CN112919671A - Treatment process and treatment system for barite ore powder purification and whitening wastewater - Google Patents

Treatment process and treatment system for barite ore powder purification and whitening wastewater Download PDF

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Publication number
CN112919671A
CN112919671A CN202110091903.5A CN202110091903A CN112919671A CN 112919671 A CN112919671 A CN 112919671A CN 202110091903 A CN202110091903 A CN 202110091903A CN 112919671 A CN112919671 A CN 112919671A
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waste liquid
tank
extraction
wastewater
whitening
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张纪锋
熊辉堂
刘正钧
覃玮
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Hunan Huazhong Mining Co ltd
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Hunan Huazhong Mining Co ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/20Halides
    • C01F11/24Chlorides
    • C01F11/28Chlorides by chlorination of alkaline-earth metal compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/20Halides
    • C01F11/24Chlorides
    • C01F11/30Concentrating; Dehydrating; Preventing the adsorption of moisture or caking
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/20Halides
    • C01F11/24Chlorides
    • C01F11/32Purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/46Sulfates
    • C01F11/462Sulfates of Sr or Ba
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/22Treatment of water, waste water, or sewage by freezing
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/44Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/441Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F2001/5218Crystallization
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/12Halogens or halogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00General aspects of water treatment
    • C02F2301/08Multistage treatments, e.g. repetition of the same process step under different conditions

Abstract

The application relates to the technical field of barite ore powder processing, and particularly discloses a barite ore powder purification and whitening wastewater treatment process and system, wherein the wastewater comprises extraction waste liquid, and the extraction waste liquid is obtained after dehydration; the wastewater treatment process comprises the following steps: removing magnesium and iron ions: adding calcium hydroxide into the wastewater, enabling the pH value of the wastewater to be 8.5-9.5, stirring and uniformly mixing, carrying out reaction treatment for 2-3h, and then standing for 0.5-1.5h to obtain a precipitate and a supernatant; calcium chloride crystallization: cooling the supernatant to 5-10 deg.C, standing, and keeping the temperature for 4-6 hr to obtain crystal and mother liquor; recovering calcium chloride hexahydrate: drying the crystal to obtain calcium chloride hexahydrate. The wastewater treatment process not only realizes the treatment of wastewater, but also reduces the wastewater treatment cost, and simultaneously obtains a byproduct of calcium chloride hexahydrate, thereby improving the practicability and stability of the wastewater treatment process.

Description

Treatment process and treatment system for barite ore powder purification and whitening wastewater
Technical Field
The application relates to the technical field of barite ore powder processing, in particular to a barite ore powder purification and whitening wastewater treatment process and system.
Background
The barite is a non-metallic mineral product with barium sulfate as a main component, pure barite is white and glossy, and can be gray, light red, light yellow and the like under the condition of mixing some impurities, and the barite mineral powder is often purified and whitened in order to improve the content and whiteness of barium sulfate in the barite mineral powder.
In the related technology, the method for purifying barite mainly comprises a physical purification method and a chemical purification method, wherein the chemical purification method mainly comprises flotation, calcination and leaching, hydrochloric acid is generally adopted as an acid leaching agent, an impregnation solution is prepared, and then the impregnation solution reacts with barite ore powder to generate impregnation wastewater. The impregnation wastewater is often subjected to an evaporation process, which invisibly increases the treatment cost and indirectly increases the purification and whitening processing cost of the barite ore powder. Therefore, there is an urgent need to develop a low-cost wastewater treatment process and reduce the environmental pollution.
Disclosure of Invention
In order to reduce the wastewater treatment cost and reduce the pollution to the environment, the application provides a treatment process and a treatment system for barite ore powder purification and whitening wastewater.
In a first aspect, the application provides a treatment process for barite ore powder purification and whitening wastewater, which adopts the following technical scheme:
a purification and whitening wastewater treatment process for barite ore powder is used for treating wastewater generated in the purification and whitening process for barite ore powder, and comprises the following steps: extracting, growing crystal, dehydrating, cleaning, dehydrating and drying the barite ore powder to obtain a product;
in the extraction step, extracting the barite mineral powder by using an extraction liquid, wherein raw materials of the extraction liquid comprise 24-26% of hydrochloric acid, 5-10% of a lattice modifier and barium chloride;
the waste water comprises extraction waste liquid, and the extraction waste liquid is obtained after dehydration;
the wastewater treatment process comprises the following steps:
removal of magnesium and iron ions
Adding calcium hydroxide into the wastewater, enabling the pH value of the wastewater to be 8.5-9.5, stirring and uniformly mixing, carrying out reaction treatment for 2-3h, and then standing for 0.5-1.5h to obtain a precipitate and a supernatant;
calcium chloride crystal
Cooling the supernatant to 5-10 deg.C, standing, and keeping the temperature for 4-6 hr to obtain crystal and mother liquor;
recovery of calcium chloride hexahydrate
Drying the crystal to obtain calcium chloride hexahydrate.
By adopting the technical scheme, the applicant finds that the barite ore powder contains a large amount of barium sulfate and BaCO3、CaCO3、CaSO4、MgCO3、Fe2O3And the like, and seriously affect the quality of the product.
In the application, the content of barium sulfate in the product is more than 95 percent, the whiteness is more than 95 percent, and the market demand is met through the synergistic action between the hydrochloric acid and the crystal lattice modifier, the synergistic action between the extraction and the crystal growing, and the synergistic action among the steps. The applicant has also found that the extraction effluent produced contains a significant amount of Cl-、Fe3+、Mg2+、Ca2+Ions.
In the application, calcium hydroxide is added into the extraction waste liquid, and the calcium hydroxide reacts with ions in the extraction waste liquid to obtain a precipitate and a supernatant, wherein the precipitate mainly comprises magnesium hydroxide and ferric hydroxide, and the supernatant mainly comprises calcium chloride. Because the solubility of calcium chloride at different temperatures is changed greatly, the temperature of the supernatant is controlled to reduce the temperature of the supernatant to 5-10 ℃, calcium chloride in the supernatant is almost completely crystallized to obtain a crystal and mother liquor, and then the crystal is dried to obtain a calcium chloride hexahydrate by-product.
Optionally, the mother liquor flows back to the extraction step and is recycled.
By adopting the technical scheme, the mother liquor is recycled, the environmental pollution is reduced, and the purification and whitening processing cost of the barite ore powder is also reduced.
Optionally, in the step of removing magnesium and iron ions, the added calcium hydroxide is a saturated calcium hydroxide solution.
By adopting the technical scheme, the calcium hydroxide solution and the extraction waste liquid are mixed and react, so that the mixing and reaction of the calcium hydroxide and the extraction waste liquid can be accelerated, and the time cost of wastewater treatment and operation is reduced.
Optionally, in the step of recovering the calcium chloride hexahydrate, the drying temperature is 65-85 ℃, and the drying time is 2-3 h.
By adopting the technical scheme, the drying temperature of the crystal is limited, the phenomenon that the drying temperature is too high and the calcium chloride hexahydrate is converted into anhydrous calcium chloride is avoided, the phenomenon that the drying temperature is too low and the drying time is prolonged is also avoided, and the time cost of wastewater treatment operation is increased.
Optionally, the waste water further comprises a cleaning waste liquid, and the cleaning waste liquid is obtained after cleaning and dewatering.
By adopting the technical scheme, the treatment of the cleaning waste liquid is realized, and the influence of the waste water on the environment in the purification and whitening waste water processing of the barite ore powder is further reduced.
Optionally, the cleaning waste liquid is concentrated to obtain concentrated waste liquid and clear water, and the concentrated waste liquid and the extraction waste liquid are mixed for wastewater treatment.
By adopting the technical scheme, the cleaning waste liquid is concentrated, the treatment capacity of the waste liquid is reduced, the cost of the wastewater treatment process is also reduced, and the treatment effect of the wastewater treatment process is improved.
Optionally, the cleaning waste liquid is concentrated by reverse osmosis.
Through adopting above-mentioned technical scheme, compare and adopt evaporation concentration, reverse osmosis concentration can effectual reduce cost, but also has the advantage of concentration simple and convenient, stable, safety.
Optionally, the total ion concentration in the clean water is less than or equal to 5%.
By adopting the technical scheme, the total ion concentration in the clear water is limited, and the influence on the discharge or use of the clear water due to the overhigh total ion concentration in the clear water is avoided.
Optionally, the clean water flows back to the cleaning and dewatering step and is recycled.
By adopting the technical scheme, the clean water is recycled, the environmental pollution is reduced, and the purification and whitening processing cost of the barite ore powder is also reduced.
In a second aspect, the present application provides a barite fine wastewater treatment system, which adopts the following technical scheme:
a barite ore powder wastewater treatment system comprises an extraction waste liquid collecting tank, a calcium hydroxide adding tank, a sedimentation tank, a freezing device, a crystallizing tank and a dehydration drying device;
the extraction waste liquid collecting tank is communicated with the sedimentation tank through a communicating pipe, and the extraction waste liquid is discharged into the sedimentation tank;
the calcium hydroxide feeding tank is communicated with the sedimentation tank through a communicating pipe, calcium hydroxide is discharged into the sedimentation tank, and the calcium hydroxide and the extraction waste liquid react in the sedimentation tank to obtain precipitate and supernatant;
the sedimentation tank is communicated with the crystallization tank through a communicating pipe, and supernatant is discharged into the crystallization tank;
the freezing equipment is communicated with the crystallization tank through a communicating pipe, and the supernatant in the crystallization tank is cooled to obtain a crystal and a mother solution;
the crystallization tank is communicated with the dehydration drying equipment through a communicating pipe, and the crystallized substances are discharged into the dehydration drying equipment and dehydrated and dried to obtain calcium chloride hexahydrate and mother liquor.
By adopting the technical scheme, the wastewater treatment system has the advantages of simplicity, convenience and stability, and when the crystallisate enters the dehydration drying equipment from the crystallization tank, part of water can be carried, so that the crystallisate is convenient to move, and the crystallisate is further dehydrated in the dehydration drying equipment and then dried, thereby improving the stability of the wastewater treatment system.
In summary, the present application has the following beneficial effects:
1. in the purification and whitening process, the barium sulfate content in the product is higher than 95 percent, the whiteness is higher than 95 percent, and the market demand is met through the synergistic effect between the hydrochloric acid and the crystal lattice modifier, the synergistic effect between the extraction and the crystal growing and the synergistic effect between the steps. In the waste water treatment process, calcium hydroxide is added to form chemical precipitation, and then calcium chloride is crystallized by utilizing temperature difference, so that the waste water treatment is realized, the pollution to the environment is reduced, the waste water treatment cost is reduced, and a calcium chloride hexahydrate byproduct is obtained.
2. Besides the extraction waste liquid, the waste water treatment method also comprises the cleaning waste liquid, and the cleaning waste liquid is subjected to concentration treatment, so that the treatment of the cleaning waste liquid is realized, the influence of a large amount of increase of the treatment capacity of the waste water due to the cleaning waste liquid is reduced, and the practicability of the waste water treatment process is improved.
3. The utility model provides a barite powdered ore effluent disposal system when the crystallization gets into dehydration drying equipment from the crystallizer, can carry part water, the removal of the crystallization of being convenient for, the further dehydration of crystallization in dehydration drying equipment, then the drying makes effluent disposal system have and uses simple and convenient, stable advantage.
Drawings
Fig. 1 is a schematic diagram of an application example of the present application.
Description of reference numerals: 11. adding barite ore powder into a tank; 12. an extract liquid feeding tank; 13. an extraction stirring pool; 14. a crystal growing and stirring tank; 15. a centrifugal dewatering device; 16. a water addition tank; 17. cleaning a dehydration stirring pool; 18. a dewatering and drying device; 2. a communicating pipe; 3. a control valve; 41. a feeding pump a; 42. a feeding pump b; 43. a feeding pump c; 44. a feeding pump d; 45. a feeding pump e; 51. a discharge pipe a; 52. a discharge pipe b; 53. a discharge pipe c; 54. a discharge pipe d; 61. an extraction waste liquid collecting tank; 62. a calcium hydroxide adding tank; 63. a sedimentation tank; 64. a refrigeration device; 65. a crystallization tank; 66. a dehydration drying device; 67. a cleaning waste liquid collecting tank; 68. reverse osmosis equipment; 71. a charging pump a; 72. a feeding pump b; 73. a feed pump c; 74. a charging pump d; 75. a charge pump e; 76. a feed pump f; 77. a feeding pump g; 81. a blanking pipe a; 82. a discharging pipe b; 83. and a discharge pipe c.
Detailed Description
The present application will be described in further detail with reference to examples.
Examples
Example 1
A process for treating the sewage generated by purifying and whitening the barite ore powder features that the barite ore powder is treated by the sewage treating process.
The purification and whitening process comprises the following steps:
s1 preparation of raw materials
Preparing barite ore powder and water for later use.
Wherein the granularity of the barite ore powder is 200 meshes, the weight content of barium sulfate in the barite ore powder is 60%, and the whiteness is 50.
Preparing an extract for later use.
Wherein, the raw materials of the extraction liquid comprise water and an extractant, the water is a solvent, the extractant is a solute, and the raw materials of the extractant comprise 26 percent of hydrochloric acid and 10 percent of lattice modifier according to weight concentration.
And the extract is prepared by the following method: adding water into a hydrochloric acid solution with the concentration of 30%, uniformly stirring, then adding a barium chloride lattice modifier, continuously stirring and uniformly mixing to obtain an extract.
S2, extraction
Adding barite ore powder into the extract liquor under the condition of stirring speed of 200r/min, wherein the weight ratio of the extract liquor to the barite ore powder is 1.5:1, continuing stirring, and extracting for 8 hours to obtain an extraction mixed liquor.
S3, growing crystal
And under the condition that the stirring speed is 60r/min, carrying out crystal growth on the extraction mixed solution for 2.5 hours to obtain slag slurry.
S4, dewatering
And (4) carrying out centrifugal separation on solid matters and liquid matters in the slag slurry to obtain a semi-finished product and extraction waste liquid.
S5, cleaning
Adding the semi-finished product into water for cleaning at a stirring speed of 60r/min for 1.5h for three times, and removing the residual extract on the surface of the semi-finished product to obtain a cleaning waste liquid and a primary finished product.
S6, drying
And drying the primary finished product at the temperature of 150 ℃ for 3h to obtain the product.
And the barium sulfate content in the product is 97.3%, the whiteness is 97.5, and chlorides are not detected.
The wastewater treatment process comprises the following steps:
SS1, removal of magnesium and iron ions
Collecting the extraction waste liquid obtained after dehydration, adding calcium hydroxide, wherein the calcium hydroxide is a pre-prepared saturated calcium hydroxide solution, adjusting the pH value of the extraction waste liquid to 9.5, stirring and mixing uniformly, carrying out reaction treatment for 2h, and then standing for 1.5h to obtain a precipitate and a supernatant.
And the precipitate is mainly magnesium hydroxide and ferric hydroxide and is discharged.
SS2 calcium chloride crystal
And cooling the supernatant to 5 ℃, standing and preserving heat for 4 hours to obtain a crystal and a mother solution.
And the mother liquor flows back to the extraction step, and the recycling of the mother liquor is realized.
SS3 recovery of calcium chloride hexahydrate
And drying the crystal at 65 ℃ for 3 h.
SS4, cleaning waste liquid treatment
Collecting the cleaning waste liquid obtained after cleaning and dewatering, and concentrating by utilizing reverse osmosis to obtain concentrated waste liquid and clear water, wherein the concentration of total ions in the clear water is less than or equal to 5%.
And the clean water flows back to the step of cleaning and dewatering, and the water is recycled. And mixing the concentrated waste liquid and the extraction waste liquid, and then carrying out waste water treatment.
Example 2
A process for treating the sewage generated by purifying and whitening the barite ore powder features that the barite ore powder is treated by the sewage treating process.
The purification and whitening process comprises the following steps:
s1 preparation of raw materials
Preparing barite ore powder and water for later use.
Wherein, the granularity of the barite ore powder is 400 meshes, the weight content of barium sulfate in the barite ore powder is 68 percent, and the whiteness is 57.
Preparing an extract for later use.
Wherein, the raw materials of the extraction liquid comprise water and an extractant, the water is a solvent, the extractant is a solute, and the raw materials of the extractant comprise 25% of hydrochloric acid and 8% of a crystal lattice modifier according to weight concentration.
And the extract is prepared by the following method: adding water into a hydrochloric acid solution with the concentration of 28%, uniformly stirring, then adding a barium chloride lattice modifier, continuously stirring and uniformly mixing to obtain an extract.
S2, extraction
Adding barite ore powder into the extract liquor under the condition of stirring speed of 250r/min, wherein the weight ratio of the extract liquor to the barite ore powder is 1.4:1, continuing stirring, and extracting for 9 hours to obtain an extraction mixed liquor.
S3, growing crystal
And under the condition that the stirring speed is 75r/min, carrying out crystal growth on the extraction mixed solution for 2 hours to obtain slag slurry.
S4, dewatering
And (4) carrying out centrifugal separation on solid matters and liquid matters in the slag slurry to obtain a semi-finished product and extraction waste liquid.
S5, cleaning and dehydrating
Adding the semi-finished product into water for cleaning for 1h at a stirring speed of 75r/min for three times, removing residual extraction liquid on the surface of the semi-finished product, and cleaning waste liquid and the primary finished product.
S6, drying
And drying the primary finished product at 165 ℃ for 2.5 hours to obtain the product.
And the barium sulfate content in the product is 98.4%, the whiteness is 97.0, and chloride is not detected.
The wastewater treatment process comprises the following steps:
SS1, removal of magnesium and iron ions
Collecting the extraction waste liquid obtained after dehydration, adding calcium hydroxide, wherein the calcium hydroxide is a pre-prepared saturated calcium hydroxide solution, the pH value of the extraction waste liquid is 9, stirring and mixing uniformly, carrying out reaction treatment for 2.5h, and then standing for 1h to obtain a precipitate and a supernatant.
And the precipitate is mainly magnesium hydroxide and ferric hydroxide and is discharged.
SS2 calcium chloride crystal
And cooling the supernatant to 8 ℃, standing and preserving heat for 5 hours to obtain a crystal and a mother solution.
And the mother liquor flows back to the extraction step, and the recycling of the mother liquor is realized.
SS3 recovery of calcium chloride hexahydrate
The crystals were dried at 75 ℃ for 2.5 h.
SS4, cleaning waste liquid treatment
Collecting the cleaning waste liquid obtained after cleaning and dewatering, and concentrating by utilizing reverse osmosis to obtain concentrated waste liquid and clear water, wherein the concentration of total ions in the clear water is less than or equal to 5%.
And the clean water flows back to the step of cleaning and dewatering, and the water is recycled. And mixing the concentrated waste liquid and the extraction waste liquid, and then carrying out waste water treatment.
Example 3
A process for treating the sewage generated by purifying and whitening the barite ore powder features that the barite ore powder is treated by the sewage treating process.
The purification and whitening process comprises the following steps:
s1 preparation of raw materials
Preparing barite ore powder and water for later use.
Wherein, the granularity of the barite ore powder is 800 meshes, the weight content of barium sulfate in the barite ore powder is 70 percent, and the whiteness is 60.
Preparing an extract for later use.
Wherein, the raw materials of the extraction liquid comprise water and an extractant, the water is a solvent, the extractant is a solute, and the raw materials of the extractant comprise 24 percent of hydrochloric acid and 5 percent of lattice modifier according to weight concentration.
And the extract is prepared by the following method: adding water into 25% hydrochloric acid solution, stirring, adding barium chloride lattice modifier, stirring, and mixing to obtain extractive solution.
S2, extraction
Adding barite ore powder into the extract liquor under the condition of stirring speed of 300r/min, wherein the weight ratio of the extract liquor to the barite ore powder is 1.2:1, continuing stirring, and extracting for 10 hours to obtain an extraction mixed liquor.
S3, growing crystal
And under the condition that the stirring speed is 90r/min, carrying out crystal growth on the extraction mixed solution for 1.5h to obtain slag slurry.
S4, dewatering
And (4) carrying out centrifugal separation on solid matters and liquid matters in the slag slurry to obtain a semi-finished product and extraction waste liquid.
S5, cleaning and dehydrating
Adding the semi-finished product into water for cleaning at a stirring speed of 90r/min for 0.5h, removing the residual extraction liquid on the surface of the semi-finished product, and cleaning the waste liquid and the semi-finished product.
S6, drying
And drying the primary finished product at the temperature of 180 ℃ for 2h to obtain the product.
And the barium sulfate content in the product is 96.5%, the whiteness is 96.5, and chlorides are not detected.
The wastewater treatment process comprises the following steps:
SS1, removal of magnesium and iron ions
Collecting the extraction waste liquid obtained after dehydration, adding calcium hydroxide, wherein the calcium hydroxide is a pre-prepared saturated calcium hydroxide solution, adjusting the pH value of the extraction waste liquid to 8.5, stirring and mixing uniformly, reacting for 3h, and standing for 0.5h to obtain a precipitate and a supernatant.
And the precipitate is mainly magnesium hydroxide and ferric hydroxide and is discharged.
SS2 calcium chloride crystal
And cooling the supernatant to 10 ℃, standing and preserving heat for 6 to obtain a crystal and a mother solution.
And the mother liquor flows back to the extraction step, and the recycling of the mother liquor is realized.
SS3 recovery of calcium chloride hexahydrate
And drying the crystal at 85 ℃ for 2 h.
SS4, cleaning waste liquid treatment
Collecting the cleaning waste liquid obtained after cleaning and dewatering, and concentrating by utilizing reverse osmosis to obtain concentrated waste liquid and clear water, wherein the concentration of total ions in the clear water is less than or equal to 5%.
And the clean water flows back to the step of cleaning and dewatering, and the water is recycled. And mixing the concentrated waste liquid and the extraction waste liquid, and then carrying out waste water treatment.
Application example
A barite ore powder purification and whitening wastewater treatment system is used for treating wastewater generated in the barite ore powder purification and whitening processing treatment system.
Referring to fig. 1, the purification and whitening processing system comprises a barite ore powder feeding tank 11, an extract liquid feeding tank 12, an extraction stirring tank 13, a crystal growing stirring tank 14, a centrifugal dehydration device 15, a water feeding tank 16, a cleaning and dehydration stirring tank 17 and a dehydration and drying device 18. Adding the barite ore powder into a barite ore powder adding tank 11 for later use; preparing an extract liquid in an extract liquid adding tank 12 for later use; water is added to a water addition tank 16 for use.
Referring to fig. 1, an extract adding tank 12 is communicated with an extraction stirring tank 13 through a communicating pipe 2, and a feeding pump a41 and a control valve 3 are arranged on the communicating pipe 2. The extract liquid feeding tank 12 feeds the extract liquid into the extraction stirring tank 13 through the communicating pipe 2, the feeding pump a41 and the control valve 3.
Referring to fig. 1, the barite ore powder adding tank 11 is located above the extraction stirring tank 13, the barite ore powder adding tank 11 and the extraction stirring tank 13 are also communicated through a communicating pipe 2, and the communicating pipe 2 is also provided with a control valve 3. The barite ore powder feeding tank 11 feeds the barite ore powder into the extraction stirring tank 13 through the communicating pipe 2 and the control valve 3, and the barite ore powder and the extraction liquid are mixed in the extraction stirring tank 13 and extracted to obtain an extraction mixed liquid.
Referring to fig. 1, the extraction stirring tank 13 and the crystal growing stirring tank 14 are also communicated through a communicating pipe 2, a feeding pump b42 is arranged on the communicating pipe 2, and a control valve 3 is also arranged on the communicating pipe 2. The extraction stirring tank 13 adds the extraction mixed liquid into the crystal growing stirring tank 14 through the communicating pipe 2, the feeding pump b42 and the control valve 3, and carries out crystal growing to obtain slag slurry.
Referring to fig. 1, the crystal growing stirring tank 14 and the centrifugal dewatering device 15 are also communicated through a communicating pipe 2, a feeding pump c43 is arranged on the communicating pipe 2, and a control valve 3 is also arranged on the communicating pipe 2. The crystal growing stirring pool 14 adds the slag slurry into a centrifugal dehydration device 15 through a communicating pipe 2, a feeding pump c43 and a control valve 3, and dehydrates the slag slurry to form extraction waste liquid and semi-finished products, wherein the centrifugal dehydration device 15 is provided with a discharge pipe a51, the discharge pipe a51 is also provided with the control valve 3, and the extraction waste liquid is discharged from a discharge pipe a 51.
Referring to fig. 1, the water adding tank 16 is located above the washing and dewatering agitation tank 17, the water adding tank 16 and the washing and dewatering agitation tank 17 are also communicated through a communicating pipe 2, and the communicating pipe 2 is also provided with a control valve 3. The water adding tank 16 adds water into the washing and dewatering stirring pool 17 through the communicating pipe 2 and the control valve 3.
Referring to fig. 1, the centrifugal dewatering device 15 and the washing, dewatering and stirring tank 17 are also communicated through a communicating pipe 2, a feeding pump d44 is arranged on the communicating pipe 2, and a control valve 3 is also arranged on the communicating pipe 2. The crystal growing stirring tank 14 adds the semi-finished product into a centrifugal dehydration device 15 through a communicating pipe 2, a feeding pump d44 and a control valve 3, the semi-finished product is mixed with water and cleaned to form cleaning waste liquid and a primary finished product. The washing and dewatering agitation tank 17 is provided with a discharge pipe b52, a control valve 3 is also provided on a discharge pipe b52, and washing waste liquid is discharged from a discharge pipe b 52.
Referring to fig. 1, the washing, dewatering and stirring tank 17 and the dewatering and drying device 18 are also communicated through a communicating pipe 2, a feeding pump e45 is arranged on the communicating pipe 2, and a control valve 3 is also arranged on the communicating pipe 2. The cleaning and dewatering stirring pool 17 adds the primary product into the dewatering and drying equipment 18 through the communicating pipe 2, the feeding pump e45 and the control valve 3, meanwhile, the primary product carries part of water when entering the dewatering and drying equipment 18, and is further dewatered in the dewatering and drying equipment 18 and then dried, so that cleaning waste liquid and products are obtained. The dewatering and drying equipment 18 is provided with a discharge pipe c53, a control valve 3 is also arranged on a discharge pipe c53, and the cleaning waste liquid is discharged from a discharge pipe c 53. The dewatering and drying equipment 18 is provided with a discharge pipe d54, a control valve 3 is also arranged on a discharge pipe d54, and products are discharged from a discharge pipe d 54.
Referring to fig. 1, the wastewater treatment system comprises an extraction waste liquid collecting tank 61, a calcium hydroxide adding tank 62, a sedimentation tank 63, a freezing device 64, a crystallizing tank 65, a dehydration drying device 66, a cleaning waste liquid collecting tank 67 and a reverse osmosis device 68. The calcium hydroxide is prepared into a saturated calcium hydroxide solution and added into a calcium hydroxide adding tank 62 for later use.
Referring to fig. 1, the centrifugal dewatering device 15 is located above the extraction waste liquid collecting tank 61, the centrifugal dewatering device 15 is communicated with the extraction waste liquid collecting tank 61 through a discharge pipe a51, and the centrifugal dewatering device 15 discharges the extraction waste liquid into the extraction waste liquid collecting tank 61 through a discharge pipe a51 and a control valve 3.
Referring to fig. 1, the extraction waste liquid collecting tank 61 and the sedimentation tank 63 are also communicated with each other through a communication pipe 2, a feed pump a71 is arranged on the communication pipe 2, and a control valve 3 is also arranged on the communication pipe 2. The extraction waste liquid collecting tank 61 feeds the extraction waste liquid into the settling tank 63 through the communicating pipe 2, the feed pump a71 and the control valve 3.
Referring to fig. 1, the calcium hydroxide adding tank 62 is also communicated with the sedimentation tank 63 through a communicating pipe 2, a feeding pump b72 is arranged on the communicating pipe 2, and a control valve 3 is also arranged on the communicating pipe 2. The calcium hydroxide adding tank 62 adds calcium hydroxide into the sedimentation tank 63 through the communicating pipe 2, the adding pump b72 and the control valve 3, and the extraction waste liquid and the calcium hydroxide are mixed and react to generate precipitate and supernatant. The sedimentation tank 63 is provided with a discharging pipe a81, the discharging pipe a81 is also provided with a control valve 3, and sediments are discharged from the discharging pipe a 81.
Referring to fig. 1, the sedimentation tank 63 is located above the crystallization tank 65, the sedimentation tank 63 and the crystallization tank 65 are also communicated through a communicating pipe 2, and the communicating pipe 2 is also provided with a control valve 3. The sedimentation tank 63 discharges the supernatant to the crystallization tank 65 through the connection pipe 2 and the control valve 3.
Referring to fig. 1, the freezing device 64 and the crystallization tank 65 are also communicated through the communicating pipe 2, and the freezing device 64 cools the crystallization tank 65, and keeps the temperature of the supernatant in the crystallization tank 65 constant, and the supernatant is cooled in the crystallization tank 65, so as to obtain a crystal and a mother liquor.
Referring to fig. 1, the crystallization tank 65 and the extraction stirring tank 13 are also communicated with each other through a communication pipe 2, and a feed pump c73 is provided on the communication pipe 2, and a control valve 3 is also provided on the communication pipe 2. The crystallization tank 65 adds the mother liquor into the extraction stirring tank 13 through the communicating pipe 2, the feed pump c73 and the control valve 3, and realizes the recycling of the mother liquor.
Referring to fig. 1, the crystallization tank 65 and the dehydration drying apparatus 66 are also connected through a connection pipe 2, and the connection pipe is provided with a feed pump d74, and the connection pipe 2 is also provided with a control valve 3. The crystallizing tank 65 feeds the crystal into the dehydration drying device 66 through the communicating tube 2, the feeding pump d74 and the control valve 3, and further dehydrates in the dehydration drying device 66, and then dries to obtain calcium chloride hexahydrate and mother liquor. The dehydration drying equipment 66 is provided with a discharging pipe b82, the discharging pipe b82 is also provided with a control valve 3, and calcium chloride hexahydrate is discharged from a discharging pipe b 82. The dewatering and drying equipment 66 is provided with a discharging pipe c83, the discharging pipe c83 is also provided with a control valve 3, and mother liquor is discharged from the discharging pipe c 83.
Referring to fig. 1, the washing and dewatering agitation tank 17 is located above the washing waste liquid collection tank 67. The washing dewatering agitation tank 17 and the washing waste liquid collection tank 67 are communicated with each other through a discharge pipe b 52. The washing and dewatering agitation tank 17 discharges the washing waste liquid into the washing waste liquid collection tank 67 through the discharge pipe b52 and the control valve 3.
Referring to fig. 1, the dehydration drying apparatus 18 is located above the washing waste liquid collecting tank 67. The dewatering and drying device 18 is communicated with the cleaning waste liquid collecting tank 67 through a discharge pipe c 53. The discharge pipe b52 is communicated with the discharge pipe c 53. The dewatering and drying device 18 discharges the cleaning waste liquid into the cleaning waste liquid collecting tank 67 through the discharge pipe c53 and the control valve 3.
Referring to fig. 1, the cleaning waste liquid collecting tank 67 and the reverse osmosis apparatus 68 are also communicated with each other through a communicating pipe 2, a feed pump e75 is provided on the communicating pipe 2, and a control valve 3 is also provided on the communicating pipe 2. The cleaning waste liquid collecting tank 67 discharges the cleaning waste liquid into the reverse osmosis device 68 through the communicating pipe 2, the feed pump e75 and the control valve 3, and concentrates the cleaning waste liquid to obtain concentrated waste liquid and clear water.
Referring to fig. 1, the reverse osmosis device 68 is also communicated with the extraction waste liquid collecting tank 61 through a communicating pipe 2, a feed pump f76 is arranged on the communicating pipe 2, and a control valve 3 is also arranged on the communicating pipe 2. The reverse osmosis device 68 discharges the concentrated waste liquid into the extraction waste liquid collecting tank 61 through the communicating pipe 2, the feed pump f76 and the control valve 3, and mixes the concentrated waste liquid with the extraction waste liquid.
Referring to fig. 1, the reverse osmosis device 68 is also communicated with the washing, dewatering and stirring tank 17 through a communicating pipe 2, a feed pump g77 is arranged on the communicating pipe 2, and a control valve 3 is also arranged on the communicating pipe 2. The reverse osmosis device 68 adds clean water into the washing and dewatering stirring pool 17 through the communicating pipe 2, the feed pump g77 and the control valve 3, so as to realize the recycling of water.
The purification and whitening processing system realizes the purification and whitening of the barite ore powder and has the advantages of simple and stable use. The waste water treatment system realizes the treatment of extraction waste liquid and cleaning waste liquid, reduces the waste water treatment cost due to no adoption of an evaporation process, and obtains a calcium chloride hexahydrate by-product. The reverse osmosis is adopted in the cleaning waste liquid for concentration, the influence of greatly increasing the wastewater treatment capacity due to the cleaning waste liquid is also reduced, the practicability of the wastewater treatment process is improved, and the wastewater treatment system has the advantages of simplicity and convenience in use and stability.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (10)

1. A treatment process of barite ore powder purification and whitening wastewater is used for treating wastewater generated in the barite ore powder extraction and whitening process, and is characterized in that: the purification whitening process comprises the following steps: extracting, growing crystal, dehydrating, cleaning, dehydrating and drying the barite ore powder to obtain a product;
in the extraction step, extracting the barite mineral powder by using an extraction liquid, wherein raw materials of the extraction liquid comprise 24-26% of hydrochloric acid, 5-10% of a lattice modifier and barium chloride;
the waste water comprises extraction waste liquid, and the extraction waste liquid is obtained after dehydration;
the wastewater treatment process comprises the following steps:
removal of magnesium and iron ions
Adding calcium hydroxide into the wastewater, enabling the pH value of the wastewater to be 8.5-9.5, stirring and uniformly mixing, carrying out reaction treatment for 2-3h, and then standing for 0.5-1.5h to obtain a precipitate and a supernatant;
calcium chloride crystal
Cooling the supernatant to 5-10 deg.C, standing, and keeping the temperature for 4-6 hr to obtain crystal and mother liquor;
recovery of calcium chloride hexahydrate
Drying the crystal to obtain calcium chloride hexahydrate.
2. The process for treating wastewater from the purification and whitening of barite ore powder as claimed in claim 1, wherein: and the mother liquor flows back to the extraction step and is recycled.
3. The process for treating wastewater from the purification and whitening of barite ore powder as claimed in claim 1, wherein: in the step of removing magnesium and iron ions, the added calcium hydroxide is saturated calcium hydroxide solution.
4. The process for treating wastewater from the purification and whitening of barite ore powder as claimed in claim 1, wherein: in the step of recovering calcium chloride hexahydrate, the drying temperature is 65-85 ℃, and the drying time is 2-3 h.
5. The process for treating wastewater from the purification and whitening of barite ore powder as claimed in claim 1, wherein: the waste water also comprises cleaning waste liquid, and the cleaning waste liquid is obtained after cleaning and dewatering.
6. The process for treating wastewater from the purification and whitening of barite ore powder as claimed in claim 5, wherein: and the washing waste liquid is concentrated to obtain concentrated waste liquid and clear water, and the concentrated waste liquid and the extraction waste liquid are mixed for wastewater treatment.
7. The process for treating wastewater from the purification and whitening of barite ore according to claim 6, wherein the process comprises the following steps: and concentrating the cleaning waste liquid by adopting reverse osmosis.
8. The process for treating wastewater from the purification and whitening of barite ore according to claim 6, wherein the process comprises the following steps: the total ion concentration in the clear water is less than or equal to 5 percent.
9. The process for treating wastewater from the purification and whitening of barite ore according to claim 8, wherein the process comprises the following steps: and the clean water flows back to the cleaning and dehydrating step and is recycled.
10. A barite ore fines purification and whitening wastewater treatment system as recited in any one of claims 1-9, further comprising: comprises an extraction waste liquid collecting tank (61), a calcium hydroxide feeding tank (62), a sedimentation tank (63), a freezing device (64), a crystallizing tank (65) and a dehydration drying device (66);
the extraction waste liquid collecting tank (61) is communicated with the sedimentation tank (63) through a communicating pipe (2), and the extraction waste liquid is discharged into the sedimentation tank (63);
the calcium hydroxide adding tank (62) is communicated with the sedimentation tank (63) through a communicating pipe (2), calcium hydroxide is discharged into the sedimentation tank (63), and the calcium hydroxide and the extraction waste liquid react in the sedimentation tank (63) to obtain a precipitate and a supernatant;
the sedimentation tank (63) is communicated with the crystallization tank (65) through a communicating pipe (2), and supernatant is discharged into the crystallization tank (65);
the freezing equipment (64) is communicated with the crystallization tank (65) through a communicating pipe (2), and the supernatant in the crystallization tank (65) is cooled to obtain a crystal and a mother liquor;
the crystallization tank (65) is communicated with the dehydration drying equipment (66) through a communicating pipe (2), and the crystal is discharged into the dehydration drying equipment (66) and is dehydrated and dried to obtain calcium chloride hexahydrate and mother liquor.
CN202110091903.5A 2021-01-23 2021-01-23 Treatment process and treatment system for barite ore powder purification and whitening wastewater Pending CN112919671A (en)

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