CN108889287A - A kind of regeneration method of aluminium oxide defluorinating agent - Google Patents
A kind of regeneration method of aluminium oxide defluorinating agent Download PDFInfo
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- CN108889287A CN108889287A CN201810813063.7A CN201810813063A CN108889287A CN 108889287 A CN108889287 A CN 108889287A CN 201810813063 A CN201810813063 A CN 201810813063A CN 108889287 A CN108889287 A CN 108889287A
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- aluminium oxide
- defluorinating agent
- alkali cleaning
- pickling
- fluorine
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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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- 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
- B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
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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
- C25C1/16—Electrolytic production, recovery or refining of metals by electrolysis of solutions of zinc, cadmium or mercury
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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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- 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
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- Engineering & Computer Science (AREA)
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- Metallurgy (AREA)
- Electrolytic Production Of Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The regeneration method for being just to provide a kind of aluminium oxide defluorinating agent of the invention, using, as regenerative raw materials, including pickling, techniques, the defluorination effect of regenerated defluorinating agent such as alkali cleaning, washing and pulp processing be good for the Defluorination of Formation Mater By Adsorption On Activated Alumina agent after zinc electrolyte fluorine removal.The regenerated defluorinating agent prepared using present invention side, the fluorine in zinc electrolyte can be reduced to 32mg/L from 500mg/L.And realize that defluorinating agent regeneration method is easy to operate, zinc, fluorine desorption rate are high, and regenerability is good, and economic benefit and environmental benefit are significant, save the cost, have good result.
Description
Technical field：
The invention belongs to non-ferrous metallurgy fields, and in particular to a kind of regeneration method of zinc electrolyte defluorinating agent, especially one
The regeneration method of kind aluminium oxide defluorinating agent.
Background technique：
Currently, in Zinc Hydrometallurgy Process, fluorine, chlorine are largely present in leaching, purification and electrowinning process, due to a large amount of fluorine
In the presence of the corrosion fracture of the high-speed rotating components such as impeller and blender of meeting acceleration pump.It also will cause the pump being in contact with medium
The corrosion dissolution of the components such as shell, axle sleeve causes the leakage of pump.Bearing, screw rod, pedestal and the valve damage of pump are also resulted in simultaneously
It is bad.Fluorine ion in zinc sulphate electrolyte will cause the corrosion of cathode aluminum plate, destroys the passivating film on cathode aluminum plate, causes to be precipitated
Zinc sticks together with aluminium sheet, and stripping zinc is difficult, also will increase the consumption of cathode aluminum plate, be normally carried out electrolytic process can not.Therefore,
In Zinc Hydrometallurgy Process, the concentration of fluorine ion in strict control zinc sulphate electrolyte.
The zinc electrolyte defluorination method for being seen in report at present mainly has aluminum phosphate coprecipitation, lime method, ion exchange
Method, silica gel method, activated alumina method etc., however these really be applied to large-scale production and it is few.Defluorination of Formation Mater By Adsorption On Activated Alumina
Aluminium oxide defluorinating agent is in agent, because it has many advantages, such as using simple, with strong points, fluorine removing rate is high, reusable, thus
Increasingly by the favor in market.
China Patent Publication No. is that 102228746 A of CN discloses a kind of activated alumina and removes fluorine in solution of zinc sulfate
Method, the Defluorination of Formation Mater By Adsorption On Activated Alumina agent application method is simple, fluorine removing rate is high, but during defluorinating agent is regenerated
There is also following deficiencies：A large amount of zinc is adsorbed for the defluorinating agent after zinc electrolyte fluorine removal, the desorption rate of water-washing process zinc is not
It is high；Alkali wash water after alkali cleaning is not reused, and wastewater treatment process, high production cost are directly entered；Containing a large amount of in alkali cleaning slag
Fluorine-containing strong alkali solution just directly applies to next batch solution of zinc sulfate fluorine removal without washing, improves to a certain extent
The pH of system and the concentration of fluorine ion, reduce fluorine removing rate.
For the deficiency of current above method technique, how a kind of Defluorination of Formation Mater By Adsorption On Activated Alumina agent regeneration technology side is provided
Method, to enhance the defluorination effect of regenerative aluminium oxide defluorinating agent.Using regenerated aluminium oxide defluorinating agent, fluorine in zinc electrolyte can be from
500mg/L is reduced to 32mg/L.And realize that defluorinating agent regeneration method is easy to operate, zinc, fluorine desorption rate are high, and regenerability is good, and
And recycling number is high, realizes that economic benefit and environmental benefit are significant.
Summary of the invention：The regeneration method for being just to provide a kind of aluminium oxide defluorinating agent of the invention.To be removed for zinc electrolyte
Defluorination of Formation Mater By Adsorption On Activated Alumina agent after fluorine is regenerative raw materials, including pickling, and the techniques such as alkali cleaning, washing and pulp processing are regenerated to remove
The defluorination effect of fluorine agent is good.The regenerated defluorinating agent prepared using present invention side, the fluorine in zinc electrolyte can be reduced from 500mg/L
To 32mg/L.And realize that defluorinating agent regeneration method is easy to operate, zinc, fluorine desorption rate are high, and regenerability is good, economic benefit and environmental protection
Remarkable benefit.Save the cost has good result.
A kind of regeneration method of aluminium oxide defluorinating agent of the present invention, for the Defluorination of Formation Mater By Adsorption On Activated Alumina after zinc electrolyte fluorine removal
Agent is regenerative raw materials, it is characterized in that comprising the technical steps that：
1) pickling,
By the active oxidation aluminum feedstock after zinc electrolyte fluorine removal, it is slowly added to dilute acid soln during pulping and washing, carries out acid
It washes, controls pH >=5.0 of pickling solution, be made as acid elution liquid and consolidate mixed liquor, be filtered into pickling slag；
2）Alkali cleaning,
By 1）The filtered pickling slag of acid elution solid-liquid mixed liquor for walking preparation is added liquid alkaline and washes under conditions of certain temperature
It washs, replaces, filtering is separated by solid-liquid separation, and obtains alkali cleaning slag；
3）Washing,
To 2）It walks in the alkali cleaning slag being prepared and water is added, under agitation, washed, reduce step 2）The alkali of alkali cleaning slag
Property and fluorine content, be made as washing alkali cleaning slag；
4）Pulp, the sour fluorine removal of benefit, preparation, regeneration aluminium oxide defluorinating agent,
To 3）Suitable dilute acid soln is added in step washing alkali cleaning slag, carries out pulp processing under agitation, carries out at pulp
Dilute acid soln is added when reason, removes the zinc hydroxide of generation and removing is adsorbed in fluorine on aluminium oxide, filtering, filter residue, for regeneration
Aluminium oxide defluorinating agent.
It is currently preferred, it is step 1）Pickling, it is 5-10 that control liquid, which consolidates mixed liquor mass ratio,：1；The diluted acid is dilute sulphur
Acid, control dilute sulfuric acid concentration are 0.5-1.0mol/L, and the dilute acid soln addition time continues 15-20min, pickling temperature when controlling pickling
Degree is 25 DEG C -40 DEG C, time 30-60min.
It preferably, is step 2）Alkali cleaning, the lye are NaOH solution, and the NaOH solution concentration for controlling alkali cleaning is 1.0-
1.8mol/L, 65 DEG C -80 DEG C of alkali cleaning temperature, time 40-60min.
Further, dilute acid concentration used is 0.5-0.7mol/L when mending acid when being pulp processing.
It preferably, is control 1）Pickling, 2）Alkali cleaning and 3）Washing, 4）Pulp is to stir when preparation, regeneration aluminium oxide defluorinating agent
It mixes and is carried out under state, control stirring rate is 90-100r/min.
The present invention using the above method itself main advantage is that：Mild acid wash is used to the aluminium oxide defluorinating agent of failure
Mode, on the basis of guaranteeing not destroying defluorinating agent crystalline structure, the most of zinc that can adsorb defluorinating agent is dissolved out, not only favorably
In the regeneration using effect of enhancing defluorinating agent, while the pickling solution containing zinc enters zinc sulfate production system, effectively increases zinc
The rate of recovery.Alkali wash water is recycled, and can reduce liquid alkaline dosage, production cost is effectively reduced.When in the alkali wash water of reuse
F- concentration is more than 30g/L, into sodium fluoride production system, can substantially reduce sewage load, economical and environmentally friendly.After alkali cleaning again
Add one of washing step, the pH of alkali cleaning slag and the content of fluorine can be effectively reduced, is conducive to enhance regenerative aluminium oxide defluorinating agent
Defluorination effect.By filling into the dissolvable hydroxide for being wrapped in defluorinating agent surface of a small amount of acid solution in regeneration defluorinating agent slurrying process
Zinc further increases defluorination effect.The failure aluminium oxide defluorinating agent handled through the method for the present invention, the wash-off rate of fluorine are reachable
98.59%, for the wash-off rate of zinc up to 96.87%, the solution of zinc sulfate of fluorine content 510mg/L can be down to 32mg/L by regeneration defluorinating agent.
Good with defluorination effect, production cost is low, advantage easy to implement, is suitble to large-scale application.And the manufacturing cost of zinc is reduced,
Receive good effect.
Preparation process of the present invention：Failure aluminium oxide defluorinating agent → pickling → filtering → filter residue adds lye → filtering → alkali wash water
→ washing → filtering → regenerative aluminium oxide defluorinating agent → plus diluted acid, pulp → fluorine removal.
Description of the process, by the aluminium oxide defluorinating agent of failure after adding dilution heat of sulfuric acid pickling, filtering, filtrate enters zinc sulfate
Production system, filter residue are added liquid alkaline solution and carry out alkali cleaning, filtering, and filtered alkali cleaning filtrate enters sodium fluoride production system, alkali
Washery slag, that is, alkali cleaning aluminium oxide is washed with water, and filtering, obtained water lotion, into sewage disposal system, the washing slag after washing filtering is
Regenerated aluminium oxide defluorinating agent further uses the aluminium oxide defluorinating agent after claiming sulfuric acid to carry out pulp to be made as defluorinating agent
With.
Specific embodiment:The present invention is described in further detail With reference to embodiment；In following tools
The each component used involved in body embodiment each means quality or mass percent, defluorinating agent described in specification and embodiment
It each means aluminium oxide defluorinating agent or makes Defluorination of Formation Mater By Adsorption On Activated Alumina agent equivalent in meaning.
A kind of regeneration method of aluminium oxide defluorinating agent disclosed by the invention, key step have：1）, pickling:Aluminium oxide fluorine removal
Agent is after zinc electrolyte fluorine removal, other than having adsorbed a large amount of fluorine, while also having carried a part of zinc sulfate secretly, has caused the damage of zinc
It loses, and influences the desorption effect of next step fluorine.Therefore, dilute by being added during aluminium oxide defluorinating agent pulping and washing
Zinc is desorbed the mode of sulfuric acid, while controlling pH not less than 5.0 to guarantee the structure for not destroying defluorinating agent, and it is solid to obtain acid elution liquid
Mixed liquor is after filtering pickling slag；2）, alkali cleaning：By step 1）Obtained acid elution liquid consolidates the filtered pickling slag of mixed liquor,
Liquid alkaline washing is added, realizes the removing of fluorine, for alkali cleaning aluminium oxide or is alkali cleaning slag；3）, washing：To reduce step 2）Alkali cleaning slag
The content of alkalinity and fluorine increases by one of washing step to alkali cleaning slag.4）, pulp mend sour fluorine removal：For avoid a small amount of zinc through alkali cleaning,
Water-washing process is changed into zinc hydroxide, and package, blocking defluorinating agent adsorb duct, by step 3）Obtained washing slag is advanced in fluorine removal
In row slurrying process, a small amount of diluted acid is added to destroy the structure of zinc hydroxide, enhances the defluorination effect of regenerative aluminium oxide defluorinating agent.
The regenerated aluminium oxide defluorinating agent of method of the invention is used in this way, and the fluorine in zinc electrolyte can be reduced to 32mg/L from 500mg/L.
The defluorinating agent regeneration method is easy to operate, and zinc, fluorine desorption rate are high, and regenerability is good, and recycling number is high.
Embodiment 1：
To fail aluminium oxide defluorinating agent, i.e., it is molten that dilute sulfuric acid is added in the Defluorination of Formation Mater By Adsorption On Activated Alumina agent raw material after zinc electrolyte fluorine removal
Liquid controls dilution heat of sulfuric acid and aluminium oxide defluorinating agent raw material, under normal temperature conditions with liquid-solid ratio 3:1 carries out pickling, controls dilute sulphur
Acid solution is slowly added in 40min, and the terminal pH of the pickling solution after controlling pickling is 5.22, and acid elution liquid is made and mixes admittedly
Liquid is filtered into pickling slag；NaOH solution is added in pickling slag, the initial concentration for controlling NaOH solution is that 1.0mol/L carries out alkali
It washes, control alkali cleaning temperature is 65 DEG C -80 DEG C, time 40-60min, after filtering, obtains alkali cleaning slag；Alkali cleaning slag is subjected to water with water
It washes, washing time 30min, the wash-off rate of fluorine is up to 90.92%, and up to 90.12%, when pulping stage, which carries out mending acid, is removed for the wash-off rate of zinc
Fluorine, regenerative aluminium oxide defluorinating agent defluorinating agent further carry out pulp and mend sour fluorine removal, and mending dilute acid concentration used when acid is 0.6mol/
L；It in above-mentioned treatment process, is carried out under stirring, control stirring rate is 90-100r/min.At present embodiment
After reason, the solution of zinc sulfate of fluorine content 510mg/L can be down to 58mg/L.
In following embodiments except it is stated that in addition to, remaining undeclared place with above-described embodiment 1.
Embodiment 2：
Defluorinating agent fail under normal temperature conditions with liquid-solid ratio 5:1 carries out pickling, and terminal pH is 5.20, and alkali cleaning NaOH solution is initially dense
Degree is 1.2mol/L, and washing time 30min, for the wash-off rate of fluorine up to 93.38%, the wash-off rate of zinc regenerates defluorinating agent up to 92.09%
Sour fluorine removal is mended in pulp, the solution of zinc sulfate of fluorine content 510mg/L can be down to 41mg/L.
Embodiment 3：
Defluorinating agent fail under normal temperature conditions with liquid-solid ratio 8:1 carries out pickling, and terminal pH is 5.37, and alkali cleaning NaOH solution is initially dense
Degree is 1.2mol/L, and washing time 30min, for the wash-off rate of fluorine up to 98.59%, the wash-off rate of zinc regenerates defluorinating agent up to 96.87%
Sour fluorine removal is mended in pulp, the solution of zinc sulfate of fluorine content 510mg/L can be down to 32mg/L.
Reference examples 1：
Defluorinating agent fail first under the conditions of 60 DEG C with liquid-solid ratio 3:1 is washed, and alkali cleaning NaOH solution initial concentration is 1.0mol/
L, the wash-off rate of fluorine is up to 63.19%, and for the wash-off rate of zinc up to 53.18%, alkali cleaning slag is directly used in solution of zinc sulfate fluorine removal, fluorine content
140mg/L is down to from 510mg/L.
Reference examples 2：
Defluorinating agent fail under normal temperature conditions with liquid-solid ratio 5:1 carries out pickling, and terminal pH is 5.20, and alkali cleaning NaOH solution is initially dense
Degree is 1.2mol/L, and the wash-off rate of fluorine is up to 90.45%, and for the wash-off rate of zinc up to 91.52%, alkali cleaning slag is directly used in solution of zinc sulfate
Fluorine removal, fluorine content are down to 118mg/L from 510mg/L.
Reference examples 3：
Defluorinating agent fail under normal temperature conditions with liquid-solid ratio 8:1 carries out pickling, and terminal pH is 5.37, and alkali cleaning NaOH solution is initially dense
Degree is 1.2mol/L, and washing time 30min, for the wash-off rate of fluorine up to 98.59%, the wash-off rate of zinc regenerates defluorinating agent up to 96.87%
Direct pulp fluorine removal, can be down to 85mg/L for the solution of zinc sulfate of fluorine content 510mg/L.
Claims (5)
1. a kind of regeneration method of aluminium oxide defluorinating agent, to be regeneration for the Defluorination of Formation Mater By Adsorption On Activated Alumina agent after zinc electrolyte fluorine removal
Raw material, it is characterized in that comprising the technical steps that：
Pickling,
By the Defluorination of Formation Mater By Adsorption On Activated Alumina agent raw material after zinc electrolyte fluorine removal, it is slowly added to dilute acid soln during pulping and washing,
Pickling is carried out, pH >=5.0 of pickling solution are controlled, acid elution liquid is made and consolidates mixed liquor, filters, relieving haperacidity washery slag；
2）Alkali cleaning,
By 1）The filtered pickling slag of acid elution solid-liquid mixed liquor for walking preparation is added liquid alkaline and washes under conditions of certain temperature
It washs, replaces, filtering is separated by solid-liquid separation, and obtains alkali cleaning slag；
3）Washing,
To 2）It walks in the alkali cleaning slag being prepared and water is added, under agitation, washed, reduce step 2）The alkali of alkali cleaning slag
Property and fluorine content, be made as washing alkali cleaning slag；
4）Pulp, the sour fluorine removal of benefit, preparation, regeneration aluminium oxide defluorinating agent,
To 3）Suitable dilute acid soln is added in step washing alkali cleaning slag, carries out pulp processing under agitation, carries out at pulp
Dilute acid soln is added when reason, removes the zinc hydroxide of generation and removing is adsorbed in fluorine on aluminium oxide, filtering, filter residue, for regeneration
Aluminium oxide defluorinating agent.
2. a kind of regeneration method of aluminium oxide defluorinating agent according to claim 1, it is characterized in that step 1）Pickling, control liquid are solid
Mixed liquor mass ratio is 5-10：1；The diluted acid is dilute sulfuric acid, and control dilute sulfuric acid concentration is 0.5-1.0mol/L, when controlling pickling
The dilute acid soln addition time continues 15-20min, and pickling temperature is 25 DEG C -40 DEG C, time 30-60min.
3. a kind of regeneration method of aluminium oxide defluorinating agent according to claim 1, it is characterized in that step 2）Alkali cleaning, the lye
For NaOH solution, the NaOH solution concentration for controlling alkali cleaning is 1.0-1.8mol/L, 65 DEG C -80 DEG C of alkali cleaning temperature, time 40-
60min。
4. a kind of regeneration method of aluminium oxide defluorinating agent according to claim 1, it is characterized in that mending sour when institute when pulp is handled
It is 0.5-0.7mol/L with dilute acid concentration.
5. a kind of regeneration method of aluminium oxide defluorinating agent according to claim 1, it is characterized in that control 1）Pickling, 2）Alkali cleaning and
3）Washing, 4）Pulp when preparation, regeneration aluminium oxide defluorinating agent, carries out under stirring, and control stirring rate is 90-100r/
min。
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| CN201810813063.7A CN108889287B (en) | 2018-07-23 | 2018-07-23 | Regeneration method of aluminum oxide defluorinating agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111139367A (en) * | 2019-12-30 | 2020-05-12 | 江西赣锋循环科技有限公司 | Method for deeply removing fluorine from LiCl solution recovered from waste battery |
| CN114477405A (en) * | 2022-01-28 | 2022-05-13 | 湖南烯富环保科技有限公司 | Method for treating electrolytic aluminum ash solid waste and co-producing acid-resistant fluorine-fixing material and application |
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|---|---|---|---|---|
| CN102228746A (en) * | 2011-07-01 | 2011-11-02 | 德阳市南邡再生资源有限公司 | Method for removing fluorine from zinc sulfate solution with active alumina |
| CN102936656A (en) * | 2012-11-20 | 2013-02-20 | 东北大学 | Method for removing fluorine in bastnaesite sulfuric acid leaching liquid by aluminiferous adsorbing agent |
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2018
- 2018-07-23 CN CN201810813063.7A patent/CN108889287B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102228746A (en) * | 2011-07-01 | 2011-11-02 | 德阳市南邡再生资源有限公司 | Method for removing fluorine from zinc sulfate solution with active alumina |
| CN102936656A (en) * | 2012-11-20 | 2013-02-20 | 东北大学 | Method for removing fluorine in bastnaesite sulfuric acid leaching liquid by aluminiferous adsorbing agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111139367A (en) * | 2019-12-30 | 2020-05-12 | 江西赣锋循环科技有限公司 | Method for deeply removing fluorine from LiCl solution recovered from waste battery |
| CN114477405A (en) * | 2022-01-28 | 2022-05-13 | 湖南烯富环保科技有限公司 | Method for treating electrolytic aluminum ash solid waste and co-producing acid-resistant fluorine-fixing material and application |
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