CN110182840A - Move back tin waste treatment processes - Google Patents
Move back tin waste treatment processes Download PDFInfo
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- CN110182840A CN110182840A CN201910550124.XA CN201910550124A CN110182840A CN 110182840 A CN110182840 A CN 110182840A CN 201910550124 A CN201910550124 A CN 201910550124A CN 110182840 A CN110182840 A CN 110182840A
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- Prior art keywords
- tin
- slurry
- filtrate
- tin waste
- treatment processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses one kind to move back tin waste treatment processes, includes the following steps: to obtain solid reactant to the progress pre-treatment of tin waste is moved back；Solid reactant, water and enough highly basic are mixed to form slurry, slurry is heated to boiling and maintain fluidized state until sufficiently reaction；Enough water is added into the slurry after abundant reaction, is filtered after dissolution is sufficiently stirred, obtains the first filtrate and the first filter residue, the first filtrate is stannate solutions product.This tin waste treatment processes of moving back are when tin waste is moved back in processing, it is only necessary to be heated to boiling to slurry, can be completed without roasting and move back tin treatment of wastes produced, significantly reduce energy consumption, the pollution to environment is effectively reduced in effective reduced cost simultaneously.
Description
Technical field
The present invention relates to scrap concrete process fields, move back tin waste treatment processes more particularly to one kind.
Background technique
It moves back tin waste and is mainly derived from printed circuit board industry, generally include tin-stripping wastewater and tin mud.Tin-stripping wastewater generates
Amount is big, and Theil indices are higher in waste, and Theil indices commonly reach 50g/L~100g/L, utility value with higher, contains in waste
There are a certain amount of copper (about 10g/L) and a certain amount of acid (content up to 20%~30%).Tin mud is stripped from PCB industry coating
The slot slag and wastewater treatment sludge generated in the process, stanniferous amount are 10%~20%.
Currently, handle to obtain solid dregs generally by precipitation and separation to moving back tin treatment of wastes produced, then by solid dregs,
Tin mud and alkali etc. carry out calcination process, last water process recycling and removal of impurities after mixing.
However, calcination process energy consumption is higher, not only increases cost, be also unfavorable for environmental protection.
Summary of the invention
Based on this, it is necessary to provide and a kind of not need to carry out calcination process to move back tin waste treatment processes.
One kind moving back tin waste treatment processes, includes the following steps:
Pre-treatment is carried out to tin waste is moved back, obtains solid reactant；
The solid reactant, water and enough highly basic are mixed to form slurry, the slurry is heated to boiling simultaneously
Fluidized state is maintained until sufficiently reaction, wherein the solid-to-liquid ratio of the slurry is 0.2~4:1；
Enough water is added into the slurry after abundant reaction, is filtered after dissolution is sufficiently stirred, obtains the first filtrate
With the first filter residue, first filtrate is stannate solutions product.
This tin waste treatment processes of moving back are when tin waste is moved back in processing, it is only necessary to be heated to boiling to slurry, be not necessarily to
Roasting, which can be completed, moves back tin treatment of wastes produced, significantly reduces energy consumption, and the dirt to environment is effectively reduced in effective reduced cost simultaneously
Dye；In addition, the solid reactant under fluidized state in slurry can react more abundant, it is also beneficial to move back the tin in tin waste
Recycling, relative to traditional technique, the rate of recovery is higher.
Detailed description of the invention
Fig. 1 is the process flow chart for moving back tin waste treatment processes of an embodiment.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to implementation of the invention
Mode is further described.
The invention discloses one kind to move back tin waste treatment processes, includes the following steps:
S10, to move back tin waste carry out pre-treatment, obtain solid reactant.
In general, moving back tin waste includes tin-stripping wastewater and tin mud.
When to move back tin waste be tin-stripping wastewater, pre-treatment is carried out to tin waste is moved back, obtains the operation of solid reactant are as follows: to moving back
It is 1~3 that sodium bicarbonate or sodium carbonate are added in tin waste water to pH, then adds enough organic polymer coargulators and sufficiently reacts
After filter, the filter residue obtained after filtering is solid reactant.
PH in tin-stripping wastewater is adjusted using sodium carbonate, the dosage of sodium carbonate can be reduced.
Preferably, organic polymer coargulator is polyacrylamide.
Preferably, the adding proportion of polyacrylamide is 0.05wt%~0.5wt%.
Preferably, the carbon dioxide gas generated when tin-stripping wastewater and sodium bicarbonate or sodium carbonate react can gather up
Come, to be used for subsequent reactions.
Move back tin waste be tin-stripping wastewater and tin mud when, solid reactant be filter residue and tin mud mixture.
In a preferred embodiment, further include the operation that filtrate is handled as follows: being evaporated after filtrate is purified
Concentration, obtains salt-cake.Purification run can be completed by purification device.Obtained salt-cake can be handled directly, it is preferred that salt-cake
It needs to process again after roasting.
S20, the solid reactant by S10 is obtained, water and enough highly basic are mixed to form slurry, and slurry is heated to boiling
Fluidized state is risen and maintained until sufficiently reaction.
Preferably, the solid-to-liquid ratio of slurry is 0.2~4:1.The solid-to-liquid ratio of slurry is 0.2~4:1, slurry can be maintained to be in
Semisolid semi-liquid stage, so that slurry can boil, so that solid reactant and highly basic can sufficiently react.
It is furthermore preferred that the solid-to-liquid ratio of slurry is 0.4~2:1.
Particularly preferred, the solid-to-liquid ratio of slurry is 0.8~1.2:1.
In the application, the solid-to-liquid ratio of slurry is the weight of all solids ingredient and the ratio with the weight of water in slurry.
Preferably, highly basic is liquid sodium hydroxide (for example, concentration is 40wt%) or liquid potassium hydroxide.Liquid highly basic is just
In being uniformly mixed, also avoid causing reaction not carrying out sufficiently since solid dissolution is insufficient.
Slurry is heated to boiling and maintains fluidized state until in the operation sufficiently reacted, the temperature of slurry under fluidized state
Degree is 105 DEG C~120 DEG C, and the time sufficiently reacted is 1h~5h.
According to the difference of the proportion of components various in slurry, the temperature under fluidized state can be slightly different, and maintain 1h~5h
It can guarantee the abundant progress of reaction.
By the operation of S20, the α metastannic acid for being not readily dissolved in alkali and β metastannic acid can be made to be converted into water-soluble tin
Hydrochlorate.
It further include that will consolidate in S20 before solid reactant, water and enough highly basic are mixed to form the operation of slurry
The dry operation of precursor reactant object.Due to provide enough highly basic, it is therefore desirable to be carried out according to the actual content of solid reactant
Compatibility, it is before mixing that solid reactant is dry, it is indispensable when for quantitative compatibility.But if not considering compatibility,
It can also be without drying, the highly basic of excessive addition.
In general, it is controlled according to the ratio between amount of substance of tin atom and hydroxide ion in 1: 4~10 ranges when compatibility
It is interior.
S30, enough water is added into the slurry after the abundant reaction that S20 is obtained, filters, obtains after dissolution is sufficiently stirred
First filtrate and the first filter residue.
Preferably, the volume ratio of the slurry sufficiently after reaction and water can be 1:3~10.The additive amount of water is not special
It is required that stannate can sufficiently be dissolved by being generally subject to.
It further include roast to the first filter residue the operation of simultaneously safety dumping after obtaining the first filter residue in S30.
First filtrate obtained in S30 is stannate solutions product, after which can continue continuation
Continuous processing can also be directly over purification process and obtain metastannic acid product and stannic oxide product.
Operation to stannate solutions purifying products are as follows: successively the first filtrate is evaporated, is concentrated, is crystallized, clean with
And it is dry, obtain the operation of stannate solid product.
S40, be passed through working gas into the first filtrate that S30 is obtained, filtered after sufficiently reacting, obtain the second filtrate and
Second filter residue.
Working gas is carbon dioxide gas or the mixed gas containing carbon dioxide.
Preferably, working gas can in S10 step, what tin-stripping wastewater and sodium bicarbonate or sodium carbonate generated when reacting
Carbon dioxide gas.
Preferably, S40 further includes being incorporated into the second filtrate after obtaining the second filtrate and moving back progress pre-treatment in tin waste
Operation.
S50, the second filter residue for obtaining S40 are dry after cleaning up, and obtain metastannic acid solid product.
Obtained metastannic acid solid product has been used directly for industry.
Preferably, S50 further includes roasting, obtaining to metastannic acid solid product after obtaining metastannic acid solid product
The operation of stannic oxide product.
This tin waste treatment processes of moving back are when tin waste is moved back in processing, it is only necessary to be heated to boiling to slurry, be not necessarily to
Roasting, which can be completed, moves back tin treatment of wastes produced, significantly reduces energy consumption, and the dirt to environment is effectively reduced in effective reduced cost simultaneously
Dye；In addition, the solid reactant under fluidized state in slurry can react more abundant, it is also beneficial to move back the tin in tin waste
Recycling, relative to traditional technique, the rate of recovery is higher.
It is below specific embodiment
For the tin-stripping wastewater handled in specific embodiment by circuit board factory, the content of each component in tin-stripping wastewater is as follows:
| Main component | Sn | HNO3 | Fe | Cu |
| Content: g/L | 68.5 | 213.6 | 3.6 | 8.2 |
Embodiment 1
The step for the treatment of process of the tin-stripping wastewater of the present embodiment, is as follows:
It is 2 that sodium bicarbonate is added into tin-stripping wastewater to pH, collects the carbon dioxide of generation as process gas, then presses
Polyacrylamide is added according to the mass ratio of 1:1000, is sufficiently filtered after reaction, the filter residue obtained after filtering is solid reactant,
Then solid reactant is dried.
By solid reactant, water and the liquid sodium hydroxide (40wt%) after drying according to mass ratio be 100:70:150
(solid-to-liquid ratio 1:1) is mixed to form slurry, and slurry is heated to boiling and maintains fluidized state 2h.
The water of 5 times of volumes is added into the slurry after abundant reaction, is filtered after dissolution is sufficiently stirred, retains the first filtrate.
It is passed through working gas into the first filtrate, is filtered after sufficiently reacting, the second filter residue is retained.
It is dry after second filter residue is cleaned up, obtain metastannic acid solid product.
Embodiment 2
The step for the treatment of process of the tin-stripping wastewater of the present embodiment, is as follows:
It is 1 that sodium bicarbonate is added into tin-stripping wastewater to pH, collects the carbon dioxide of generation as process gas, then presses
Polyacrylamide is added according to the mass ratio of 5:1000, is sufficiently filtered after reaction, the filter residue obtained after filtering is solid reactant,
Then solid reactant is dried.
By solid reactant, water and the liquid sodium hydroxide (40wt%) after drying according to mass ratio be 100:110:
150 are mixed to form slurry (solid-to-liquid ratio 0.8:1), and slurry is heated to boiling and maintains fluidized state 1h.
The water of 3 times of volumes is added into the slurry after abundant reaction, is filtered after dissolution is sufficiently stirred, retains the first filtrate.
It is passed through working gas into the first filtrate, is filtered after sufficiently reacting, the second filter residue is retained.
It is dry after second filter residue is cleaned up, obtain metastannic acid solid product.
Embodiment 3
The step for the treatment of process of the tin-stripping wastewater of the present embodiment, is as follows:
It is 3 that sodium carbonate is added into tin-stripping wastewater to pH, collects the carbon dioxide of generation as process gas, then according to
The mass ratio of 0.5:1000 adds polyacrylamide, sufficiently filters after reaction, and the filter residue obtained after filtering is solid reactant,
Then solid reactant is dried.
By solid reactant, water and the liquid sodium hydroxide (40wt%) after drying according to mass ratio be 100:43.3:
150 are mixed to form slurry (solid-to-liquid ratio 1.2:1), and slurry is heated to boiling and maintains fluidized state 5h.
The water of 8 times of volumes is added into the slurry after abundant reaction, is filtered after dissolution is sufficiently stirred, retains the first filtrate.
It is passed through working gas into the first filtrate, is filtered after sufficiently reacting, the second filter residue is retained.
It is dry after second filter residue is cleaned up, obtain metastannic acid solid product.
Comparative example
The step for the treatment of process of the tin-stripping wastewater of this comparative example, is as follows:
Will it is dry made from embodiment 1 after solid reactant, water and sodium hydroxide according to mass ratio be 100:50:60
Mixing, heats the mixture to 200 DEG C of roasting 2h.
The water of 5 times of volumes is added into the slurry after abundant reaction, is filtered after dissolution is sufficiently stirred, retains the first filtrate.
It is passed through working gas obtained in embodiment 1 into the first filtrate, is filtered after sufficiently reacting, retains the second filter
Slag.
It is dry after second filter residue is cleaned up, obtain metastannic acid solid product.
Solid reactant after the drying that embodiment 1 is obtained carries out Theil indices measurement, then to first that embodiment 1 obtains
The first filtrate that filtrate and comparative example 1 obtain carries out tin element assay respectively, in conjunction with as a result, it has been found that embodiment 1 obtain
The leaching rate of tin element in one filtrate is about 96.8%, and the leaching rate of the tin element in the first filtrate that comparative example obtains is about
It is 90%.
It can be seen that the boiling reaction in embodiment 1 has the leaching rate of tin element under same experimental condition
Biggish promotion has biggish industrial application value.
Only several embodiments of the present invention are expressed for embodiment described above, and the description thereof is more specific and detailed, but
It cannot be construed as a limitation to the scope of the present invention.It should be pointed out that for the ordinary skill people of this field
For member, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to of the invention
Protection scope.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. one kind moves back tin waste treatment processes, which comprises the steps of:
Pre-treatment is carried out to tin waste is moved back, obtains solid reactant；
The solid reactant, water and enough highly basic are mixed to form slurry, the slurry is heated to boiling and be maintained
Fluidized state is until sufficiently reaction, wherein the solid-to-liquid ratio of the slurry is 0.2~4:1；And
Enough water is added into the slurry after abundant reaction, is filtered after dissolution is sufficiently stirred, obtains the first filtrate and the
One filter residue, first filtrate are stannate solutions product.
2. according to claim 1 move back tin waste treatment processes, which is characterized in that further include to first filtrate successively
It is evaporated, is concentrated, crystallizes, cleans and dries, obtain the operation of stannate solid product.
3. according to claim 1 move back tin waste treatment processes, which is characterized in that the tin waste that moves back includes moving back tin to give up
Water；
Described pair is moved back tin waste and carries out pre-treatment, obtains the operation of solid reactant are as follows: add carbonic acid in Xiang Suoshu tin-stripping wastewater
Hydrogen sodium or sodium carbonate are 1~3 to pH, then add enough organic polymer coargulators and filter after sufficiently reacting, after filtering
To filter residue be the solid reactant.
4. according to claim 3 move back tin waste treatment processes, which is characterized in that the organic polymer coargulator is poly-
Acrylamide；
The tin waste that moves back further includes tin mud, and the solid reactant is the mixture of the filter residue and the tin mud.
5. according to claim 3 move back tin waste treatment processes, which is characterized in that further include as follows to filtrate progress
The operation of processing: it will be concentrated by evaporation after filtrate purification, obtain salt-cake.
6. according to claim 1 move back tin waste treatment processes, which is characterized in that further include by the solid reaction
Object, water and enough highly basic are mixed to form before the operation of slurry, by the operation that the solid reactant is dry.
7. according to claim 1 move back tin waste treatment processes, which is characterized in that the highly basic be liquid sodium hydroxide or
Liquid potassium hydroxide；
The slurry is heated to boiling and maintains fluidized state until in the operation sufficiently reacted, it is described under the fluidized state
The temperature of slurry is 105 DEG C~120 DEG C, and the time sufficiently reacted is 1h~5h.
8. according to claim 1, moving back tin waste treatment processes described in any one of 3~7, which is characterized in that described in obtaining
Further include operating as follows after first filtrate:
It is passed through working gas into first filtrate, is filtered after sufficiently reacting, the second filtrate and the second filter residue are obtained,
In, the working gas is carbon dioxide gas or the mixed gas containing carbon dioxide；And
It is dry after second filter residue is cleaned up, obtain metastannic acid solid product.
9. according to claim 8 move back tin waste treatment processes, which is characterized in that further include to obtain the metastannic acid solid
After body product, the metastannic acid solid product is roasted, the operation of stannic oxide product is obtained；
The working gas is the tin-stripping wastewater and sodium bicarbonate or the gas that sodium carbonate reaction generates.
10. according to claim 8 move back tin waste treatment processes, which is characterized in that further include obtaining first filter residue
Afterwards, roast to first filter residue operation of simultaneously safety dumping；
It further include that second filtrate is incorporated into the behaviour for moving back progress pre-treatment in tin waste after obtaining second filtrate
Make.
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|---|---|---|---|---|
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