CN104098076A - Method for reclaiming phosphoric acid and aluminium phosphate in formation waste liquid - Google Patents
Method for reclaiming phosphoric acid and aluminium phosphate in formation waste liquid Download PDFInfo
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- CN104098076A CN104098076A CN201410364903.8A CN201410364903A CN104098076A CN 104098076 A CN104098076 A CN 104098076A CN 201410364903 A CN201410364903 A CN 201410364903A CN 104098076 A CN104098076 A CN 104098076A
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- phosphoric acid
- waste liquid
- aluminum phosphate
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- aluminium phosphate
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Abstract
The invention belongs to a chemical engineering production processing technique and particularly relates to a method for reclaiming phosphoric acid and aluminium phosphate in formation waste liquid. The method comprises the following steps: adding a flocculating agent in the formation waste liquid, standing, filtering, removing ions from the filtrate to obtain the phosphoric acid solution, and drying the filter cake to obtain solid aluminium phosphate, so that both phosphoric acid and aluminium phosphate can be recovered. According to the invention, while phosphoric acid and aluminium phosphate are separated and recovered from the formation waste liquid, the purity of the recovered phosphoric acid is guaranteed. By adopting the method, the discharge and the control cost of waste phosphoric acid are reduced, and the manufacturing cost is lowered for formation enterprises.
Description
Technical field
The invention belongs to a kind of chemical technology field, be specifically related to a kind of recovery and change into the method for phosphoric acid and aluminum phosphate in waste liquid.
Background technology
Along with the develop rapidly of electronic industry, aluminium electrolutic capacitor more and more applies in life, work, a requisite link in capacitor fabrication process and change into production, change in production process and with the phosphoric acid of capacitor stage purity, oxide film is carried out to Passivation Treatment in a large number, prevent aluminum foil oxidation film and water generation hydration, the work-ing life of reduce leakage current, improving product.In formation process, constantly enter along with aluminum ions, thereby cause the effective concentration of phosphoric acid to decline, passivation effect weakens, and namely said tank liquor is aging, can not continue to use, and must constantly add new phosphoric acid solution.
But the waste and old waste liquid that changes into contains a large amount of phosphoric acid and aluminum phosphate, the domestic enterprise that changes into adopts emission treatment mostly at present, causes the wasting of resources and a large amount of environmental protection treatment expenses.
At present treating method generally adopts waste collection-add the mode processing that alkali neutralization-sedimentation processing-press filtration-waste residue is transported outward, and processing cost is high, poor effect, the problem such as uneconomical economically.
Summary of the invention
The object of the invention is to provide a kind of recovery to change into the method for phosphoric acid and aluminum phosphate in waste liquid.The method can separate the phosphoric acid and the aluminum phosphate that change in waste liquid efficiently, removes the foreign ions such as aluminum ion free in phosphoric acid, reclaims phosphoric acid.
Technical problem to be solved by this invention is to provide a kind of recovery and changes into the method for phosphoric acid and aluminum phosphate in waste liquid.The method comprises the following steps: add flocculation agent changing in waste liquid, staticly settle rear filtration, collect filtrate, remove filtrate intermediate ion and obtain phosphoric acid solution, filtration cakes torrefaction obtains aluminum phosphate solid.
Preferably, in aforesaid method, by weight, the add-on of flocculation agent accounts for and changes into 0.01～1% of waste liquid.
Preferably, in aforesaid method, described flocculation agent is polyacrylamide.
Preferably, in aforesaid method, time of repose is 5～10h.
Preferably, in aforesaid method, described is dried as dry 1～3h at 70～150 DEG C.
Preferably, in aforesaid method, described filtration adopts in millipore filtration, activated carbon filtration or multi-medium filtering any one.
Further, in aforesaid method, described multimedium is quartz sand, hard coal, gac, magnetite, opens up at least two kinds in garnet, pottery, baton round.
Preferably, in aforesaid method, adopt anion and cation exchange membrane method, reverse osmosis membrane processing method or diffusive dialysis method to remove the ion in filtrate.
The inventive method has thoroughly solved the recycling problem that changes into phosphoric acid in industry waste liquid, can from change into waste liquid, reclaim efficiently aluminum phosphate and phosphoric acid, the method production efficiency is high, cost recovery is low, save a large amount of phosphoric acid use costs for changing into produce, reduced the quantity discharged of phosphorus content refuse and a large amount of environment protection treating expenses.Adopt the inventive method, make to change into phosphoric acid recovery utilization rate in waste liquid and reach more than 80%, the purity of the aluminum phosphate pressed powder of recovery reaches 95% left and right.Utilize present method that phosphoric acid use cost has been declined more than 30%, aluminum phosphate pressed powder has also been created extra value, has reached desired result.
Embodiment
Recovery changes into a method for phosphoric acid and aluminum phosphate in waste liquid, comprises the following steps: add flocculation agent changing in waste liquid, staticly settle rear filtration, collect filtrate, remove filtrate intermediate ion and obtain phosphoric acid solution, filtration cakes torrefaction obtains aluminum phosphate solid.
Preferably, in aforesaid method, for precipitate phosphoric acid aluminium well, by weight, the add-on of flocculation agent accounts for and changes into 0.01～1% of waste liquid.
Preferably, in aforesaid method, described flocculation agent is polyacrylamide.
Preferably, in aforesaid method, described time of repose is 5～10h.
Preferably, in aforesaid method, described is dried as dry 1～3h at 70～150 DEG C.
Preferably, in aforesaid method, described filtration adopts in millipore filtration, activated carbon filtration or multi-medium filtering any one.
Further, in aforesaid method, described multimedium is quartz sand, hard coal, gac, magnetite, opens up at least two kinds in garnet, pottery, baton round.
Preferably, in aforesaid method, adopt anion and cation exchange membrane method, reverse osmosis membrane processing method or diffusive dialysis method to remove the ion in filtrate.
Concrete, in aforesaid method, changing into phosphoric acid concentration in waste liquid is 0.3～0.8mol/L, aluminum phosphate concentration is 10～40g/L.
The flocculation agent adding in the present invention carries out flocculation sediment to the aluminum phosphate changing in waste liquid, and when the concentration of aluminum phosphate is high, flocculation agent can be suitably more; When the concentration of aluminum phosphate is low, flocculation agent can suitably lack.Change in enterprise field, the general concentration that changes into phosphoric acid in waste liquid of collecting is 0.3～0.8mol/L, and aluminum phosphate concentration is 10～40g/L.Do not waste again the raw material of flocculation agent for precipitate phosphoric acid aluminium well, can correspondingly add and account for the flocculation agent that changes into waste liquid weight 0.01～1%.
In the art, the treating method that changes into waste liquid generally adopts the method for throwing alkali neutralization, anaerobism, oxygen consumption bacterium and process qualified discharge, does not recycle phosphoric acid in waste liquid etc.Prior art is rare to changing into reporting for work of phosphoric acid recycling in waste liquid.The present inventor finds through research: add suitable flocculation agent just the aluminum phosphate in waste liquid can be precipitated out changing in waste liquid, after filtration, then the method such as binding film processing removes the ion in filtrate, thereby obtained the higher phosphoric acid of purity.The method is simple, easy to operate, and the material reclaiming meets the needs that again utilize, thereby reaches the object of again utilizing.
Embodiment 1
Collect 4m
3change into waste liquid, wherein phosphoric acid concentration is that 0.5mol/L, aluminum phosphate concentration are 36g/L, and being driven into volume is 5m
3retort in, in retort, add the polyacrylamide that accounts for waste liquid weight 0.5%, leave standstill 8h, filter by millipore filtration equipment, filter cake is dry 3h under 80 DEG C of conditions, obtains 140.5kg aluminum phosphate, purity 96%, filtrate, by anion and cation exchange membrane, obtains phosphoric acid and reclaims liquid 3.8m
3, concentration is 0.47mol/L.
Embodiment 2
Collect 3m
3change into waste liquid, wherein phosphoric acid concentration is that 0.4mol/L, aluminum phosphate concentration are 27g/L, and being driven into volume is 5m
3retort in, in retort, add the polyacrylamide that accounts for waste liquid weight 0.3%, leave standstill 6h, by activated carbon filtration 4 times, filter cake is dry 2.5h under 100 DEG C of conditions, obtains 79.2kg aluminum phosphate, purity 94%, filtrate, by anion and cation exchange membrane, obtains phosphoric acid and reclaims liquid 2.8m
3, concentration is 0.38mol/L.
Embodiment 3
Collect 4.5m
3change into waste liquid, wherein phosphoric acid concentration is that 0.3mol/L, aluminum phosphate concentration are 27g/L, and being driven into volume is 5m
3retort in, in retort, add the polyacrylamide that accounts for waste liquid weight 0.1%, leave standstill 8h, filter by millipore filtration equipment, filter cake is dry 2h under 120 DEG C of conditions, obtains 116.4kg aluminum phosphate, purity 96%, filtrate, by reverse osmosis membrane, obtains phosphoric acid and reclaims liquid 4.3m
3, concentration is 0.28mol/L.
Embodiment 4
Collect 5m
3change into waste liquid, wherein phosphoric acid concentration is that 0.3mol/L, aluminum phosphate concentration are 22g/L, and being driven into volume is 5m
3retort in, in retort, add the polyacrylamide that accounts for waste liquid weight 0.1%, leave standstill 9h, by multi-medium filtering, filter cake is dry 1.5h under 140 DEG C of conditions, obtains 106.3kg aluminum phosphate, purity 94%, filtrate, by diffusion dialysis device, obtains phosphoric acid and reclaims liquid 4.8m
3, concentration is 0.26mol/L.
Claims (8)
1. a recovery changes into the method for phosphoric acid and aluminum phosphate in waste liquid, it is characterized in that: comprise the following steps: add flocculation agent changing in waste liquid, staticly settle rear filtration, collect filtrate, the ion of removing in filtrate obtains phosphoric acid solution, and filtration cakes torrefaction obtains aluminum phosphate solid.
2. method according to claim 1, is characterized in that: by weight, the add-on of flocculation agent accounts for and changes into 0.01～1% of waste liquid.
3. method according to claim 1, is characterized in that: described flocculation agent is polyacrylamide.
4. method according to claim 1, is characterized in that: time of repose is 5～10h.
5. method according to claim 1, is characterized in that: described is dried as dry 1～3h at 70～150 DEG C.
6. method according to claim 1, is characterized in that: filter and adopt in millipore filtration, activated carbon filtration or multi-medium filtering any one.
7. method according to claim 6, is characterized in that: described multimedium is quartz sand, hard coal, gac, magnetite, opens up at least two kinds in garnet, pottery, baton round.
8. method according to claim 1, is characterized in that: adopt anion and cation exchange membrane method, reverse osmosis membrane processing method or diffusive dialysis method to remove filtrate intermediate ion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410364903.8A CN104098076A (en) | 2014-07-29 | 2014-07-29 | Method for reclaiming phosphoric acid and aluminium phosphate in formation waste liquid |
Applications Claiming Priority (1)
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| CN201410364903.8A CN104098076A (en) | 2014-07-29 | 2014-07-29 | Method for reclaiming phosphoric acid and aluminium phosphate in formation waste liquid |
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| CN104098076A true CN104098076A (en) | 2014-10-15 |
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| CN201410364903.8A Pending CN104098076A (en) | 2014-07-29 | 2014-07-29 | Method for reclaiming phosphoric acid and aluminium phosphate in formation waste liquid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828795A (en) * | 2015-05-13 | 2015-08-12 | 南京工业大学 | Wet phosphoric acid production process through ceramic membrane method |
| CN106966414A (en) * | 2016-12-22 | 2017-07-21 | 新疆智诚同欣环保科技有限公司 | A kind of waste phosphoric acid processing method for producing electrode foil |
| CN110820028A (en) * | 2018-08-09 | 2020-02-21 | 湖北工业大学 | Treatment method for recycling waste acid of aluminum profile anodic oxidation tank |
| CN115259116A (en) * | 2021-04-29 | 2022-11-01 | 中国科学院过程工程研究所 | Regeneration method of phosphoric acid-containing waste liquid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102826691A (en) * | 2012-09-25 | 2012-12-19 | 四川俊宏环保科技有限公司 | Electrode foil formation section phosphoric acid waste liquor treatment technique |
| CN103030126A (en) * | 2011-10-10 | 2013-04-10 | 徐州特瑞达环保科技有限公司 | Recovery method for waste phosphoric acid liquor generated in production process of formed foil |
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2014
- 2014-07-29 CN CN201410364903.8A patent/CN104098076A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030126A (en) * | 2011-10-10 | 2013-04-10 | 徐州特瑞达环保科技有限公司 | Recovery method for waste phosphoric acid liquor generated in production process of formed foil |
| CN102826691A (en) * | 2012-09-25 | 2012-12-19 | 四川俊宏环保科技有限公司 | Electrode foil formation section phosphoric acid waste liquor treatment technique |
Non-Patent Citations (1)
| Title |
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| 陈观文等: "《分离膜应用与工程案例》", 30 November 2007 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828795A (en) * | 2015-05-13 | 2015-08-12 | 南京工业大学 | Wet phosphoric acid production process through ceramic membrane method |
| CN106966414A (en) * | 2016-12-22 | 2017-07-21 | 新疆智诚同欣环保科技有限公司 | A kind of waste phosphoric acid processing method for producing electrode foil |
| CN106966414B (en) * | 2016-12-22 | 2018-10-12 | 新疆智诚同欣环保科技有限公司 | A kind of waste phosphoric acid processing method producing electrode foil |
| CN110820028A (en) * | 2018-08-09 | 2020-02-21 | 湖北工业大学 | Treatment method for recycling waste acid of aluminum profile anodic oxidation tank |
| CN110820028B (en) * | 2018-08-09 | 2021-07-30 | 湖北工业大学 | Treatment method for recycling waste acid of aluminum profile anodic oxidation tank |
| CN115259116A (en) * | 2021-04-29 | 2022-11-01 | 中国科学院过程工程研究所 | Regeneration method of phosphoric acid-containing waste liquid |
| CN115259116B (en) * | 2021-04-29 | 2024-01-30 | 中国科学院过程工程研究所 | Regeneration method of phosphoric acid-containing waste liquid |
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