CN109574304A - A kind of method of comprehensive utilization containing phosphorus waste liquid - Google Patents
A kind of method of comprehensive utilization containing phosphorus waste liquid Download PDFInfo
- Publication number
- CN109574304A CN109574304A CN201811480886.9A CN201811480886A CN109574304A CN 109574304 A CN109574304 A CN 109574304A CN 201811480886 A CN201811480886 A CN 201811480886A CN 109574304 A CN109574304 A CN 109574304A
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- CN
- China
- Prior art keywords
- monohydrogen phosphate
- calcium monohydrogen
- calcium
- waste liquid
- water
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
-
- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a kind of method of comprehensive utilization containing phosphorus waste liquid, comprising the following steps: step 1, calcium carbonate is added in batches into waste phosphoric acid and is reacted, obtain reaction mixture；Step 2, calcium oxide is added into reaction mixture, as the addition of calcium oxide is diluted with water simultaneously, obtains calcium monohydrogen phosphate suspension；Step 3, the calcium monohydrogen phosphate suspension that reaction generates is subjected to filters pressing with filter press is pumped into, is passed through tap water rinse again after pressure is full, a small amount of free acid for remaining in calcium monohydrogen phosphate gap is washed out to improve product quality；Step 4, the calcium monohydrogen phosphate after rinsing goes out machine after filter press filters pressing, obtains the calcium monohydrogen phosphate semi-finished product of free water content 20wt%~40wt%；Step 5, calcium monohydrogen phosphate semi-finished product are dried through hot pump in low temp, and product quality requirement is met after free water content≤15%, and packaging is sold.Method of comprehensive utilization concise in technology, equipment cost of the present invention containing phosphorus waste liquid are cheap；Complete recycling and utilization have been carried out to the phosphoric acid in waste liquid, realized the zero-emission of phosphorus-containing wastewater, has reduced the pollution to environment.
Description
Technical field
The invention belongs to hazardous waste disposals to utilize technical field, more particularly to the comprehensive utilization side containing phosphorus waste liquid
Method.
Background technique
In aluminium etching, dry ecthing of the industry frequently with the wet etch method of chemical reagent, ion(ic) etching and plasma etching
Method.Wet etch method is by cheap chemical reagent and more at low cost than dry ecthing method without using expensive equipment.In addition, wet etching
Method can also handle the metal material of various shapes and can handle the material with three-dimensional structure.In addition, wet etching
Method is also easy to recycle aluminium, aluminium from spent etching solution.In this way, wet etch method is widely used in aluminium etching.
It is phosphoric acid (content is 50% to 65%) that a large amount of waste phosphoric acid liquid main component can be generated in aluminium etching, and containing few
Measure nitric acid and acetic acid.Currently, the main processing mode of waste phosphoric acid be by after acid-base neutralization, waste liquid enter sewage disposal system into
It is discharged after row processing.Although by the technique wave of a large amount of phosphoric acid can be caused by waste phosphoric acid processing to discharge standard
Take, aggravated the burden of sewage treatment, can not achieve the effective use of resource.
Summary of the invention
The object of the present invention is to provide a kind of method of comprehensive utilization containing phosphorus waste liquid, are caused largely with solving existing method
The waste of phosphoric acid, the problem of can not achieve the effective use of resource.
The technical scheme to solve the above technical problems is that a kind of method of comprehensive utilization containing phosphorus waste liquid, including
Following steps:
Step 1, calcium carbonate is added in batches into waste phosphoric acid to be reacted, stops calcium carbonate before waste phosphoric acid total overall reaction
It is added, obtains reaction mixture at this time；
Step 2, calcium oxide is added into reaction mixture, adjusts Ph value between 4~6, as the addition of calcium oxide adds simultaneously
Water dilution, obtains calcium monohydrogen phosphate suspension；
Step 3, the calcium monohydrogen phosphate suspension that reaction generates is subjected to filters pressing with filter press is pumped into, is passed through tap water again after pressure is full
Rinsing washes out a small amount of free acid for remaining in calcium monohydrogen phosphate gap to improve product quality；
Step 4, the calcium monohydrogen phosphate after rinsing goes out machine after filter press filters pressing, obtains free water content 20wt%~40wt%
Calcium monohydrogen phosphate semi-finished product；
Step 5, calcium monohydrogen phosphate semi-finished product are dried through hot pump in low temp, and product quality requirement, packaging are met after free water content≤15%
It sells.
The present invention is as described above containing the method for comprehensive utilization of phosphorus waste liquid, it is preferred that before step 1 operation carries out, first
Waste phosphoric acid is diluted using tap water or recycle-water.
The present invention is as described above containing the method for comprehensive utilization of phosphorus waste liquid, it is preferred that in the treatment process of step 3, filtrate
Into reuse water collecting groove, rinse water also enters reuse water collecting groove；Recycle-water in collecting tank is in step 1 and/or step 2
It is utilized again in dilution.
The present invention is as described above containing the method for comprehensive utilization of phosphorus waste liquid, it is preferred that the detailed process of step 1 are as follows: to useless
Calcium carbonate is added in phosphoric acid in batches to be reacted, with the progress of reaction, sediment increases so that solution gradually becomes sticky,
It needs moisturizing excessively sticky to avoid solution and damages stirring rod.
The present invention is as described above containing the method for comprehensive utilization of phosphorus waste liquid, it is preferred that in the treatment process of step 3, filtrate
Into reuse water collecting groove, rinse water also enters reuse water collecting groove；Recycle-water in collecting tank is during the moisturizing of step 1
It utilizes again.
Method of comprehensive utilization concise in technology, equipment cost of the present invention containing phosphorus waste liquid are cheap；Phosphoric acid in waste liquid is carried out
Complete recycling and utilization, realize the zero-emission of phosphorus-containing wastewater, reduce the pollution to environment.
Specific embodiment
The embodiment recorded herein is specific specific embodiment of the invention, for illustrating design of the invention,
Be it is explanatory and illustrative, should not be construed as the limitation to embodiment of the present invention and the scope of the invention.Except what is recorded herein
Outside embodiment, those skilled in the art can also based on the claim of this application book and specification disclosure of that using aobvious and
The other technical solutions being clear to, these technical solutions include using any obvious to making for the embodiment recorded herein
The technical solution of substitutions and modifications.
Device therefor specifications and models are as shown in table 1 in following embodiment.
Table 1
Embodiment 1
Method of comprehensive utilization of the present embodiment containing phosphorus waste liquid is the following steps are included: step 1, carbonic acid is added into waste phosphoric acid in batches
Calcium is reacted, and is stopped the addition of calcium carbonate before waste phosphoric acid total overall reaction, is obtained reaction mixture at this time；Step 2, to anti-
It answers and calcium oxide is added in mixture, adjust Ph value between 4~6, as the addition of calcium oxide is diluted with water simultaneously, obtain phosphoric acid
Hydrogen calcium suspension；Step 3, the calcium monohydrogen phosphate suspension that reaction generates is subjected to filters pressing with filter press is pumped into, led to again after pressure is full
Enter tap water rinse, a small amount of free acid for remaining in calcium monohydrogen phosphate gap is washed out to improve product quality；Step 4, after rinsing
Calcium monohydrogen phosphate, after filter press filters pressing go out machine, obtain the calcium monohydrogen phosphate semi-finished product of free water content 20wt%~40wt%；
Step 5, calcium monohydrogen phosphate semi-finished product are dried through hot pump in low temp, and product quality requirement is met after free water content≤15%, is packed out
It sells.
Method of comprehensive utilization of the present embodiment containing phosphorus waste liquid uses step 1 and step 2 knot according to the content of phosphoric acid in waste liquid
The two sections of precipitation method closed, adjust pH value by the way that calcium oxide is added to 4-6, complete precipitate phosphoric acid root, improve production efficiency with
Product quality.
Embodiment 2
Method of comprehensive utilization of the present embodiment containing phosphorus waste liquid is the following steps are included: first with tap water or recycle-water to waste phosphoric acid
It is diluted then operation processing in accordance with the following steps.Step 1, calcium carbonate is added in batches into waste phosphoric acid to be reacted,
The addition for stopping calcium carbonate before waste phosphoric acid total overall reaction, obtains reaction mixture at this time；Step 2, add into reaction mixture
Enter calcium oxide, adjust Ph value between 4~6, as the addition of calcium oxide is diluted with water simultaneously, obtains calcium monohydrogen phosphate suspension；
Step 3, the calcium monohydrogen phosphate suspension that reaction generates is subjected to filters pressing with filter press is pumped into, is passed through tap water drift after pressure is full again
It washes, a small amount of free acid for remaining in calcium monohydrogen phosphate gap is washed out to improve product quality；Step 4, the calcium monohydrogen phosphate after rinsing,
Go out machine after filter press filters pressing, obtains the calcium monohydrogen phosphate semi-finished product of free water content 20wt%~40wt%；Step 5, phosphoric acid
Hydrogen calcium semi-finished product are dried through hot pump in low temp, and product quality requirement is met after free water content≤15%, and packaging is sold.
Embodiment 3
Method of comprehensive utilization of the present embodiment containing phosphorus waste liquid is the following steps are included: step 1, carbonic acid is added into waste phosphoric acid in batches
Calcium is reacted, and with the progress of reaction, sediment increases so that solution gradually becomes sticky, needs moisturizing to avoid solution mistake
In sticky and damage stirring rod；The addition for stopping calcium carbonate before waste phosphoric acid total overall reaction, obtains reaction mixture at this time；Step
Rapid 2, calcium oxide is added into reaction mixture, adjusts Ph value between 4~6, as the addition of calcium oxide is diluted with water simultaneously,
Obtain calcium monohydrogen phosphate suspension；Step 3, the calcium monohydrogen phosphate suspension that reaction generates is subjected to filters pressing with filter press is pumped into, pressed
It is passed through tap water rinse again after full, a small amount of free acid for remaining in calcium monohydrogen phosphate gap is washed out to improve product quality；Step
4, the calcium monohydrogen phosphate after rinsing goes out machine after filter press filters pressing, obtains the phosphoric acid hydrogen of free water content 20wt%~40wt%
Calcium semi-finished product；Step 5, calcium monohydrogen phosphate semi-finished product are dried through hot pump in low temp, and product quality is met after free water content≤15% and is wanted
It asks, packaging is sold.
Embodiment 4
Method of comprehensive utilization of the present embodiment containing phosphorus waste liquid is the following steps are included: step 1, carbonic acid is added into waste phosphoric acid in batches
Calcium is reacted, and with the progress of reaction, sediment increases so that solution gradually becomes sticky, needs moisturizing to avoid solution mistake
In sticky and damage stirring rod；The addition for stopping calcium carbonate before waste phosphoric acid total overall reaction, obtains reaction mixture at this time；Step
Rapid 2, calcium oxide is added into reaction mixture, adjusts Ph value between 4~6, as the addition of calcium oxide is diluted with water simultaneously,
Obtain calcium monohydrogen phosphate suspension；Step 3, the calcium monohydrogen phosphate suspension that reaction generates is subjected to filters pressing with filter press is pumped into, pressed
It is passed through tap water rinse again after full, a small amount of free acid for remaining in calcium monohydrogen phosphate gap is washed out to improve product quality；Filtrate
Into reuse water collecting groove, rinse water also enters reuse water collecting groove；Recycle-water in collecting tank is during the moisturizing of step 1
It utilizes again, the recycle-water in collecting tank can also utilize again in the dilution of step 1 and/or step 2；Step 4, it floats
Calcium monohydrogen phosphate after washing goes out machine after filter press filters pressing, obtains the calcium monohydrogen phosphate half of free water content 20wt%~40wt%
Finished product；Step 5, calcium monohydrogen phosphate semi-finished product are dried through hot pump in low temp, and product quality requirement, packet are met after free water content≤15%
It takes on and sells.
Each technical characteristic of above-mentioned disclosure is not limited to disclosed and other feature combination, and those skilled in the art are also
Can carry out other combinations between each technical characteristic according to the purpose of invention, be subject to realize the present invention purpose.
Claims (5)
1. a kind of method of comprehensive utilization containing phosphorus waste liquid, which comprises the following steps:
Step 1, calcium carbonate is added in batches into waste phosphoric acid to be reacted, stops calcium carbonate before waste phosphoric acid total overall reaction
It is added, obtains reaction mixture at this time；
Step 2, calcium oxide is added into reaction mixture, adjusts Ph value between 4~6, as the addition of calcium oxide adds simultaneously
Water dilution, obtains calcium monohydrogen phosphate suspension；
Step 3, the calcium monohydrogen phosphate suspension that reaction generates is subjected to filters pressing with filter press is pumped into, is passed through tap water again after pressure is full
Rinsing washes out a small amount of free acid for remaining in calcium monohydrogen phosphate gap to improve product quality；
Step 4, the calcium monohydrogen phosphate after rinsing goes out machine after filter press filters pressing, obtains free water content 20wt%~40wt%
Calcium monohydrogen phosphate semi-finished product；
Step 5, calcium monohydrogen phosphate semi-finished product are dried through hot pump in low temp, and product quality requirement, packaging are met after free water content≤15%
It sells.
2. the method for comprehensive utilization according to claim 1 containing phosphorus waste liquid, which is characterized in that before step 1 operation carries out,
Waste phosphoric acid is diluted first with tap water or recycle-water.
3. the method for comprehensive utilization according to claim 2 containing phosphorus waste liquid, which is characterized in that in the treatment process of step 3,
Filtrate enters reuse water collecting groove, and rinse water also enters reuse water collecting groove；Recycle-water in collecting tank is in step 1 and/or step
It is utilized again in rapid 2 dilution.
4. the method for comprehensive utilization according to claim 1 containing phosphorus waste liquid, which is characterized in that the detailed process of step 1 are as follows:
Calcium carbonate is added in batches into waste phosphoric acid to be reacted, with the progress of reaction, sediment increases so that solution gradually becomes
It is sticky, it needs moisturizing excessively sticky to avoid solution and damages stirring rod.
5. the method for comprehensive utilization according to claim 4 containing phosphorus waste liquid, which is characterized in that in the treatment process of step 3,
Filtrate enters reuse water collecting groove, and rinse water also enters reuse water collecting groove；The moisturizing of recycle-water in collecting tank in step 1
It is utilized again in journey.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811480886.9A CN109574304A (en) | 2018-12-05 | 2018-12-05 | A kind of method of comprehensive utilization containing phosphorus waste liquid |
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| CN201811480886.9A CN109574304A (en) | 2018-12-05 | 2018-12-05 | A kind of method of comprehensive utilization containing phosphorus waste liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114684967A (en) * | 2022-04-06 | 2022-07-01 | 深圳大学 | Synergistic treatment method for calcareous solid waste and phosphorus-containing waste liquid and application of product thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120113351A (en) * | 2011-04-05 | 2012-10-15 | 허재수 | Manufacturing method of calcium phosphate using waste water |
| CN103213962A (en) * | 2013-04-19 | 2013-07-24 | 武汉工程大学 | Method for preparing feed-grade calcium hydrophosphate from phosphoric acid-containing mixed acid etching waste liquid |
| CN104445730A (en) * | 2014-11-21 | 2015-03-25 | 贵阳中化开磷化肥有限公司 | Comprehensive utilization method of wastewater containing phosphorus and fluorine |
| CN106276837A (en) * | 2016-08-15 | 2017-01-04 | 东江环保股份有限公司 | Phosphoric acid waste liquid prepares the method for calcium hydrophosphate fodder |
| CN106829904A (en) * | 2017-02-28 | 2017-06-13 | 连云港市德邦精细化工有限公司 | A kind of preparation method of graininess calcium phosphate dibasic anhydrous |
-
2018
- 2018-12-05 CN CN201811480886.9A patent/CN109574304A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120113351A (en) * | 2011-04-05 | 2012-10-15 | 허재수 | Manufacturing method of calcium phosphate using waste water |
| CN103213962A (en) * | 2013-04-19 | 2013-07-24 | 武汉工程大学 | Method for preparing feed-grade calcium hydrophosphate from phosphoric acid-containing mixed acid etching waste liquid |
| CN104445730A (en) * | 2014-11-21 | 2015-03-25 | 贵阳中化开磷化肥有限公司 | Comprehensive utilization method of wastewater containing phosphorus and fluorine |
| CN106276837A (en) * | 2016-08-15 | 2017-01-04 | 东江环保股份有限公司 | Phosphoric acid waste liquid prepares the method for calcium hydrophosphate fodder |
| CN106829904A (en) * | 2017-02-28 | 2017-06-13 | 连云港市德邦精细化工有限公司 | A kind of preparation method of graininess calcium phosphate dibasic anhydrous |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114684967A (en) * | 2022-04-06 | 2022-07-01 | 深圳大学 | Synergistic treatment method for calcareous solid waste and phosphorus-containing waste liquid and application of product thereof |
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