process phosphoric acid, reduce the discharge amount of phosphogypsum in the production process of the wet-process phosphoric acid and improve the purity of calcium sulfate dihydrate in the phosphogypsum.
The invention has the following remarkable advantages:
(1) the final phosphate concentrate has a high P content compared to a reverse flotation demagging concentrate alone2O5Low SiO content2And low sesquioxide.
(2) The method has the characteristics of simple medicament system, no need of adjusting the pH value of ore pulp in reverse flotation MgO removal operation, no influence of slime, strong adaptability to different phosphate ores and the like.
(3) The method is also characterized by aiming at SiO2Sesquioxide is enriched in the micro-fine fraction, the dissociation degree in the micro-fine fraction is good, and the reverse flotation process is adopted to remove SiO specially aiming at the finer particles (micro-fine fraction) in the ore pulp2And sesquioxide, high removal efficiency, better selectivity than a method for directly discarding tailings by graded desliming, P2O5The recovery rate is higher.
(4) The invention belongs to the ultra-fine particle flotation technology, and relates to SiO removed by reverse flotation2And the granularity of the sesquioxide tailings is less than 30 mu m.
(5) The phosphate concentrate prepared by the method can reduce the discharge amount of the phosphogypsum in the production process of wet-process phosphoric acid and improve the purity of calcium sulfate dihydrate in the phosphogypsum.
(6) The magnesium removal collecting agent used in the method adopts sodium oleate, stearic acid and ether amine according to the mass ratio of 1:0.5:0.1, and the sodium oleate and the stearic acid are used as MgO collecting agents and can play a synergistic effect when being used in a matched manner. The ether amine being SiO2The collecting agent has good desiliconization selectivity but weak collecting capability, and a small amount of collecting agent is added in the magnesium removal stage, so that the magnesium removal is not influenced, but the collecting agent and SiO can be prolonged2The action time of (1).
(7) The method uses SiO removal2And sesquioxideThe collecting agent is prepared by mixing dodecyl primary amine hydrochloride, polyether amine and tributyl phosphate according to the mass ratio of 1:0.2:0.1, wherein the dodecyl primary amine hydrochloride is opposite to SiO2The collecting capability of the collector is strong, but the selectivity is slightly poor, and the SiO of the collector can be improved by adding the polyether amine2And selectivity to sesquioxide. The flotation of the two is rich in foam in the flotation process, and the yield of the flotation foam can be regulated and controlled by adding tributyl phosphate.
Drawings
FIG. 1 shows reverse flotation, MgO removal, classification, reverse flotation and SiO removal of phosphate ore2And a flow chart of the sesquioxide.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited to these examples.
The phosphate ore treated in the embodiment is a production ore for a certain large national phosphate ore dressing enterprise in China:
the phosphorus ore P2O5：20.15%，MgO：4.97%，SiO2: 16.13 percent and 3.06 percent of sesquioxide. The ore is ground to-200 meshes which are more than 92%, the monomer dissociation degree is more than 85%, the flotation concentration of the ore pulp is adjusted to 25%, 10 kg/t of sulfuric acid, 1 kg/t of phosphoric acid, 4.5 of pH value and 2.6 kg/t of a magnesium removal collecting agent are added based on the dry basis weight of the flotation ore pulp for reverse flotation to remove MgO, and the magnesium removal collecting agent is prepared by mixing sodium oleate, stearic acid and ether amine according to the mass ratio of 1:0.5: 0.1.
The index of the magnesium-removed rough phosphate concentrate obtained after MgO removal reverse flotation is P2O5：27.45%，MgO：1.17%，SiO2: 19.23 percent of sesquioxide, 2.78 percent of sesquioxide; the demagging raw phosphate concentrate was subjected to particle size sieve analysis and the results are shown in the following table:
from the above table, SiO is seen2And sesquioxide in-450 mesh fraction, especially higher sesquioxide concentration, and the fraction yield is up to 42.62 percent, and P2O5Content 27.88%。
Reverse flotation SiO removal is carried out on the minus 450-mesh fraction2And sesquioxide, wherein the concentration of flotation pulp is 15%, the pH value of the flotation pulp is 4.5, 100g/t of humic acid sodium salt and 200g/t of desiliconization collecting agent are added on the basis of the dry basis weight of the flotation pulp, the collecting agent is prepared by mixing dodecyl primary amine hydrochloride, polyether amine and tributyl phosphate according to the mass ratio of 1:0.2:0.1, and the product indexes shown in the following table are obtained:
the final concentrate index of the-450 mesh reverse flotation concentrate combined with the demagging phosphate concentrate +450 mesh is shown in the following table:
the combined final concentrate is subjected to MgO removal process by pure reverse flotation2O5Improved by 1.64 percentage points, SiO2The reduction is 5.04 percentage points, and the reduction of the sesquioxide is 1.14 percentage points. The combined final concentrate product meets the index requirement of 'first-class product' in the 'phosphate ore for acid processing' (HG/T2673-one 1995) standard, and compared with the phosphate concentrate index of a pure reverse flotation MgO removal process, the phosphate concentrate index is greatly improved, and SiO2And the content of sesquioxide is obviously reduced, the product is used for processing phosphoric acid by a wet method, the production efficiency of the phosphoric acid is greatly improved, the purity of calcium sulfate dihydrate of the byproduct phosphogypsum is higher, and the reduction and discharge of the phosphogypsum can be realized.
The following table shows the analysis of the components of the by-product phosphogypsum produced by preparing phosphoric acid from the magnesium-removed rough phosphate concentrate by a wet method after the MgO reverse flotation:
the following table shows further SiO removal of the magnesium-removed rough phosphate concentrate obtained after reverse flotation of MgO2And the component analysis of the phosphorus concentrate product after sesquioxide for preparing phosphoric acid by a wet method and the byproduct phosphogypsum is as follows:
as can be seen from the above table, further SiO removal was performed2The phosphorus concentrate after being mixed with sesquioxide reaches the secondary product pair CaSO in the standard of phosphogypsum GB/T23456-201842(H2O) content of more than 80%.
The chemical reaction principle of wet-process phosphoric acid production is as follows:
the general chemical reaction equation for wet process phosphoric acid production is as follows:
wherein the HF produced is mixed with SiO entrained in the phosphate rock2The following reactions occur:
small part of SiO in phosphorus ore2Will be consumed in this step but will remain mostly in the phosphogypsum, reducing the CaSO in the phosphogypsum42(H2O) purity.
In addition, iron and aluminum (sesquioxide) in the phosphorite react as follows:
as can be seen from the above reaction formula, the sesquioxide in the phosphorite consumes the phosphoric acid, the generated precipitate can greatly reduce the phosphoric acid concentration efficiency, and the amount of the slag phosphoric acid generated by concentration can be greatly increased.
The phosphate concentrate produced by the technology of the invention ensures higher P2O5The recovery rate is improved, and simultaneously the SiO is greatly reduced2And sesquioxide impurity content, the concentration efficiency of phosphoric acid production can be improved by more than 10 percent, the amount of the phosphoric acid residue generated by concentration is less than 90 percent of that of the MgO-removed reverse flotation phosphate concentrate, and high-quality phosphate concentrate can be obtainedPhosphoric acid product.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (10)
1. A method for producing high quality phosphate concentrate, comprising the steps of:
(1) crushing and grinding phosphate ore, wherein the particle size of minus 200 meshes is more than 90%, the monomer dissociation degree is more than 85%, and the grinding concentration is 40-50%;
(2) adding sulfuric acid, phosphoric acid and a reverse flotation MgO removal collecting agent into the ore pulp prepared in the step (1) to perform reverse flotation MgO removal operation to obtain a magnesium-removed rough phosphate concentrate, wherein the concentration of the ore pulp in the step is 20-30%, and the pH value of the ore pulp in the step is 3.5-5.9;
(3) grading the magnesium-removed rough phosphate concentrate prepared in the step (2), wherein the coarse fraction is used as 'concentrate 1', and the fine fraction is subjected to reverse flotation to remove SiO2And a sesquioxide;
(4) sequentially adding an inhibitor and reverse flotation SiO removal into the ore pulp with the finer fraction obtained in the step (3)2Removing SiO by reverse flotation with sesquioxide collecting agent2And sesquioxide, wherein the product in the tank is 'concentrate 2', the concentration of the flotation pulp in the step is 10-20%, and the pH value of the flotation pulp is 4.0-5.9;
(5) combining the concentrate 1 in the step (3) and the concentrate 2 in the flotation tank in the step (4) to obtain the high P2O5Low SiO content2And final phosphate concentrate of low sesquioxide.
2. The method according to claim 1, wherein the phosphate ore in step (1) is collophanite, the MgO content is 3-6% by mass, and SiO content is2The mass percentage of the sesquioxide is 12-26%, and the mass percentage of the sesquioxide is 2-4%.
3. The method according to claim 1, wherein the sulfuric acid, the phosphoric acid and the reverse flotation MgO removal collecting agent are used in the step (2) based on the dry basis weight of the flotation pulp, the sulfuric acid is used in an amount of 8 to 16 kg/t, the phosphoric acid is used in an amount of 0.5 to 2 kg/t, and the reverse flotation MgO removal collecting agent is used in an amount of 1 to 3 kg/t.
4. The method according to claim 3, wherein the reverse flotation de-MgO collecting agent is prepared by mixing sodium oleate, stearic acid and ether amine according to the mass ratio of 1:0.5: 0.1.
5. The method of claim 1, wherein said classifying of step (3) is performed using a fine particle classifying apparatus, said fine particle classifying apparatus comprising: a swirler, a high-frequency vibrating screen and a dense settling classification.
6. The method according to claim 1, wherein the coarse-fine classification in step (3) is to divide the ore size into two relatively coarse fractions, and the classification operation is performed according to the actual ore size screening analysis data, and the classification limit comprises the fraction from ± 100 meshes to ± 800 meshes.
7. The method of claim 6, wherein the coarser fraction is +450 mesh and the finer fraction is-450 mesh.
8. The method according to claim 1, wherein the inhibitor in the step (4) is a fully water-soluble humic acid sodium salt or humic acid potassium salt, and the dosage is 50-300 g/t based on the dry weight of the flotation pulp.
9. The method of claim 1, wherein step (4) reverse flotation SiO removal2And the sesquioxide collecting agent can remove SiO by reverse flotation under the acidic condition2And the efficient collecting agent of the sesquioxide is prepared by mixing dodecyl primary amine hydrochloride, polyether amine and tributyl phosphate according to the mass ratio of 1:0.2:0.1, and the using amount of the efficient collecting agent is 50-300 g/t on the basis of the dry weight of the flotation pulp.
10. The method as claimed in claim 1, wherein step (4) achieves ultra-fine flotation, with SiO removed2And sesquioxide ore particle size < 30 microns.
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Cited By (3)
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| CN111617885A (en) * | 2020-05-18 | 2020-09-04 | 宜都兴发化工有限公司 | Synchronous reverse flotation process for low-magnesium high-sesqui collophanite |
| CN113600344A (en) * | 2021-07-21 | 2021-11-05 | 宜都兴发化工有限公司 | Ore dressing process for removing sesquioxide from collophanite by intermediate grading and retreatment |
| CN113976325A (en) * | 2021-10-27 | 2022-01-28 | 山东理工大学 | Desiliconization reagent and double-reverse flotation method for separating collophanite and quartz |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111617885A (en) * | 2020-05-18 | 2020-09-04 | 宜都兴发化工有限公司 | Synchronous reverse flotation process for low-magnesium high-sesqui collophanite |
| CN113600344A (en) * | 2021-07-21 | 2021-11-05 | 宜都兴发化工有限公司 | Ore dressing process for removing sesquioxide from collophanite by intermediate grading and retreatment |
| CN113976325A (en) * | 2021-10-27 | 2022-01-28 | 山东理工大学 | Desiliconization reagent and double-reverse flotation method for separating collophanite and quartz |
| CN113976325B (en) * | 2021-10-27 | 2024-03-12 | 山东理工大学 | Desilication agent and double reverse flotation method for separating collophanite and quartz |
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