CN115010167B - Novel process for recycling calcium silicate slag containing copper and molybdenum - Google Patents
Novel process for recycling calcium silicate slag containing copper and molybdenum Download PDFInfo
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- CN115010167B CN115010167B CN202210505592.7A CN202210505592A CN115010167B CN 115010167 B CN115010167 B CN 115010167B CN 202210505592 A CN202210505592 A CN 202210505592A CN 115010167 B CN115010167 B CN 115010167B
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- molybdenum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a novel process for recycling calcium silicate slag containing copper and molybdenum, which comprises the following steps: 1) Adding sulfuric acid into the calcium silicate slag containing copper and molybdenum, and adjusting the pH value to carry out acid washing; 2) Carrying out primary filter pressing after the acid washing, washing with sulfuric acid after the filter pressing is finished, and carrying out air blowing and slag discharging after the washing is finished; 3) Adding sodium hydroxide into the copper-molybdenum mixed solution obtained in the step 2), and adjusting the pH value to precipitate copper; 4) Carrying out secondary filter pressing on the solution after copper deposition, washing after the filter pressing is finished, and carrying out air blowing and slag discharging after the washing is finished; 5) Adding sulfuric acid into the molybdenum solution obtained in the step 4), and adjusting the pH value to precipitate molybdenum; 6) And (3) carrying out pressure filtration on the solution after molybdenum precipitation for three times, washing with sulfuric acid after the pressure filtration is finished, and carrying out air blowing and slag discharging after the pressure filtration is finished, wherein the slag is molybdic acid, and the filtrate is sulfuric acid with the pH value of 1-2. The invention adopts a precipitation method to separate copper and molybdenum solutions, shortens the production flow and realizes the aim of being friendly to the environment and operators.
Description
Technical Field
The invention belongs to the technical field of industrial waste residue recovery treatment, and relates to a novel process for recovering and treating calcium silicate slag containing copper and molybdenum.
Background
Along with the development of economic construction, the requirements for high-copper, high-calcium and high-silicon molybdenum concentrates are increasingly larger, but the molybdenum resources have the problems of more lean ores, less rich ores, serious co-occurrence, more other useful components, fine embedding granularity and the like, the recovery rate of molybdenum is low in the smelting process, and the main components of the generated waste residues are copper-containing and molybdenum-calcium silicate residues and the copper-molybdenum separation is difficult.
Along with the development of economic construction, the requirement on copper and molybdenum is larger and larger, but copper and molybdenum resources have the problems of more lean ores, less rich ores, serious co-occurrence, more other useful components, fine embedding granularity and the like, so that the copper and molybdenum are difficult to separate. The currently available molybdenum and copper solution separation methods are mainly extraction separation methods. The molybdenum and copper solutions are separated by an extraction method, and the method has the characteristics of long production flow, expensive extractant, volatile extractant and easy toxicity making, and is not friendly to the environment and operators.
In addition, the recovery treatment of the calcium silicate slag containing copper and molybdenum is not reported in China, and the industry has no similar method.
Disclosure of Invention
The invention aims to provide a novel process for recycling calcium silicate slag containing copper and molybdenum, which adopts a precipitation method to separate copper and molybdenum solutions, shortens the production flow and realizes the aim of being friendly to the environment and operators.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a novel process for recycling calcium silicate slag containing copper and molybdenum comprises the following steps:
1) Adding sulfuric acid into the calcium silicate slag containing copper and molybdenum, and adjusting the pH value for pickling;
2) Washing with sulfuric acid after the acid washing is finished, blowing and deslagging after the acid washing is finished, wherein the slag is mixed slag of silicic acid and calcium sulfate, and the filtrate is copper-molybdenum mixed solution with the pH value of 3-4;
3) Adding sodium hydroxide into the copper-molybdenum mixed solution obtained in the step 2), and adjusting the pH value to precipitate copper;
4) Carrying out secondary filter pressing on the solution after copper deposition, washing after the filter pressing is finished, and carrying out air blowing and slag discharging after the filter pressing is finished, wherein slag is copper hydroxide slag, and filtrate is molybdenum solution with pH value of 7-8;
5) Adding sulfuric acid into the molybdenum solution obtained in the step 4), and adjusting the pH value to precipitate molybdenum;
6) And (3) carrying out pressure filtration on the solution after molybdenum precipitation for three times, washing with sulfuric acid after the pressure filtration is finished, and carrying out air blowing and slag discharging after the pressure filtration is finished, wherein the slag is molybdic acid, and the filtrate is sulfuric acid with the pH value of 1-2.
Preferably, in step 1), the pH is adjusted to 3-4, and the stirring is started to wash for more than 1 hour, so that copper and molybdenum enter the solution, and silicon and calcium exist in the solid phase in the form of silicic acid and calcium sulfate slag.
Preferably, in the step 2), the pickling is carried out by a filter press for one time, and after the filter pressing is finished, the pickling is carried out by sulfuric acid with the volume of 2 times of the chamber volume of the filter press.
More preferably, step 2) is washed with sulfuric acid having a concentration of 0.0096-0.096g/l after the completion of one press filtration.
Preferably, in step 3), copper is precipitated by adjusting the pH between 7 and 8, the copper precipitates as copper hydroxide and the molybdenum continues to remain in solution in ionic form.
Preferably, in the step 4), the solution after copper deposition is subjected to secondary pressure filtration through a pressure filter, and after the pressure filtration is finished, water with the volume of 2 times of the pressure filter cavity is used for washing.
Preferably, in the step 5), the pH value is adjusted to be between 1 and 2, the mixture is heated to 80 to 100 ℃ and kept for more than 2 hours, and molybdenum reacts to form molybdic acid solid.
Preferably, in the step 6), the solution after molybdenum precipitation is subjected to three times of filter pressing through a filter press, and the solution is washed by sulfuric acid with the volume of 2 times of the chamber volume of the filter press after the filter pressing is finished.
More preferably, step 6) is followed by washing with sulfuric acid at a concentration of 0.96-9.6g/l after the completion of the three press filtration.
Preferably, the method further comprises the step of returning the sulfuric acid obtained in the step 6) to the step 1) for pickling.
In the application, the calcium silicate slag containing copper and molybdenum is pickled by sulfuric acid, silicon and calcium exist in a solid phase in the form of silicic acid and calcium sulfate slag, copper and molybdenum exist in a solution in the form of ions, after primary liquid-solid separation, the copper and molybdenum solution is subjected to pH value adjustment by adding alkali to enable copper to precipitate into copper hydroxide slag to be reserved in the solid phase, molybdenum continues to be reserved in the solution in the form of ions, after secondary liquid-solid separation, the molybdenum-containing solution is added with sulfuric acid to enable molybdenum to precipitate into molybdic acid to be reserved in the solid phase, and after tertiary liquid-solid separation, the acid filtrate is returned to wash the calcium silicate slag containing copper and molybdenum.
The invention has the beneficial effects that:
the calcium silicate slag containing copper and molybdenum is recovered and treated, and the copper solution and the molybdenum solution are separated by adopting a precipitation method, so that the production flow is shortened, and the purposes of environmental friendliness and operator friendliness are realized.
Drawings
Fig. 1 is a process flow diagram of the present invention.
Detailed Description
In order to more clearly illustrate the present invention, the present invention will be described in further detail below with reference to examples and with reference to the accompanying drawings. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and that this invention is not limited to the details given herein.
Examples
1. Application range
The method is suitable for recycling the calcium silicate slag containing copper and molybdenum.
2. Principle of the method
The method comprises the steps of carrying out acid washing on copper-molybdenum-containing calcium silicate slag by sulfuric acid, enabling silicon and calcium to exist in solid phases in the form of silicic acid and calcium sulfate slag, enabling copper and molybdenum to exist in solution in the form of ions, enabling copper to be precipitated into copper hydroxide slag to be reserved in the solid phases by adding alkali to adjust pH value after primary liquid-solid separation, enabling molybdenum to be reserved in the solution continuously in the form of ions, enabling molybdenum to be precipitated into molybdic acid to be reserved in the solid phases by adding sulfuric acid into the molybdenum-containing solution after secondary liquid-solid separation, and enabling acid filtrate to return to wash the copper-molybdenum-containing calcium silicate slag after tertiary liquid-solid separation.
3. Operating procedure
The embodiment is used for treating smelting waste slag containing high copper, high calcium and high silicon molybdenum concentrate of China department, wherein the copper content is more than or equal to 10%, the calcium content is more than or equal to 7% and the silicon content is more than or equal to 8%. Referring to fig. 1, the process steps of the present invention mainly include:
3.1 acid washing
Adding sulfuric acid with the concentration of 30-50% into calcium silicate slag containing copper and molybdenum, regulating the pH value to 3-4, starting stirring and washing for more than 1 hour, enabling copper and molybdenum to enter into solution, and enabling silicon and calcium to exist in solid phase in the form of silicic acid and calcium sulfate slag.
3.2 one time press filtration and washing
And after the acid washing is finished, carrying out primary filter pressing through a filter press, washing by adopting sulfuric acid with the volume of 2 times of the cavity volume of the filter press, wherein the concentration of the sulfuric acid is 0.0096-0.096g/l, and carrying out air blowing and slag discharging after washing, wherein the slag is mixed slag of silicic acid and calcium sulfate, and the filtrate is copper-molybdenum mixed solution with the pH value of 3-4. After the steps of acid washing, primary pressure filtration and washing, the copper content in the calcium silicate slag containing copper and molybdenum is less than or equal to 0.05 percent, and the molybdenum content is less than or equal to 0.01 percent.
3.3 copper deposition
Adding 200-400g/l sodium hydroxide solution into the copper-molybdenum mixed solution under stirring, adjusting the pH value to 7-8, precipitating copper into copper hydroxide, and keeping molybdenum in the solution in an ionic state.
3.4 secondary pressure filtration and washing
And (3) carrying out secondary filter pressing on the solution after copper precipitation through a filter press, washing the solution after the filter pressing by adopting water with the volume of 2 times of the cavity volume of the filter press, and carrying out air blowing and slag discharging after washing, wherein the slag is copper hydroxide slag, and the filtrate is molybdenum solution with the pH value of 7-8. After copper deposition, secondary filter pressing and washing steps, the copper content in the solution can reach less than or equal to 5mg/l, and the copper content of the produced copper hydroxide is between 63.5 and 64.5 percent.
3.5 molybdenum deposition
Adding sulfuric acid with the concentration of 30-50% into molybdenum solution with the pH value of 7-8 under stirring, adjusting the pH value to 1-2, heating to 80-100 ℃, maintaining the reaction time for more than 2 hours, and reacting molybdenum to generate molybdic acid solid.
3.6 three times of filter pressing and washing
And (3) carrying out three times of filter pressing on the solution after molybdenum precipitation through a filter press, washing the solution after the filter pressing by sulfuric acid with the volume of 2 times of the chamber volume of the filter press, blowing air and discharging slag after the sulfuric acid concentration is 0.96-9.6g/l, wherein the slag is molybdic acid, and returning the filtrate which is sulfuric acid with the pH value of 1-2 to 3.1 for pickling. After molybdenum deposition, three times of filter pressing and washing, the molybdenum content in the solution can reach less than or equal to 2mg/l, and the content of the produced molybdenum molybdate is 57-58.5%.
It should be understood that the foregoing examples of the present invention are merely illustrative of the present invention and not limiting of the embodiments of the present invention, and that various other changes and modifications can be made by those skilled in the art based on the above description, and it is not intended to be exhaustive of all the embodiments of the present invention, and all obvious changes and modifications that come within the scope of the invention are defined by the following claims.
Claims (10)
1. A novel process for recycling calcium silicate slag containing copper and molybdenum comprises the following steps:
1) Adding sulfuric acid into the calcium silicate slag containing copper and molybdenum, and adjusting the pH value for pickling;
2) Washing with sulfuric acid after the acid washing is finished, blowing and deslagging after the acid washing is finished, wherein the slag is mixed slag of silicic acid and calcium sulfate, and the filtrate is copper-molybdenum mixed solution with the pH value of 3-4;
3) Adding sodium hydroxide into the copper-molybdenum mixed solution obtained in the step 2), and adjusting the pH value to precipitate copper;
4) Carrying out secondary filter pressing on the solution after copper deposition, washing after the filter pressing is finished, and carrying out air blowing and slag discharging after the filter pressing is finished, wherein slag is copper hydroxide slag, and filtrate is molybdenum solution with pH value of 7-8;
5) Adding sulfuric acid into the molybdenum solution obtained in the step 4), and adjusting the pH value to precipitate molybdenum;
6) And (3) carrying out pressure filtration on the solution after molybdenum precipitation for three times, washing with sulfuric acid after the pressure filtration is finished, and carrying out air blowing and slag discharging after the pressure filtration is finished, wherein the slag is molybdic acid, and the filtrate is sulfuric acid with the pH value of 1-2.
2. The novel process for recycling copper-molybdenum-containing calcium silicate slag in step 1), wherein in step 1), the pH value is adjusted to 3-4, stirring is started and washing is performed for more than 1 hour, copper and molybdenum are put into solution, and silicon and calcium exist in solid phase in the form of silicic acid and calcium sulfate slag.
3. The novel process for recycling calcium silicate slag containing copper and molybdenum according to claim 1, wherein in the step 2), the acid washing is completed by one-time press filtration through a press filter, and the washing is performed by 2 times of sulfuric acid in the chamber volume of the press filter after the press filtration is completed.
4. The novel process for recycling copper-molybdenum-containing calcium silicate slag in accordance with claim 3, wherein the step 2) is carried out by washing with sulfuric acid with a concentration of 0.0096-0.096g/l after the completion of the one-time press filtration.
5. The novel process for the recovery treatment of copper-molybdenum-containing calcium silicate slag according to claim 1, characterized in that in step 3), copper is precipitated by adjusting the pH between 7 and 8, copper precipitates as copper hydroxide, and molybdenum continues to remain in solution in an ionic state.
6. The novel process for recycling copper-molybdenum-containing calcium silicate slag in step 4) according to claim 1, wherein the solution after copper deposition is subjected to secondary pressure filtration by a filter press, and after the pressure filtration is completed, the solution is washed by water with a volume of 2 times of the chamber volume of the filter press.
7. The novel process for recycling calcium silicate slag containing copper and molybdenum according to claim 1, wherein in step 5), the pH value is adjusted to be between 1 and 2, the mixture is heated to be between 80 and 100 ℃ and kept for more than 2 hours, and molybdenum reacts to form molybdic acid solid.
8. The novel process for recycling copper-molybdenum-containing calcium silicate slag in step 6) according to claim 1, wherein the solution after molybdenum precipitation is subjected to three times of filter pressing by a filter press, and the solution is washed by sulfuric acid with a volume of 2 times of the chamber volume of the filter press after the filter pressing is finished.
9. The novel process for recycling copper-molybdenum-containing calcium silicate slag in accordance with claim 8, wherein, after the three times of press filtration in step 6), sulfuric acid with concentration of 0.96-9.6g/l is used for washing.
10. The novel process for recycling calcium silicate slag containing copper and molybdenum according to any one of claims 1-9, further comprising returning sulfuric acid obtained in step 6) to step 1) for pickling.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4444733A (en) * | 1983-02-28 | 1984-04-24 | Amax Inc. | Process for recovering molybdenum and copper from sulfide concentrates |
| CN102811977A (en) * | 2010-09-10 | 2012-12-05 | 哈斯科公司 | Agricultural blend containing sulfate source and calcium silicate and method of forming the same |
| RU2535254C1 (en) * | 2013-10-31 | 2014-12-10 | Игорь Александрович Фарбер | Method of complex processing of serpentine-chromite crude ore |
| DE102016007030A1 (en) * | 2016-06-08 | 2018-01-18 | GbR Projektservice (vertretungsberechtigter Gesellschafter Dr. sc. oec. Lutz Koch, 06295 Lutherstdt Eisleben) | Process for the complete metallurgical processing of Manfeld copper slags by production of polymineral mass products |
| CN109468468A (en) * | 2018-11-29 | 2019-03-15 | 成都虹波钼业有限责任公司 | A method of comprehensive utilization and processing molybdenum copper ashes |
| CN112831660A (en) * | 2020-12-30 | 2021-05-25 | 成都虹波钼业有限责任公司 | Process for comprehensively utilizing molybdenum ore leaching slag |
| CN113528857A (en) * | 2021-06-16 | 2021-10-22 | 福建常青新能源科技有限公司 | Continuous production method for recovering cobalt from cobalt-containing waste residues |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ZA848015B (en) * | 1983-12-30 | 1985-08-28 | Stauffer Chemical Co | Treatment for spent petroleum cracking catalyst |
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- 2022-05-10 CN CN202210505592.7A patent/CN115010167B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4444733A (en) * | 1983-02-28 | 1984-04-24 | Amax Inc. | Process for recovering molybdenum and copper from sulfide concentrates |
| CN102811977A (en) * | 2010-09-10 | 2012-12-05 | 哈斯科公司 | Agricultural blend containing sulfate source and calcium silicate and method of forming the same |
| RU2535254C1 (en) * | 2013-10-31 | 2014-12-10 | Игорь Александрович Фарбер | Method of complex processing of serpentine-chromite crude ore |
| DE102016007030A1 (en) * | 2016-06-08 | 2018-01-18 | GbR Projektservice (vertretungsberechtigter Gesellschafter Dr. sc. oec. Lutz Koch, 06295 Lutherstdt Eisleben) | Process for the complete metallurgical processing of Manfeld copper slags by production of polymineral mass products |
| CN109468468A (en) * | 2018-11-29 | 2019-03-15 | 成都虹波钼业有限责任公司 | A method of comprehensive utilization and processing molybdenum copper ashes |
| CN112831660A (en) * | 2020-12-30 | 2021-05-25 | 成都虹波钼业有限责任公司 | Process for comprehensively utilizing molybdenum ore leaching slag |
| CN113528857A (en) * | 2021-06-16 | 2021-10-22 | 福建常青新能源科技有限公司 | Continuous production method for recovering cobalt from cobalt-containing waste residues |
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