CN105161788B - A kind of method that AGM partition boards are removed in lead-acid accumulator waste diachylon - Google Patents
A kind of method that AGM partition boards are removed in lead-acid accumulator waste diachylon Download PDFInfo
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- CN105161788B CN105161788B CN201510560666.7A CN201510560666A CN105161788B CN 105161788 B CN105161788 B CN 105161788B CN 201510560666 A CN201510560666 A CN 201510560666A CN 105161788 B CN105161788 B CN 105161788B
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention discloses a kind of methods that AGM partition boards are removed in lead-acid accumulator waste diachylon, belong to Lead-acid Battery Technology field, in the recovery stage for solving prior art accumulator, recycling crushing plant all carries out violence and disassembles, so that the technical issues of AGM partition boards and waste diachylon are difficult to detach, greatly reduce lead recovery.The present invention includes crushing lead-acid accumulator, drying, weighing, and determines the mass percent of AGM partition boards contained in waste diachylon；Then it adds in reaction kettle, adds in sodium hydroxide solution；After fully being reacted under conditions of stirring, reaction mass is taken out, carries out press filtration, separation of solid and liquid is completed, obtains filter cake and filtrate；Filter cake is washed with pure water, and the silicate of the lye in filter cake and generation is cleaned up, and is dried；Filtrate is washed with doctor solution, salts out silicic acid, five steps such as to recycle of alkali liquor recycle.
Description
Technical field
The invention belongs to Lead-acid Battery Technology fields, are related to removing AGM partition boards in a kind of lead-acid accumulator waste diachylon
Method.
Background technology
Superfine glass fibre partition board is commonly called as AGM partition boards.AGM partition boards are mainly the glass fibre using different decomposition degree, are pressed
It is fabricated according to different proportion using wet papermaking technology, as essential material in valve-regulated lead-acid battery, to electricity
Bring more benefit in pond.Analysing valve control type lead-acid accumulator battery is with the main function of AGM partition boards：(1) prevent positive/negative pole plate from contacting with each other
And internal short-circuit of battery occurs；(2) make accumulator close fit, reduce battery volume；(3) pole plate deformation, bending are prevented and is lived
Property substance comes off；(4) as the porous separator between pole plate, wherein the electrolyte of necessary amount can be stored, it is higher to ensure
Electric conductivity, meet the needs of cell reaction；(5) prevent some from the substance that battery is harmful to is migrated and being expanded by partition board
It dissipates；(6) oxygen cycle inside analysing valve control type lead-acid accumulator battery is realized.Therefore, AGM partition boards are referred to as the of analysing valve control type lead-acid accumulator battery
Tri-electrode.
But in the recovery stage of accumulator, need to recycle the lead in waste diachylon.In existing lead recycling side
In method, it is broadly divided into pyrogenic process and wet recycling process.In pyrogenic process recovery process, due to the presence of ultra-fine fibre glass, into
When row starts lead bullion melting, ultra-fine fibre glass will form a kind of eutectic with lead oxide, reduce the fusing point of its lead oxides, band
Carry out certain benefit.But in the subsequent electrorefining stage, it will the content of anode mud is substantially increased, increases electrolysis energy consumption,
Great difficulty is brought to the recycling of other noble metals.And in wet recycling process, due to the presence of ultra-fine fibre glass, master
It is SiO to want ingredient2, eutectic is formed in firing stage, increases its hardness, larger difficulty is brought to subsequent broken work,
Larger difficulty is brought to lead recovery process.And SiO2Bring the quality that will substantially reduce product into, will be to lead recovery process
Very big factor to affect.
In the recovery stage of existing accumulator, crushing plant is crushed substantially using violence, and AGM partition boards are as battery
A part by the broken of device for disassembling, along with AGM partition boards are in itself after the multiple charge and discharge cycles of battery, has changed
Its initial performance, causes AGM partition boards to become tiny cotton shape, is bundled together with waste diachylon, use general machinery
Method is difficult to be detached.For example the separation of AGM partition boards is carried out using experiment vibrating screen, it is general to carry out level-one vibrations, secondary shake
It is dynamic to obtain most of separation of AGM partition boards, but still greatly reduce lead containing more lead plaster in the AGM partition boards detached and return
Yield also brings larger negative effect to environment and production efficiency.
Invention content
The invention discloses a kind of methods that AGM partition boards are removed in lead-acid accumulator waste diachylon, can obtain more pure
Waste diachylon, and in process of production without waste water scrap lead generate, environmentally protective, energy saving economy.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：In a kind of lead-acid accumulator waste diachylon
Except the method for AGM partition boards, include the following steps successively：
Step 1: obtaining waste diachylon after lead-acid accumulator is crushed, is dried, waste diachylon is accurately weighed, is determined useless
The mass percent of contained AGM partition boards in old lead plaster；
Step 2: the waste diachylon in step 1 is added in reaction kettle, sodium hydroxide solution is added in；
Step 3: after unlatching reaction kettle, waste diachylon and sodium hydroxide solution fully react under conditions of stirring, turn off
Reaction kettle takes out reaction mass, carries out press filtration, completes separation of solid and liquid, obtains filter cake and filtrate；
Step 4: the filter cake that step 3 obtains is washed with pure water, by the lye in filter cake and the silicic acid of generation
Salt cleans up, drying, accurately determines the mass percent of AGM partition boards contained in filter cake；
Step 5: the filtrate that step 3 obtains is washed with doctor solution, silicic acid is salted out, recycle of alkali liquor is carried out
It recycles.
There are larger problem, existing non-maintaining lead for the recycling of China and countries in the world to maintenance-free lead accumulator at present
The partition board that acid accumulator uses is AGM ultra-fine fibre glasses, and in battery after hundreds of charge and discharge cycles, AGM partition boards go out
It is now stained with and pays and soften, lose original physical arrangement.And existing recycling crushing plant all carries out violence and disassembles, and is being crushed
Afterwards, AGM partition boards will become relatively thin, it is impossible to be detached, larger impact is brought to present lead recycling.
The present invention is raw material using common industrial chemicals, molten by the way that the AGM partition boards in existing waste diachylon are carried out
The method for solving separation carries out separation of solid and liquid, and so as to obtain more pure waste diachylon, obtained solid is washed to neutrality, into
The recycling of quadrat cream, filtrate then can be recycled, and extract useful silicate waste byproduct, to subsequent recycling band
Carry out larger economic and technical benefit.This method is easy to operate, and cycle supplement can be carried out to the lye after reaction, to lead plaster into
Divide and do not bring impurity, reliable in quality, while having carried out recycling to lye, without the discharge of sewage, effect on environment
It is small, great benefit, while reducing cost, energy conservation and environmental protection are brought to the recycling of lead-acid accumulator.In addition, the present invention passes through letter
Single easy method prepares the anode additive red lead that lead-acid accumulator can re-use, and can both reduce production cost,
Benefit can also be brought to the curing, chemical conversion and initial capacity of accumulator, lead-acid accumulator industry can combine itself practical feelings
Condition carries out large-scale production.
Preferably, in step 1, the quality percentage of AGM partition boards contained in waste diachylon is determined by following steps
Than：The waste diachylon accurately weighed is added in conical flask, the ammonium acetate solution of extra mass a concentration of 20% is added in, boils
15min, to remove the lead sulfate in waste diachylon；It after filter residue pure water washes clean, goes back in above-mentioned conical flask, adds in
Excessive salpeter solution and excessive hydrogen peroxide, the volume ratio of nitric acid and water is 1 in the salpeter solution:4, it boils, with removal
Lead oxide, lead, brown lead oxide and additives of lead-acid battery in waste diachylon, filtering, with pure water washing filter residue to lead
Until ion is washed totally；Filter residue after washing is transferred in crucible, crucible and filter residue are put into high temperature furnace together,
3h is dried under conditions of 800 DEG C；Crucible is removed, filter residue is transferred in drier and is cooled to room temperature, weighs filter residue quality, as
The mass percent of AGM partition boards contained in waste diachylon is calculated in the quality of AGM partition boards.The present invention is surveyed using physics and chemistry
The method of examination determines the mass percent of AGM partition boards contained in waste diachylon.
Preferably, in step 2, the mass concentration of sodium hydroxide solution is 30~40%.The lye of various concentration will shadow
The solid-to-liquid ratio of reaction is rung, different influences will be brought to reaction condition.For example concentration of lye is low, it is certain in the amount for adding in piece alkali
Under conditions of, the amount of the lye of addition will become more, to that will bring different degrees of influence on stirring and heating time in reaction.
Preferably, in step 2, add in AGM partition boards contained in sodium hydroxide solution and waste diachylon mole amount
The ratio between be 1:1~4.Lye and the equation of AGM partition boards reaction are as follows：
mSiO2+2NaOH—→Na2O·mSiO2+H2O
Since reaction product will have moisture generation, it will bring the decline of concentration of lye, therefore in reacting m value one
As control 0.5~2 be best.
Preferably, in step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle control
At 100~300 DEG C, pressure control controls in 80~300r/min, reaction time 1 system in 0.1~5Mpa, mixing speed control
~4h.
Further, in step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle
At 150~200 DEG C, pressure control is controlled in 0.2~0.4Mpa, mixing speed control in 150~200r/min, reaction time for control
System is in 1~2h.When pressure is mesolow, reaction has to react under conditions of pressure.Since the density of lead plaster is larger, make
With the stirring of more strength, material can uniformly be broken up, more can be with lye haptoreaction, the reaction time is longer, and reaction is got over
Completely, but for it is energy saving etc. the considerations of, the reaction time control it is more suitable in 1~2h.
Further, in step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle
At 250~300 DEG C, pressure control is controlled in 0.8~1Mpa, mixing speed control in 80~120r/min, reaction time for control
In 3~4h.
Further, in step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle
At 200~250 DEG C, pressure control is controlled in 0.6~0.8Mpa, mixing speed control in 100~200r/min, reaction time for control
System is in 2~3h.
Compared with prior art, it is an advantage of the invention that：The invention discloses in a kind of lead-acid accumulator waste diachylon
It is raw material using common industrial chemicals except the method for AGM partition boards, by the way that the AGM partition boards in existing waste diachylon are carried out
The method of separated and dissolved carries out separation of solid and liquid, so as to obtain more pure waste diachylon, subsequent recycling is brought larger
Economic and technical benefit.This method is easy to operate, can carry out cycle supplement to the lye after reaction, the ingredient of lead plaster is not brought
Impurity, reliable in quality, while having carried out recycling to lye, without the discharge of sewage, energy conservation and environmental protection.In addition, this hair
It is bright that the anode additive red lead that lead-acid accumulator can re-use is prepared by simple and practicable method, and can extract and have
Silicate waste byproduct can both reduce production cost, and the curing, chemical conversion and initial capacity of accumulator can also be brought
Benefit, lead-acid accumulator industry can combine own actual situation and carry out large-scale production.
The invention will be further described With reference to embodiment：
Specific embodiment
The embodiment of the method 1 of AGM partition boards is removed in a kind of lead-acid accumulator waste diachylon of the present invention, successively including following
Step：
Step 1: obtaining waste diachylon after lead-acid accumulator is crushed, is dried, waste diachylon is accurately weighed, is determined useless
The mass percent of contained AGM partition boards in old lead plaster；
The mass percent of AGM partition boards contained in waste diachylon is determined by following steps：By what is accurately weighed
Waste diachylon is added in conical flask, is added in the ammonium acetate solution of extra mass a concentration of 20%, is boiled 15min, waste and old to remove
Lead sulfate in lead plaster；After filter residue pure water washes clean, go back in above-mentioned conical flask, add in excessive salpeter solution and
Excessive hydrogen peroxide, the volume ratio of nitric acid and water is 1 in the salpeter solution:4, it boils, to remove the oxidation in waste diachylon
Lead, lead, brown lead oxide and additives of lead-acid battery, filtering are washed to lead ion with pure water washing filter residue and are totally
Only；Filter residue after washing is transferred in crucible, crucible and filter residue are put into high temperature furnace together, is dried under conditions of 800 DEG C
3h；Crucible is removed, filter residue is transferred in drier and is cooled to room temperature, weighs the quality of filter residue quality, as AGM partition boards, is calculated
Obtain the mass percent of AGM partition boards contained in waste diachylon.In the present embodiment using waste and old lead acid accumulator lead plaster come
Derived from Anhui great Hua Co., Ltds, waste diachylon chemical composition stability obtains AGM partition boards in waste diachylon by measure and calculation
Mass percent is 2~10%, and moisture is 5~25%.
Step 2: the waste diachylon in step 1 is added in reaction kettle, sodium hydroxide solution is added in；The hydrogen-oxygen added in
The mass concentration for changing sodium solution is 30~40%, and addition sodium hydroxide solution rubs with AGM partition boards contained in waste diachylon
The ratio between your amount is 1:1~4.The mass concentration of sodium hydroxide solution can be 5~60%, it is contemplated that reaction condition band
Carry out different influences, more preferably to select when the mass concentration of sodium hydroxide solution is 30~40%.
Step 3: after unlatching reaction kettle, waste diachylon and sodium hydroxide solution fully react under conditions of stirring, turn off
Reaction kettle takes out reaction mass, carries out press filtration, completes separation of solid and liquid, obtains filter cake and filtrate；
In the reaction process, at 100~150 DEG C, pressure is controlled in 0.1~2Mpa, mixing speed for temperature in the kettle control
Control is controlled in 100~200r/min, reaction time in 2~4h.
Step 4: the filter cake that step 3 obtains is washed with pure water, by the lye in filter cake and the silicic acid of generation
Salt cleans up, drying, and the mass percent for accurately determining AGM partition boards contained in filter cake is 0.3%；It is namely waste and old
The AGM partition boards being measured to after AGM partition boards are removed in lead plaster and participate in content.
Step 5: the filtrate that step 3 obtains is washed with doctor solution, silicic acid is salted out, recycle of alkali liquor is carried out
It recycles.
The embodiment of the method 2 of AGM partition boards is removed in a kind of lead-acid accumulator waste diachylon of the present invention, step is with implementing
Example 1 is substantially similar, difference lies in：
In step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle is controlled 100
~150 DEG C, pressure control is controlled in 200~300r/min, reaction time in 1~2h in 2~3Mpa, mixing speed control.
In step 4, the mass percent for accurately determining AGM partition boards contained in filter cake is 0.26%.
The embodiment of the method 3 of AGM partition boards is removed in a kind of lead-acid accumulator waste diachylon of the present invention, step is with implementing
Example 1 is substantially similar, difference lies in：
In step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle is controlled 150
~200 DEG C, pressure control in 0.2~0.4Mpa, mixing speed control in 150~200r/min, reaction time control 1~
2h。
In step 4, the mass percent for accurately determining AGM partition boards contained in filter cake is 0.12%.
The embodiment of the method 4 of AGM partition boards is removed in a kind of lead-acid accumulator waste diachylon of the present invention, step is with implementing
Example 1 is substantially similar, difference lies in：
In step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle is controlled 250
~300 DEG C, pressure control is controlled in 80~120r/min, reaction time in 3~4h in 0.8~1Mpa, mixing speed control.
In step 4, the mass percent for accurately determining AGM partition boards contained in filter cake is 0.15%.
The embodiment of the method 5 of AGM partition boards is removed in a kind of lead-acid accumulator waste diachylon of the present invention, step is with implementing
Example 1 is substantially similar, difference lies in：
In step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle is controlled 200
~250 DEG C, pressure control in 0.6~0.8Mpa, mixing speed control in 100~200r/min, reaction time control 2~
3h。
In step 4, the mass percent for accurately determining AGM partition boards contained in filter cake is 0.08%.
The embodiment of the method 6 of AGM partition boards is removed in a kind of lead-acid accumulator waste diachylon of the present invention, step is with implementing
Example 1 is substantially similar, difference lies in：
In step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle is controlled 200
~300 DEG C, pressure control is controlled in 200~300r/min, reaction time in 1~2h in 3~5Mpa, mixing speed control.
In step 4, the mass percent for accurately determining AGM partition boards contained in filter cake is 0.24%.
Contained by after removing AGM partition boards in the reaction condition of above-described embodiment 1 to 6 and final waste diachylon
The mass percent of AGM partition boards is compared as it can be seen that the mass percent of contained AGM partition boards is by original 2~10% in waste diachylon
Drop to 0.5% hereinafter, when the pressure in reaction kettle is less than 1Mpa, content even drops to less than 0.2%.Also, it stirs
Mix speed it is higher when, required reaction time shortens, and illustrates that the density of lead plaster is larger, can general using the stirring of more strength
Material is uniformly broken up, and is more advantageous to reacting.In the waste diachylon of embodiment 3 to 5 it can be seen from the data of embodiment 1 to 6
The mass percent of contained AGM partition boards drops to 0.2% hereinafter, the mixing speed still in embodiment 4,5 is relatively low, during reaction
Between need the long period, comprehensive various aspects factor considers, embodiment 3 is more preferably.
Technical characteristic the foregoing is merely specific embodiments of the present invention, but the present invention is not limited thereto, Ren Heben
The technical staff in field in the field of the invention, all cover among the scope of the claims of the present invention by the variation or modification made.
Claims (5)
1. the method for AGM partition boards is removed in a kind of lead-acid accumulator waste diachylon, it is characterised in that：Include the following steps successively：
Step 1: obtaining waste diachylon after lead-acid accumulator is crushed, is dried, waste diachylon is accurately weighed, determines waste and old lead
The mass percent of contained AGM partition boards in cream；
The mass percent of AGM partition boards contained in waste diachylon is determined by following steps：It is waste and old by what is accurately weighed
Lead plaster is added in conical flask, is added in the ammonium acetate solution of extra mass a concentration of 20%, 15min is boiled, to remove waste diachylon
In lead sulfate；After filter residue pure water washes clean, go back in above-mentioned conical flask, add in excessive salpeter solution and excess
Hydrogen peroxide, the volume ratio of nitric acid and water is 1 in the salpeter solution:4, boil, with remove the lead oxide in waste diachylon,
Lead, brown lead oxide and additives of lead-acid battery, filtering, with pure water washing filter residue to lead ion be washed it is clean until；
Filter residue after washing is transferred in crucible, crucible and filter residue are put into high temperature furnace together, 3h is dried under conditions of 800 DEG C；
Crucible is removed, filter residue is transferred in drier and is cooled to room temperature, the quality of filter residue quality, as AGM partition boards is weighed, is calculated
The mass percent of contained AGM partition boards in waste diachylon；
Step 2: the waste diachylon in step 1 is added in reaction kettle, sodium hydroxide solution is added in；
Step 3: after unlatching reaction kettle, waste diachylon and sodium hydroxide solution fully react under conditions of stirring, turn off reaction
Kettle takes out reaction mass, carries out press filtration, completes separation of solid and liquid, obtains filter cake and filtrate；
Step 4: the filter cake that step 3 obtains is washed with pure water, the silicate of the lye in filter cake and generation is clear
Wash clean is dried, and accurately determines the mass percent of AGM partition boards contained in filter cake；
Step 5: the filtrate that step 3 obtains is washed with doctor solution, silicic acid is salted out, recycle of alkali liquor is recycled
It utilizes；
In step 2, the mass concentration of sodium hydroxide solution is 30~40%；
In step 2, add in AGM partition boards contained in sodium hydroxide solution and waste diachylon mole the ratio between amount be 1:1~
4。
2. the method for AGM partition boards is removed in a kind of lead-acid accumulator waste diachylon as described in claim 1, it is characterised in that：
In step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle is controlled at 100~300 DEG C,
Pressure control is controlled in 80~300r/min, reaction time in 1~4h in 0.1~5Mpa, mixing speed control.
3. the method for AGM partition boards is removed in a kind of lead-acid accumulator waste diachylon as claimed in claim 2, it is characterised in that：
In step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle is controlled at 150~200 DEG C,
Pressure control is controlled in 150~200r/min, reaction time in 1~2h in 0.2~0.4Mpa, mixing speed control.
4. the method for AGM partition boards is removed in a kind of lead-acid accumulator waste diachylon as claimed in claim 2, it is characterised in that：
In step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle is controlled at 250~300 DEG C,
Pressure control is controlled in 80~120r/min, reaction time in 3~4h in 0.8~1Mpa, mixing speed control.
5. the method for AGM partition boards is removed in a kind of lead-acid accumulator waste diachylon as claimed in claim 2, it is characterised in that：
In step 3, in reaction kettle in waste diachylon and the reaction process of sodium hydroxide solution, temperature in the kettle is controlled at 200~250 DEG C,
Pressure control is controlled in 100~200r/min, reaction time in 2~3h in 0.6~0.8Mpa, mixing speed control.
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| CN102410968A (en) * | 2011-08-11 | 2012-04-11 | 江苏理士电池有限公司 | Analytical method for content of short fibers in pole plate lead paste of lead-acid battery |
| CN102689922A (en) * | 2011-03-24 | 2012-09-26 | 杨春晓 | Lead compound nano-powder preparation method for recovery and manufacture of lead-acid battery |
| CN103050745A (en) * | 2013-01-07 | 2013-04-17 | 华中科技大学 | Pretreatment method for lead plaster of waste lead-acid accumulators |
| WO2013142904A1 (en) * | 2012-03-30 | 2013-10-03 | Sita Australia Pty Ltd | Processing of mixed waste to remove non-compost compatible materials |
| CN103509949A (en) * | 2012-06-15 | 2014-01-15 | 杨春晓 | Methods and equipment for recovering waste diachylon by wet method and manufacturing electrode active material of high performance lead acid battery by wet method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102689922A (en) * | 2011-03-24 | 2012-09-26 | 杨春晓 | Lead compound nano-powder preparation method for recovery and manufacture of lead-acid battery |
| CN102410968A (en) * | 2011-08-11 | 2012-04-11 | 江苏理士电池有限公司 | Analytical method for content of short fibers in pole plate lead paste of lead-acid battery |
| WO2013142904A1 (en) * | 2012-03-30 | 2013-10-03 | Sita Australia Pty Ltd | Processing of mixed waste to remove non-compost compatible materials |
| CN103509949A (en) * | 2012-06-15 | 2014-01-15 | 杨春晓 | Methods and equipment for recovering waste diachylon by wet method and manufacturing electrode active material of high performance lead acid battery by wet method |
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