CN103030126A - Recovery method for waste phosphoric acid liquor generated in production process of formed foil - Google Patents
Recovery method for waste phosphoric acid liquor generated in production process of formed foil Download PDFInfo
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- CN103030126A CN103030126A CN2011103037856A CN201110303785A CN103030126A CN 103030126 A CN103030126 A CN 103030126A CN 2011103037856 A CN2011103037856 A CN 2011103037856A CN 201110303785 A CN201110303785 A CN 201110303785A CN 103030126 A CN103030126 A CN 103030126A
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Abstract
The invention discloses a recovery method for waste phosphoric acid liquor generated in a production process of formed foil. The method comprises the following steps of: step 1, adding an alkaline solution in the waste phosphoric acid liquor, regulating PH value to be 3.0-7.0 to obtain aluminum phosphate sediment, and filtering to get filtrate; and step 2, adding metal chloride, metal oxide or metal hydroxide in the filtrate from which the aluminum phosphate sediment is filtered out, regulating the PH value to be 6-9 to generate corresponding sediment, filtering, and discharging the waste liquor. According to the recovery method, firstly, the alkaline solution is used for reacting with aluminum in the waste liquor to produce aluminum phosphate, and aluminum phosphate is settled and recovered, thus, resource is saved; and then, the residual filtrate is mixed with metal chloride, metal oxide and the like for reaction, so that phosphoric acid in the filtrate generates various phosphate compounds, phosphoric acid in the waste liquor is eliminated, and the harm to environment is reduced.
Description
Technical field
The present invention relates to chemical field, be specifically related to the recovery method of the waste phosphoric acid liquid that produces in a kind of Waste Acid From Hua Cheng Foil production process.
Background technology
The Waste Acid From Hua Cheng Foil industry uses the dilute phosphoric acid of content 5% that aluminium foil surface is processed in a large number, when the content of aluminium in the phosphoric acid reaches certain value, then discharges as spent acid, contains AlPO in the waste phosphoric acid of this discharge
4Be about about 2%, phosphoric acid is about about 4%.And Waste Acid From Hua Cheng Foil producer only is the method that adopts film to reclaim to waste phosphoric acid, the phosphoric acid rate of recovery of this method only has 60%, does not also reclaim aluminum phosphate wherein, and aluminum phosphate is discharged as refuse, not only waste resource but also to environment, form again new pollution in the regenerative process of this external film.
Summary of the invention
Not thorough for solving the liquid waste disposal that produces in the Waste Acid From Hua Cheng Foil production process, the problem of waste resource and contaminate environment the invention provides and a kind ofly waste liquid is carried out twice processing makes the phosphide in the waste liquid generate the method that precipitation reclaims.
Concrete scheme of the present invention is as follows: the recovery method of the waste phosphoric acid liquid that produces in a kind of Waste Acid From Hua Cheng Foil production process, comprise the steps,
Step 1, in waste phosphoric acid liquid, add basic solution, regulate pH value to 3.0-7.0, obtain the aluminum phosphate precipitation, filter, obtain filtrate;
Add metal chloride, metal oxide or metal hydroxides in step 2, the filtrate after leaching the aluminum phosphate precipitation, regulating the pH value is 6-9, generates accordingly precipitation, filters effluent discharge.
Further, the basic solution in the described step 1 is selected from least a in sodium carbonate solution, sodium hydroxide solution, potassium hydroxide solution or the ammoniacal liquor.
Further, when adding basic solution, stir; Waste phosphoric acid liquid and basic solution reaction times are 1～2 hour; Obtain aluminum phosphate and be deposited in 100～150 ℃ of lower oven dry 1～2 hour.
Further, the precipitation in the described step 2 obtains as follows: stir when adding solid metal muriate, metal oxide or metal hydroxides; The reaction times of filtrate and metal chloride, metal oxide or metal hydroxides is 1～1.5 hour; Corresponding 100～150 ℃ of lower oven dry 1～2 hour that is deposited in that generates.
Further, the mass percent of described step 1 neutral and alkali solution is 20%～40%, and the weight percent that accounts for waste phosphoric acid liquid is 1/30～1/20.
Further, metal chloride, metal oxide or metal hydroxides are that solid and the weight percent that accounts for filtrate are 1/30～1/20 in the described step 2.
Further, the chemical reaction that occurs in step 1 is selected from least a in the following chemical equation:
Al(H
2PO
4)
3+Na
2CO
3＝AlPO
4↓+2NaH
2PO
4+CO
2↑+H
2O；
Or Al (H2PO4) 3+K2CO3=AlPO4 ↓+2KH2PO4+CO2 ↑+H2O;
Or Al (H2PO4) 3+ (NH4) 2CO3=AlPO4 ↓+2NH4H2PO4+CO2 ↑+H2O;
Or Al (H2PO4) 3+NaOH=AlPO4 ↓+2NaH2PO4+2H2O;
Or Al (H
2PO
4)
3+ KOH=AlPO
4↓+2KH
2PO
4+ 2H
2O;
Or Al (H
2PO
4)
3+ NH
3H
2O=AlPO4 ↓+2NH
4H
2PO
4+ 2H
2O.
Further, the chemical reaction that occurs in step 2 is selected from least a in the following chemical equation:
2XH2PO4+MCl2+2MO＝M3(PO4)2↓+2XCl+2H2O
Wherein X represents a kind of of basic metal or ammonium, and M represents a kind of in calcium, zinc, the magnesium.
Effect of the present invention: at first react with the aluminium in basic solution and the waste liquid and obtain aluminum phosphate and precipitation reclaims, saved resource, again hybrid metal muriate, oxide compound etc. in the remaining filtrate are reacted, make the phosphoric acid in the filtrate generate various phosphate cpds, thereby eliminated the phosphoric acid in the waste liquid, reduced the harm to environment.
Embodiment
The recovery method of the waste phosphoric acid liquid that produces in a kind of Waste Acid From Hua Cheng Foil production process comprises the steps,
101, in waste phosphoric acid liquid, add basic solution, regulate pH value to 3.0-7.0, obtain the aluminum phosphate precipitation, filter, obtain filtrate;
In a certain amount of waste phosphoric acid, add a kind of in yellow soda ash, sodium hydroxide, potassium hydroxide or the ammoniacal liquor, by stirring reaction, make the pH value of waste liquid reach 3.0-7.0, A1PO wherein
4Precipitate, because AlPO
4Be a kind of water-fast material, therefore can separate by solid-liquid, waste phosphoric acid liquid and basic solution reaction times are 1～2 hour; Obtain aluminum phosphate and be deposited in 100～150 ℃ of lower oven dry 1～2 hour, more remaining waste liquid is discharged in another reactor.Wherein the mass percent of basic solution is 20%～40%, and the weight percent that accounts for waste phosphoric acid liquid is 1/30～1/20.The chemical reaction that occurs is at least a in the following chemical equation:
Al(H2PO4)3+Na2CO3＝AlPO4↓+2NaH2PO4+CO2↑+H2O；
Or A1 (H2PO4) 3+K2CO3=AlPO4 ↓+2KH2PO4+CO2 ↑+H2O;
Or A1 (H2PO4) 3+ (NH4) 2CO3=AlPO4 ↓+2NH4H2PO4+CO2 ↑+H2O;
Or Al (H2PO4) 3+2NaOH=A l PO4 ↓+2NaH2PO4+2H2O;
Or Al (H2PO4) 3+2KOH=AlPO4 ↓+2KH2PO4+2H2O;
Or Al (H2PO4) 3+2NH3H2O=AlPO4 ↓+2NH4H2PO4+2H2O.
102, add metal chloride, metal oxide or metal hydroxides in the filtrate after leaching the aluminum phosphate precipitation, regulating the pH value is 6-9, generates accordingly precipitation, filters effluent discharge.
When adding solid metal muriate, metal oxide or metal hydroxides, stir, the weight percent that metal chloride, metal oxide or metal hydroxides account for filtrate is 1/30～1/20, and the reaction times of filtrate and metal chloride, metal oxide or metal hydroxides is 1～3 hour; Corresponding 100～150 ℃ of lower oven dry 1～2 hour that is deposited in that generates.The chemical reaction that occurs is at least a in the following chemical equation:
2XH2PO4+MCl2+2MO＝M3(PO4)2↓+2XC1+2H2O
Wherein X represents a kind of of basic metal or ammonium, and M represents a kind of in calcium, zinc, the magnesium.
By the pollution of having stopped phosphoric acid in the waste phosphoric acid liquid after the above-mentioned steps processing, and aluminum phosphate can be separated out separately the independent product of formation, save resource, protect environment.
Embodiment 1
Get waste phosphoric acid 500g (content 5.4%) in the 1000ml beaker, stir lower 32% sodium hydroxide solution, 40 grams that add, reaction 1h, pH is 3.6, have a large amount of Precipitations this moment, filters rear 150 ℃ of oven dry, gets aluminum phosphate product 11.2g, zinc chloride 20 grams of adding 98% in waste liquid, stirring reaction 1h under the normal temperature, surveying pH is 2.68, adds 95% zinc oxide, 16 grams again, stirring reaction 1h under the normal temperature, surveying pH is 6.76, leaves standstill suction filtration, solid is at 150 ℃ of oven dry 2h, and zinc phosphate product 51.9g weighs to get.
Embodiment 2
Get waste phosphoric acid 500g (content 5.4%) in the 1000ml beaker, stir lower yellow soda ash 22 grams that add, reaction 1.5h, this moment, pH was 6.01, and have a large amount of Precipitations this moment, filters rear 150 ℃ of oven dry, get aluminum phosphate product 11.5g, in filtrate, add the 35g Calcium dichloride dihydrate, stirring reaction 1h under the normal temperature, surveying pH is 2; After adding 6 gram calcium hydroxide stirring reaction 2h, surveying pH value of solution is 9.0 again, leave standstill, and suction filtration, solid is at 150 ℃ of oven dry 1.5h, and calcium phosphate product 33.7g weighs to get.
Embodiment 3
Example 3, get waste phosphoric acid 500g (content 5.4%) in the 1000ml beaker, stir lower yellow soda ash 22 grams that add, reaction 1.5h, this moment, pH was 5.97, and have a large amount of Precipitations this moment, filters rear 150 ℃ of oven dry, get aluminum phosphate product 11.3g, add the 35g Calcium dichloride dihydrate in filtrate, stirring reaction 1h under the normal temperature surveys pH 2; After adding 5 gram calcium hydroxide stirring reaction 2h, pH value of solution is 6.7 again, leave standstill, and suction filtration, solid is at 150 ℃ of oven dry 1.5h, and calcium phosphate product 33.2g weighs to get.
Embodiment 4
Get waste phosphoric acid 500g (content 5.4%) in the 1000ml beaker, stir lower yellow soda ash 22 grams that add, reaction 1.5h, this moment, pH was 6.04, and have a large amount of Precipitations this moment, filters rear 150 ℃ of oven dry, get aluminum phosphate product 13.2g, add the 30g Calcium dichloride dihydrate in filtrate, stirring reaction 1h under the normal temperature surveys pH 2.66; After adding 8 gram calcium hydroxide stirring reaction 2h, pH value of solution is 7.47 again, leave standstill, and suction filtration, solid is at 150 ℃ of oven dry 1.5h, and calcium phosphate product 37.1g weighs to get.
Above demonstration and described basic structure of the present invention, ultimate principle, principal character and advantage of the present invention.The technician of the industry should understand, and the present invention is not restricted to the described embodiments, and that describes in above-described embodiment and the specification sheets just illustrates basic structure of the present invention and ultimate principle.The present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the scope of protection of present invention.
Claims (8)
1. the recovery method of the waste phosphoric acid liquid that produces in the Waste Acid From Hua Cheng Foil production process is characterized in that, comprises the steps,
Step 1, in waste phosphoric acid liquid, add basic solution, regulate pH value to 3.0-7.0, obtain the aluminum phosphate precipitation, filter, obtain filtrate;
Add metal chloride, metal oxide or metal hydroxides in step 2, the filtrate after leaching the aluminum phosphate precipitation, regulating the pH value is 6-9, generates accordingly precipitation, filters effluent discharge.
2. recovery method as claimed in claim 1 is characterized in that, the basic solution in the described step 1 is selected from least a in sodium carbonate solution, sodium hydroxide solution, potassium hydroxide solution or the ammoniacal liquor.
3. recovery method as claimed in claim 1 is characterized in that, in the described step 1, stirs when adding basic solution; Waste phosphoric acid liquid and basic solution reaction times are 1～2 hour;
Obtain aluminum phosphate and be deposited in 100～150 ℃ of lower oven dry 1～2 hour.
4. recovery method as claimed in claim 1 is characterized in that, the precipitation in the described step 2 obtains as follows: stir when adding solid metal muriate, metal oxide or metal hydroxides; The reaction times of filtrate and metal chloride, metal oxide or metal hydroxides is 1～1.5 hour;
Corresponding 100～150 ℃ of lower oven dry 1～2 hour that is deposited in that generates.
5. recovery method as claimed in claim 1 is characterized in that, the mass percent of described step 1 neutral and alkali solution is 20%～40%, and the weight percent that accounts for waste phosphoric acid liquid is 1/30～1/20.
6. recovery method as claimed in claim 1 is characterized in that, metal chloride, metal oxide or metal hydroxides are that solid and the weight percent that accounts for filtrate are 1/30～1/20 in the described step 2.
7. recovery method as claimed in claim 1 is characterized in that, the chemical reaction that occurs in step 1 is selected from least a in the following chemical equation:
Al(H
2PO
4)
3+Na
2CO
3＝AlPO
4↓+2NaH
2PO
4+CO
2↑+H
2O；
Or Al (H2PO4) 3+K2CO3=AlPO4 ↓+2KH2PO4+CO2 ↑+H2O;
Or Al (H2PO4) 3+ (NH4) 2CO3=AlPO4 ↓+2NH4H2PO4+CO2 ↑+H2O;
Or Al (H2PO4) 3+NaOH=AlPO4 ↓+2NaH2PO4+2H2O;
Or Al (H
2PO
4)
3+ KOH=AlPO
4↓+2KH
2PO
4+ 2H
2O;
Or Al (H
2PO
4)
3+ NH
3H
2O=AlPO4 ↓+2NH
4H
2PO
4+ 2H
2O.
8. recovery method as claimed in claim 1 is characterized in that, the chemical reaction that occurs in step 2 is selected from least a in the following chemical equation:
2XH2PO4+MCl2+2MO＝M3(PO4)2↓+2XCl+2H2O
Wherein X represents a kind of of basic metal or ammonium, and M represents a kind of in calcium, zinc, the magnesium.
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|---|---|---|---|
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|---|---|---|---|
| CN2011103037856A CN103030126A (en) | 2011-10-10 | 2011-10-10 | Recovery method for waste phosphoric acid liquor generated in production process of formed foil |
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| CN103030126A true CN103030126A (en) | 2013-04-10 |
Family
ID=48017592
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288067A (en) * | 2013-06-27 | 2013-09-11 | 武汉科梦环境工程有限公司 | Method for recycling phosphates from formed foil pickling wastewater |
| CN104098076A (en) * | 2014-07-29 | 2014-10-15 | 四川立业电子有限公司 | Method for reclaiming phosphoric acid and aluminium phosphate in formation waste liquid |
| CN105198147A (en) * | 2015-09-15 | 2015-12-30 | 博天环境集团股份有限公司 | Treatment method for organic amine waste water generated by producing molecular sieve and carrier catalyst thereof |
| CN106219507A (en) * | 2016-07-08 | 2016-12-14 | 宿迁久巨环保科技有限公司 | A kind of Application way of electronic material pickling waste phosphoric acid |
| CN106744759A (en) * | 2016-12-23 | 2017-05-31 | 新疆智诚同欣环保科技有限公司 | A kind of recovery method high of waste phosphoric acid film when producing electrode foil |
| 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 |
| CN110156056A (en) * | 2019-04-18 | 2019-08-23 | 新疆众和股份有限公司 | A method of special-alumina is prepared containing phosphorus waste liquid using corrosive aluminum foil |
| CN110446608A (en) * | 2016-12-15 | 2019-11-12 | 萨巴瑞提股份有限公司 | Be recycled and packaged the method and apparatus of material |
| CN110498402A (en) * | 2019-09-25 | 2019-11-26 | 龚典局 | A kind of phosphorous spent acid method of comprehensive utilization |
| CN112707406A (en) * | 2021-02-07 | 2021-04-27 | 深圳瑞赛环保科技有限公司 | Chemical waste-throwing phosphoric acid treatment and synthesis method of aluminium phosphate molecular sieve |
| CN116161632A (en) * | 2022-12-20 | 2023-05-26 | 无锡中天固废处置有限公司 | Method for improving quality of sodium dihydrogen phosphate generated by aluminum-containing phosphoric acid |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103288067A (en) * | 2013-06-27 | 2013-09-11 | 武汉科梦环境工程有限公司 | Method for recycling phosphates from formed foil pickling wastewater |
| CN104098076A (en) * | 2014-07-29 | 2014-10-15 | 四川立业电子有限公司 | Method for reclaiming phosphoric acid and aluminium phosphate in formation waste liquid |
| CN105198147A (en) * | 2015-09-15 | 2015-12-30 | 博天环境集团股份有限公司 | Treatment method for organic amine waste water generated by producing molecular sieve and carrier catalyst thereof |
| CN105198147B (en) * | 2015-09-15 | 2017-05-31 | 博天环境集团股份有限公司 | The processing method of the organic amine wastewater that production molecular sieve and its carried catalyst are produced |
| CN106219507A (en) * | 2016-07-08 | 2016-12-14 | 宿迁久巨环保科技有限公司 | A kind of Application way of electronic material pickling waste phosphoric acid |
| CN110446608A (en) * | 2016-12-15 | 2019-11-12 | 萨巴瑞提股份有限公司 | Be recycled and packaged the method and apparatus of material |
| US11535022B2 (en) | 2016-12-15 | 2022-12-27 | saperatec GmbH | Method and apparatus for recycling packaging material |
| CN110446608B (en) * | 2016-12-15 | 2022-07-01 | 萨巴瑞提股份有限公司 | Method and apparatus for recycling packaging material |
| 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 |
| CN106744759B (en) * | 2016-12-23 | 2019-03-15 | 新疆智诚同欣环保科技有限公司 | A kind of high recovery method of waste phosphoric acid film when producing electrode foil |
| CN106744759A (en) * | 2016-12-23 | 2017-05-31 | 新疆智诚同欣环保科技有限公司 | A kind of recovery method high of waste phosphoric acid film when producing electrode foil |
| CN110156056B (en) * | 2019-04-18 | 2021-12-28 | 新疆众和股份有限公司 | Method for preparing special alumina by using phosphorus-containing waste liquid generated by corroding aluminum foil |
| CN110156056A (en) * | 2019-04-18 | 2019-08-23 | 新疆众和股份有限公司 | A method of special-alumina is prepared containing phosphorus waste liquid using corrosive aluminum foil |
| CN110498402A (en) * | 2019-09-25 | 2019-11-26 | 龚典局 | A kind of phosphorous spent acid method of comprehensive utilization |
| CN112707406A (en) * | 2021-02-07 | 2021-04-27 | 深圳瑞赛环保科技有限公司 | Chemical waste-throwing phosphoric acid treatment and synthesis method of aluminium phosphate molecular sieve |
| CN112707406B (en) * | 2021-02-07 | 2023-05-16 | 深圳瑞赛环保科技有限公司 | Chemical waste disposal phosphoric acid treatment and aluminum phosphate molecular sieve synthesis method |
| CN116161632A (en) * | 2022-12-20 | 2023-05-26 | 无锡中天固废处置有限公司 | Method for improving quality of sodium dihydrogen phosphate generated by aluminum-containing phosphoric acid |
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Application publication date: 20130410 |