CN112403028A - Method for purifying lead electrolyte by using columnar activated carbon - Google Patents
Method for purifying lead electrolyte by using columnar activated carbon Download PDFInfo
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- CN112403028A CN112403028A CN202010817378.6A CN202010817378A CN112403028A CN 112403028 A CN112403028 A CN 112403028A CN 202010817378 A CN202010817378 A CN 202010817378A CN 112403028 A CN112403028 A CN 112403028A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
- B01D15/203—Equilibration or regeneration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/18—Electrolytic production, recovery or refining of metals by electrolysis of solutions of lead
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/06—Operating or servicing
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
Abstract
The invention discloses a method for purifying lead electrolyte by using columnar activated carbon, which relates to the technical field of purifying lead electrolyte by using activated carbon, in particular to a method for purifying lead electrolyte by using columnar activated carbon, and comprises the following steps: s1, purifying lead electrolyte; s2, desorbing and regenerating the active carbon exchange column group; s3, neutralizing and recycling the waste water. The method for purifying the lead electrolyte by using the columnar activated carbon adopts the activated carbon adsorption exchange column group for purification, has simple operation, does not need other auxiliary reagents, and generally needs desorption regeneration for three months after the activated carbon exchange column group works for a period of time; adsorbing substances in the solution to be separated by using active carbon; calcium chloride is used as a desorption agent for desorption and regeneration of the activated carbon; CaCl2 is selected as a desorption agent, so that the adsorption stability of the activated carbon on the adsorbate can be reduced, and the aim of reducing desorption activation energy is fulfilled; the ions such as bismuth and antimony absorbed in the activated carbon are eluted through desorption operation, and the carbon column is washed by purified water to achieve the purpose of activated carbon regeneration.
Description
Technical Field
The invention relates to the technical field of purifying lead electrolyte by activated carbon, in particular to a method for purifying lead electrolyte by using columnar activated carbon.
Background
In the electrolytic refining of the lead bullion, the lead bullion anode usually contains impurities such as gold, silver, copper, antimony, arsenic, tin, bismuth and the like, and during the electrolytic refining process, metals with a potential negative than that of the lead, such as zinc, iron, cadmium, cobalt, nickel and the like, contained in the anode are dissolved out from the anode together with the lead, but are not generally precipitated at the cathode; metals with positive potential than lead, such as antimony, bismuth, copper, gold and the like, hardly enter the electrolyte and are left in the anode mud; in actual production, a small amount of the metal ions enter the electrolyte, particularly bismuth, and main impurities forming electrolytic lead are separated out at the cathode under the action of electrophoresis.
In order to recover lead and silicofluoric acid in the anode slime, the anode slime is washed by water, and the impurity content of the lead electrolyte is ultrahigh due to the fact that the washing water of the anode slime contains high bismuth and antimony.
In order to purify the lead electrolyte and ensure the normal operation of the lead electrolysis process and the quality of the electrolytic lead, the harmful impurities such as bismuth, copper, antimony, silver and the like in the lead electrolyte must be continuously removed.
For purifying the lead electrolyte, various purification methods can be used, such as a chemical method, an activated carbon adsorption method, an extraction method, an ion exchange method, and the like. The chemical method adds other reagents and introduces impurities, and has the disadvantages of long process flow, high energy consumption and environmental pollution caused by organic solvents in the extraction method and the ion exchange process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for purifying lead electrolyte by using columnar activated carbon, which solves the problem that in the prior art, a small amount of metal ions, particularly bismuth, enter the electrolyte in actual production and are precipitated at a cathode under the action of electrophoresis to form main impurities of electrolytic lead.
In order to achieve the purpose, the invention is realized by the following technical scheme: the method for purifying the lead electrolyte by using the columnar activated carbon comprises the following steps:
s1, lead electrolyte purification: opening a liquid storage tank valve of lead electrolyte to be purified, starting an anti-corrosion pump and related valves, controlling the flow rate to be 50L/min, enabling the lead electrolyte to be purified to enter an activated carbon exchange column group, sampling and analyzing harmful impurities such as bismuth, antimony and the like in the lead electrolyte to be purified after the lead electrolyte to be purified completely passes through the activated carbon exchange column group, taking purified liquid for detection, merging the purified liquid into a lead electrolyte circulating system after the purified liquid meets the requirements, and repeatedly purifying unqualified purified liquid until the purified liquid is qualified;
s2, desorption and regeneration of the activated carbon exchange column group: the active carbon exchange column group is required to be desorbed and regenerated after running for about three months; during desorption operation, lead electrolyte containing harmful impurities such as bismuth, antimony and the like to be purified passes through a columnar active carbon exchange column group to adsorb harmful impurity ions in the lead electrolyte to be purified, calcium chloride liquid is added into a desorption agent box, 6-10g/L of calcium chloride is controlled, an anticorrosion pump and a relevant valve are opened to carry out desorption, pure water is added into the desorption agent box to wash the exchange column for three times after desorption is completed, and purification operation can be carried out after washing is completed;
s3, neutralizing and recycling wastewater: and pumping the desorption solution and the washing solution to a wet workshop for neutralization and precipitation, recovering valuable elements in the solution, and delivering the waste solution to a sewage station for disposal.
Optionally, in the step S1, during the purification of the lead electrolyte, the activated carbon exchange column group is formed by connecting three activated carbon exchange columns in series, the activated carbon exchange columns are made of organic glass, and the height-diameter ratio is 5: 1.
optionally, the exchange column is connected by transparent high-pressure plastic hose, and the hose diameter is 50mm, and pumping power is anticorrosive pump, and the power of pump motor is 5.5 KW.
Optionally, the activated carbon in the activated carbon exchange column group is columnar coconut shell activated carbon.
Optionally, in the step S1 and the lead electrolyte purification, the purification mode is a dynamic mode.
Optionally, the dynamic mode is that the lead electrolyte to be purified is pumped into the activated carbon exchange column group by an anticorrosive pump, the flow rate is controlled to be 50L/min, the lead electrolyte to be purified completely passes through the activated carbon exchange column group, then, the lead electrolyte is sampled and analyzed for harmful impurities such as bismuth, antimony and the like, and the lead electrolyte can be merged into the lead electrolyte circulating system after being qualified.
Optionally, in step S2 and the desorption and regeneration of the activated carbon exchange column group, the activated carbon desorption and regeneration system shares the anticorrosion pump, and the desorption agent is contained in the desorption agent box which is specially manufactured and is connected with the outlet pipe diameter of the anticorrosion pump through a tee joint and a valve.
The invention provides a method for purifying lead electrolyte by using columnar activated carbon, which has the following beneficial effects:
the invention relates to a lead electrolyte purification method, which comprises the steps of contacting electrolyte containing impurities such as bismuth and antimony to be purified with columnar carbon, adsorbing the impurities such as bismuth and antimony by the activated carbon, and regenerating the activated carbon by using calcium chloride as a desorption agent after the activated carbon is used for three months. The method has the advantages of friendly operation environment, low energy consumption, recyclable regenerated columnar activated carbon, low cost, no change of the main components of the lead electrolyte and direct utilization of the purified electrolyte;
the purification by adopting the activated carbon adsorption exchange column group has simple operation and does not need other auxiliary reagents, and the activated carbon adsorption exchange column group generally needs to be desorbed and regenerated for three months after working for a period of time; adsorbing substances in the solution to be separated by using active carbon; calcium chloride is used as a desorption agent for desorption and regeneration of the activated carbon; CaCl2 is selected as a desorption agent, so that the adsorption stability of the activated carbon on the adsorbate can be reduced, and the aim of reducing desorption activation energy is fulfilled; the ions such as bismuth and antimony absorbed in the activated carbon are eluted through desorption operation, and the carbon column is washed by purified water to achieve the purpose of activated carbon regeneration.
Drawings
FIG. 1 is a schematic diagram of the process steps of the present invention;
FIG. 2 is a simplified flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1 to 2, the present invention provides a technical solution: the method for purifying the lead electrolyte by using the columnar activated carbon comprises the following steps:
s1, lead electrolyte purification: opening a liquid storage tank valve of lead electrolyte to be purified, starting an anti-corrosion pump and related valves, controlling the flow rate to be 50L/min, enabling the lead electrolyte to be purified to enter an activated carbon exchange column group, sampling and analyzing harmful impurities such as bismuth, antimony and the like in the lead electrolyte to be purified after the lead electrolyte to be purified completely passes through the activated carbon exchange column group, taking purified liquid for detection, merging the purified liquid into a lead electrolyte circulating system after the purified liquid meets the requirements, and repeatedly purifying unqualified purified liquid until the purified liquid is qualified;
s2, desorption and regeneration of the activated carbon exchange column group: the active carbon exchange column group is required to be desorbed and regenerated after running for about three months; during desorption operation, lead electrolyte containing harmful impurities such as bismuth, antimony and the like to be purified passes through a columnar active carbon exchange column group to adsorb harmful impurity ions in the lead electrolyte to be purified, calcium chloride liquid is added into a desorption agent box, 6-10g/L of calcium chloride is controlled, an anticorrosion pump and a relevant valve are opened to carry out desorption, pure water is added into the desorption agent box to wash the exchange column for three times after desorption is completed, and purification operation can be carried out after washing is completed;
s3, neutralizing and recycling wastewater: and pumping the desorption solution and the washing solution to a wet workshop for neutralization and precipitation, recovering valuable elements in the solution, and delivering the waste solution to a sewage station for disposal.
In the invention:
further, in the step S1, during the purification of the lead electrolyte, the activated carbon exchange column group is composed of three activated carbon exchange columns connected in series, the activated carbon exchange columns are made of organic glass, and the height-diameter ratio is 5: 1.
Furthermore, the exchange column is connected by transparent high-pressure plastic hose, and the hose diameter is 50mm, and pumping power is anticorrosive pump, and the power of pump motor is 5.5 KW.
Furthermore, the active carbon in the active carbon exchange column group is columnar coconut shell active carbon.
5. The method for purifying lead electrolyte using columnar activated carbon as claimed in claim 1, wherein: in the step S1 and the lead electrolyte purification, the purification mode is a dynamic mode.
Furthermore, the lead electrolyte to be purified is pumped into the active carbon exchange column group by an anticorrosive pump in a dynamic mode, the flow rate is controlled to be 50L/min, the lead electrolyte to be purified completely passes through the active carbon exchange column group, then, the lead electrolyte is sampled and analyzed for harmful impurities such as bismuth, antimony and the like in the lead electrolyte, and the lead electrolyte can be merged into a lead electrolyte circulating system after being qualified.
Further, in the desorption regeneration of the activated carbon exchange column group in the step S2, the activated carbon desorption regeneration system shares the anticorrosion pump, and the desorption agent is contained in the desorption agent box which is specially manufactured and is connected with the outlet pipe diameter of the anticorrosion pump through a tee joint and a valve.
In summary, the method for purifying the lead electrolyte by using the columnar activated carbon comprises the steps of opening a valve of a liquid storage tank of the lead electrolyte to be purified, starting an anti-corrosion pump and related valves, controlling the flow rate to be 50L/min, taking the purified liquid for detection, merging the purified liquid into a lead electrolyte circulating system after the purified liquid meets the requirement, and repeatedly purifying unqualified purified liquid until the purified liquid is qualified; secondly, the active carbon exchange column group needs to be desorbed and regenerated after running for about three months. During desorption operation, adding calcium chloride liquid into a desorption agent box, controlling 6-10g/L of calcium chloride, starting an anticorrosive pump and a related valve for desorption, adding pure water into the desorption agent box to wash the exchange column for three times after desorption is completed, and then, carrying out purification operation after washing is completed; then, the desorption solution and the washing solution are pumped to a wet workshop for neutralization and precipitation, valuable elements in the solution are recovered, and the waste solution is sent to a sewage station for disposal.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. The method for purifying the lead electrolyte by using the columnar activated carbon comprises the following steps:
s1, lead electrolyte purification: opening a liquid storage tank valve of lead electrolyte to be purified, starting an anti-corrosion pump and related valves, controlling the flow rate to be 50L/min, enabling the lead electrolyte to be purified to enter an activated carbon exchange column group, sampling and analyzing harmful impurities such as bismuth, antimony and the like in the lead electrolyte to be purified after the lead electrolyte to be purified completely passes through the activated carbon exchange column group, taking purified liquid for detection, merging the purified liquid into a lead electrolyte circulating system after the purified liquid meets the requirements, and repeatedly purifying unqualified purified liquid until the purified liquid is qualified;
s2, desorption and regeneration of the activated carbon exchange column group: the active carbon exchange column group is required to be desorbed and regenerated after running for about three months; during desorption operation, lead electrolyte containing harmful impurities such as bismuth, antimony and the like to be purified passes through a columnar active carbon exchange column group to adsorb harmful impurity ions in the lead electrolyte to be purified, calcium chloride liquid is added into a desorption agent box, 6-10g/L of calcium chloride is controlled, an anticorrosion pump and a relevant valve are opened to carry out desorption, pure water is added into the desorption agent box to wash the exchange column for three times after desorption is completed, and purification operation can be carried out after washing is completed;
s3, neutralizing and recycling wastewater: and pumping the desorption solution and the washing solution to a wet workshop for neutralization and precipitation, recovering valuable elements in the solution, and delivering the waste solution to a sewage station for disposal.
2. The method for purifying lead electrolyte using columnar activated carbon as claimed in claim 1, wherein: in S1 and lead electrolyte purification, the active carbon exchange column group is composed of three active carbon exchange columns which are connected in series, the active carbon exchange columns are made of organic glass, and the height-diameter ratio is 5: 1.
3. the method for purifying lead electrolyte using columnar activated carbon as claimed in claim 2, wherein: the exchange column is connected by transparent high-pressure plastic hose, and the hose diameter is 50mm, and pumping power is anticorrosive pump, and the power of pump motor is 5.5 KW.
4. The method for purifying lead electrolyte using columnar activated carbon as claimed in claim 1, wherein: the active carbon in the active carbon exchange column group is columnar coconut shell active carbon.
5. The method for purifying lead electrolyte using columnar activated carbon as claimed in claim 1, wherein: in the step S1 and the lead electrolyte purification, the purification mode is a dynamic mode.
6. The method for purifying lead electrolyte using columnar activated carbon as claimed in claim 1, wherein: the dynamic mode is that the lead electrolyte to be purified is pumped into the active carbon exchange column group by an anticorrosive pump, the flow rate is controlled to be 50L/min, the lead electrolyte to be purified completely passes through the active carbon exchange column group, then the sample is taken to analyze harmful impurities such as bismuth, antimony and the like in the lead electrolyte, and the lead electrolyte can be merged into a lead electrolyte circulating system after being qualified.
7. The method for purifying lead electrolyte using columnar activated carbon as claimed in claim 1, wherein: and in the step S2 and the desorption and regeneration of the activated carbon exchange column group, the activated carbon desorption and regeneration system shares the anticorrosion pump, and the desorption agent is filled in a desorption agent box which is specially manufactured and is connected with the outlet pipe diameter of the anticorrosion pump through a tee joint and a valve.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114045530A (en) * | 2021-11-30 | 2022-02-15 | 广东先导稀材股份有限公司 | Method for purifying and removing tin from indium sulfate electrolyte |
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| EP2532760A1 (en) * | 2011-06-06 | 2012-12-12 | Atotech Deutschland GmbH | Device and method for recovering nickel from a nickel plating bath fluid |
| CN105858779A (en) * | 2016-04-15 | 2016-08-17 | 江南大学 | Method for recycling metal from low-concentration heavy metal ion wastewater |
| CN108339520A (en) * | 2018-04-10 | 2018-07-31 | 黄山学院 | A kind of depth goes nano-sized iron oxide-charcoal complex, preparation method and its application method of heavy metal in water removal |
| CN111151221A (en) * | 2020-01-13 | 2020-05-15 | 黄山学院 | Macroporous biochar-based hybrid material for ultra-fast removal of heavy metals in water body and preparation method and application thereof |
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2020
- 2020-08-13 CN CN202010817378.6A patent/CN112403028A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1091479A (en) * | 1993-02-25 | 1994-08-31 | 北京有色金属研究总院 | A kind of processing method of clarifying lead electrolytic solution |
| EP2532760A1 (en) * | 2011-06-06 | 2012-12-12 | Atotech Deutschland GmbH | Device and method for recovering nickel from a nickel plating bath fluid |
| CN105858779A (en) * | 2016-04-15 | 2016-08-17 | 江南大学 | Method for recycling metal from low-concentration heavy metal ion wastewater |
| CN108339520A (en) * | 2018-04-10 | 2018-07-31 | 黄山学院 | A kind of depth goes nano-sized iron oxide-charcoal complex, preparation method and its application method of heavy metal in water removal |
| CN111151221A (en) * | 2020-01-13 | 2020-05-15 | 黄山学院 | Macroporous biochar-based hybrid material for ultra-fast removal of heavy metals in water body and preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114045530A (en) * | 2021-11-30 | 2022-02-15 | 广东先导稀材股份有限公司 | Method for purifying and removing tin from indium sulfate electrolyte |
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