CN102229454A - Technology for preparing phosphate product with phosphorus-containing wastewater - Google Patents
Technology for preparing phosphate product with phosphorus-containing wastewater Download PDFInfo
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- CN102229454A CN102229454A CN 201110109878 CN201110109878A CN102229454A CN 102229454 A CN102229454 A CN 102229454A CN 201110109878 CN201110109878 CN 201110109878 CN 201110109878 A CN201110109878 A CN 201110109878A CN 102229454 A CN102229454 A CN 102229454A
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Abstract
The invention discloses a technology for preparing a phosphate product with phosphorus-containing wastewater. Specifically, the technology comprises the steps of: a. heating the phosphorus-containing wastewater to a temperature of 75-85 DEG C, adding ammonia salt gradually until the PH value of the wastewater reaches 4-7, then conducting a metathesis reaction in which the conversion rate of waste phosphoric acid can reach over 98%, thus generating an ammonium dihydrogen phosphate solution; b. adding a decolorizer which accounts for 3%-5% of the gross weight of the phosphorus-containing wastewater into the reacted solution for decolouring; c. filtering the ammonium dihydrogen phosphate solution after decolouring; d. subjecting the filtered ammonium dihydrogen phosphate solution to cooling, crystallization, centrifugation and drying, thus obtaining a finished product. With simple processes, the technology of the invention makes good use of waste materials and protects the environment.
Description
Technical field
Chemical field of the present invention relates to a kind of industrial wastewater treatment and waste water resource and utilizes technology again.Be specifically related to a kind of technology of utilizing phosphorus-containing wastewater to produce the series of phosphate product.
Background technology
Phosphoric acid is the important source material of producing the series of phosphate product, because the phosphoric acid price is expensive, causes the series of phosphate production cost of products quite high.
And in the process of producing synthetic perfume, medicine, chemical industry agricultural chemicals, can produce a large amount of phosphorus-containing wastewaters, and these waste water generally all are to run off in vain, manufacturing enterprise does not deal with, and directly influences the development of enterprise.The a large amount of phosphorus-containing wastewaters that spill out simultaneously cause very big harm to environment.So these phosphorus-containing wastewaters of what use is made of become the problem of needing solution at present badly.
Summary of the invention
At existing problem in the background technology, the invention provides a kind of not only environmental protection but also can effectively utilize the technology of the preparation phosphate product of waste water.
The objective of the invention is to utilize to produce and produce a large amount of phosphorus-containing wastewaters in synthetic perfume, medicine intermediate, the chemical color process; from above-mentioned phosphorus-containing wastewater, extract phosphoric acid and transform the series of phosphate product; make deleterious phosphorus-containing wastewater be converted into useful resource; above-mentioned manufacturing enterprise has been developed production; to social protection environment; manufacturers has reduced production cost to phosphate product, increases economic efficiency, and reaches three purposes of winning.
The technical solution used in the present invention is as follows: a kind of technology of utilizing phosphorus-containing wastewater to prepare phosphate product, and concrete steps are as follows: a kind of technology of utilizing phosphorus-containing wastewater to prepare phosphate product, concrete steps are as follows:
A, phosphorus-containing wastewater is heated to 80 ± 5 ℃, progressively add ammonia salt and carry out replacement(metathesis)reaction until reaching under the condition that pH value is 4-7, generate the biphosphate amine aqueous solution, the waste phosphoric acid transformation efficiency reaches more than 98% in reaction;
B, in reacted solution, add the discoloring agent of the 3%-5% account for the phosphorus-containing wastewater gross weight, decolour;
After c, decolouring are finished, the biphosphate amine aqueous solution is filtered;
D, the biphosphate amine aqueous solution after will filtering cool off, crystallization, centrifugal and dry after finished product.
Preferably, among the step a phosphorus-containing wastewater is heated to 80 ± 5 ℃, progressively add ammonia salt and carry out replacement(metathesis)reaction, generate the biphosphate amine aqueous solution until reaching under the condition that pH value is 4-5.
Preferably, the ammonium salt among the step a is a bicarbonate of ammonia.
Preferably, the discoloring agent among the step b is a gac.
Preferably, the discoloring agent among the step b is that mass ratio is a wilkinite: the mixture of hydrogen peroxide: potassium permanganate=3:2:1.
Preferably, the crystallisation by cooling process in the steps d is as follows: the biphosphate amine aqueous solution after will filtering is put into reactor, and reactor is taked coil pipe heating, stirring, air draught, the mode that froths, and reaches 100～110 ℃ in temperature, cools off behind mother-in-law U.S. degree 35, crystallization.
Preferably, the centrifugal and drying process in the steps d is as follows: it is centrifugal that fluidised form work in-process after the crystallization are passed to whizzer, extrudes moisture content, when water content has 3%～5%, discharging approximately; Will be after the centrifugal discharge input drying machine drying or drying room oven dry, dry by the fire to the product water content be 0.2%～0.3%, be finished product.
The present invention has following beneficial effect: treatment of Phosphorus Containing Waste Water technology of the present invention, phosphorus-containing wastewater is effectively changed into useful biphosphate ammonium fertilizer, and not only finish the task of refuse reclamation, and helped environment protection.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The invention will be further described below in conjunction with accompanying drawing and specific embodiment.The following all embodiment of the present invention all operate according to schema as shown in Figure 1.
Embodiment 1
A kind of technology of utilizing phosphorus-containing wastewater to prepare phosphate product, concrete steps are as follows:
1,1 ton of phosphorus-containing wastewater is heated to 80 ± 5 ℃, progressively add bicarbonate of ammonia and until pH value be under 4 the condition and carry out replacement(metathesis)reaction, generate the biphosphate amine aqueous solution, the waste phosphoric acid transformation efficiency reaches more than 98% in reaction;
2, in reacted solution, add the discoloring agent gac of 30kg, decolour;
3, after decolouring is finished, the biphosphate amine aqueous solution is filtered;
4, the biphosphate amine aqueous solution after will filtering is squeezed into concentrated cobalt (being reactor), concentrated cobalt is taked the coil pipe heating, stirring, air draught when temperature reaches 100～110 ℃, froth, stirring velocity is 80～100 rev/mins, suction air volume is 9000 cubic metres/hour, cools off after mother-in-law U.S. degree is 35, crystallization;
5, after the crystallization fluidised form work in-process to be passed to whizzer centrifugal, extrude moisture content, when water content has 3%～5%, discharging approximately;
6, input drying machine drying or drying room oven dry after the centrifugal discharge, dry by the fire to the product water content be 0.2%～0.3%, can be packaged into qualified phosphoric acid dihydro amine.
Embodiment 2
A kind of technology of utilizing phosphorus-containing wastewater to prepare phosphate product, concrete steps are as follows:
1,1 ton of phosphorus-containing wastewater is heated to 80 ± 5 ℃, add bicarbonate of ammonia and until pH value be under 5 the condition and carry out replacement(metathesis)reaction, generate the biphosphate amine aqueous solution, the waste phosphoric acid transformation efficiency reaches more than 98% in reaction;
2, in reacted solution, add the discoloring agent gac of 40kg, decolour;
3, after decolouring is finished, the biphosphate amine aqueous solution is filtered;
4, the biphosphate amine aqueous solution after will filtering is squeezed into concentrated cobalt (being reactor), concentrated cobalt is taked the coil pipe heating, stirring, air draught when temperature reaches 100～110 ℃, froth, stirring velocity is 80～100 rev/mins, suction air volume is 9000 cubic metres/hour, cools off after mother-in-law U.S. degree is 35, crystallization;
5, after the crystallization fluidised form work in-process to be passed to whizzer centrifugal, extrude moisture content, when water content has 3%～5%, discharging approximately;
6, input drying machine drying or drying room oven dry after the centrifugal discharge, dry by the fire to the product water content be 0.2%～0.3%, can be packaged into qualified phosphoric acid dihydro amine.
Embodiment 3
A kind of technology of utilizing phosphorus-containing wastewater to prepare phosphate product, concrete steps are as follows:
1,1 ton of phosphorus-containing wastewater is heated to 80 ± 5 ℃, add bicarbonate of ammonia and until pH value be under 4.5 the condition and carry out replacement(metathesis)reaction, generate the biphosphate amine aqueous solution, the waste phosphoric acid transformation efficiency reaches more than 98% in reaction;
2, in reacted solution, add the discoloring agent gac of 50kg, decolour;
3, after decolouring is finished, the biphosphate amine aqueous solution is filtered;
4, the biphosphate amine aqueous solution after will filtering is squeezed into concentrated cobalt (being reactor), concentrated cobalt is taked the coil pipe heating, stirring, air draught when temperature reaches 100～110 ℃, froth, stirring velocity is 80～100 rev/mins, suction air volume is 9000 cubic metres/hour, cools off after mother-in-law U.S. degree is 35, crystallization;
5, after the crystallization fluidised form work in-process to be passed to whizzer centrifugal, extrude moisture content, when water content has 3%～5%, discharging approximately;
6, input drying machine drying or drying room oven dry after the centrifugal discharge, dry by the fire to the product water content be 0.2%～0.3%, can be packaged into qualified phosphoric acid dihydro amine.
Embodiment 4
A kind of technology of utilizing phosphorus-containing wastewater to prepare phosphate product, concrete steps are as follows:
1,1 ton of phosphorus-containing wastewater is heated to 80 ± 5 ℃, add bicarbonate of ammonia and until pH value be under 6 the condition and carry out replacement(metathesis)reaction, generate the biphosphate amine aqueous solution, the waste phosphoric acid transformation efficiency reaches more than 98% in reaction;
2, in reacted solution, add the discoloring agent gac of 50kg, decolour;
3, after decolouring is finished, the biphosphate amine aqueous solution is filtered;
4, the biphosphate amine aqueous solution after will filtering is squeezed into concentrated cobalt (being reactor), concentrated cobalt is taked the coil pipe heating, stirring, air draught when temperature reaches 100～110 ℃, froth, stirring velocity is 80～100 rev/mins, suction air volume is 9000 cubic metres/hour, cools off after mother-in-law U.S. degree is 35, crystallization;
5, after the crystallization fluidised form work in-process to be passed to whizzer centrifugal, extrude moisture content, when water content has 3%～5%, discharging approximately;
6, input drying machine drying or drying room oven dry after the centrifugal discharge, dry by the fire to the product water content be 0.2%～0.3%, can be packaged into qualified phosphoric acid dihydro amine.
Embodiment 5
A kind of technology of utilizing phosphorus-containing wastewater to prepare phosphate product, concrete steps are as follows:
1,1 ton of phosphorus-containing wastewater is heated to 80 ± 5 ℃, add bicarbonate of ammonia and until pH value be under 4.5 the condition and carry out replacement(metathesis)reaction, generate the biphosphate amine aqueous solution, the waste phosphoric acid transformation efficiency reaches more than 98% in reaction;
2, the discoloring agent of adding 40kg decolours in reacted solution, and described discoloring agent is that mass ratio is a wilkinite: the mixture of hydrogen peroxide: potassium permanganate=3:2:1;
3, after decolouring is finished, the biphosphate amine aqueous solution is filtered;
4, the biphosphate amine aqueous solution after will filtering is squeezed into concentrated cobalt (being reactor), concentrated cobalt is taked the coil pipe heating, stirring, air draught when temperature reaches 100～110 ℃, froth, stirring velocity is 80～100 rev/mins, suction air volume is 9000 cubic metres/hour, cools off after mother-in-law U.S. degree is 35, crystallization;
5, after the crystallization fluidised form work in-process to be passed to whizzer centrifugal, extrude moisture content, when water content has 3%～5%, discharging approximately;
6, input drying machine drying or drying room oven dry after the centrifugal discharge, dry by the fire to the product water content be 0.2%～0.3%, can be packaged into qualified phosphoric acid dihydro amine.
Embodiment 6
A kind of technology of utilizing phosphorus-containing wastewater to prepare phosphate product, concrete steps are as follows:
1,1 ton of phosphorus-containing wastewater is heated to 80 ± 5 ℃, add bicarbonate of ammonia and until pH value be under 5 the condition and carry out replacement(metathesis)reaction, generate the biphosphate amine aqueous solution, the waste phosphoric acid transformation efficiency reaches more than 98% in reaction;
2, the discoloring agent of adding 30kg decolours in reacted solution, and described discoloring agent is that mass ratio is a wilkinite: the mixture of hydrogen peroxide: potassium permanganate=3:2:1;
3, after decolouring is finished, the biphosphate amine aqueous solution is filtered;
4, the biphosphate amine aqueous solution after will filtering is squeezed into concentrated cobalt (being reactor), concentrated cobalt is taked the coil pipe heating, stirring, air draught when temperature reaches 100～110 ℃, froth, stirring velocity is 80～100 rev/mins, suction air volume is 9000 cubic metres/hour, cools off after mother-in-law U.S. degree is 35, crystallization;
5, after the crystallization fluidised form work in-process to be passed to whizzer centrifugal, extrude moisture content, when water content has 3%～5%, discharging approximately;
6, input drying machine drying or drying room oven dry after the centrifugal discharge, dry by the fire to the product water content be 0.2%～0.3%, can be packaged into qualified phosphoric acid dihydro amine.
Embodiment 7
A kind of technology of utilizing phosphorus-containing wastewater to prepare phosphate product, concrete steps are as follows:
1,1 ton of phosphorus-containing wastewater is heated to 80 ± 5 ℃, add bicarbonate of ammonia and until pH value be under 4 the condition and carry out replacement(metathesis)reaction, generate the biphosphate amine aqueous solution, the waste phosphoric acid transformation efficiency reaches more than 98% in reaction;
2, the discoloring agent of adding 50kg decolours in reacted solution, and described discoloring agent is that mass ratio is a wilkinite: the mixture of hydrogen peroxide: potassium permanganate=3:2:1;
3, after decolouring is finished, the biphosphate amine aqueous solution is filtered;
4, the biphosphate amine aqueous solution after will filtering is squeezed into concentrated cobalt (being reactor), concentrated cobalt is taked the coil pipe heating, stirring, air draught when temperature reaches 100～110 ℃, froth, stirring velocity is 80～100 rev/mins, suction air volume is 9000 cubic metres/hour, cools off after mother-in-law U.S. degree is 35, crystallization;
5, after the crystallization fluidised form work in-process to be passed to whizzer centrifugal, extrude moisture content, when water content has 3%～5%, discharging approximately;
6, input drying machine drying or drying room oven dry after the centrifugal discharge, dry by the fire to the product water content be 0.2%～0.3%, can be packaged into qualified phosphoric acid dihydro amine.
Claims (7)
1. technology of utilizing phosphorus-containing wastewater to prepare phosphate product is characterized in that concrete steps are as follows:
A, phosphorus-containing wastewater is heated to 80 ± 5 ℃, progressively add ammonia salt and carry out replacement(metathesis)reaction until reaching under the condition that pH value is 4-7, generate the biphosphate amine aqueous solution, the waste phosphoric acid transformation efficiency reaches more than 98% in reaction;
B, in reacted solution, add the discoloring agent of the 3%-5% account for the phosphorus-containing wastewater gross weight, decolour;
After c, decolouring are finished, the biphosphate amine aqueous solution is filtered;
D, the biphosphate amine aqueous solution after will filtering cool off, crystallization, centrifugal and dry after finished product.
2. the technology of utilizing phosphorus-containing wastewater to prepare phosphate product as claimed in claim 1, it is characterized in that: among the step a phosphorus-containing wastewater is heated to 80 ± 5 ℃, progressively add ammonia salt and carry out replacement(metathesis)reaction, generate the biphosphate amine aqueous solution until reaching under the condition that pH value is 4-5.
3. the technology of utilizing phosphorus-containing wastewater to prepare phosphate product as claimed in claim 1 or 2 is characterized in that: the ammonium salt among the step a is a bicarbonate of ammonia.
4. the technology of utilizing phosphorus-containing wastewater to prepare phosphate product as claimed in claim 1 or 2 is characterized in that: the discoloring agent among the step b is a gac.
5. the technology of utilizing phosphorus-containing wastewater to prepare phosphate product as claimed in claim 1 or 2 is characterized in that: the discoloring agent among the step b is that mass ratio is a wilkinite: the mixture of hydrogen peroxide: potassium permanganate=3:2:1.
6. the technology of utilizing phosphorus-containing wastewater to prepare phosphate product as claimed in claim 1 or 2, it is characterized in that: the crystallisation by cooling process in the steps d is as follows: the biphosphate amine aqueous solution after will filtering is put into reactor, reactor is taked coil pipe heating, stirring, air draught, mode froths, reach 100～110 ℃ in temperature, cool off behind mother-in-law U.S. degree 35, crystallization.
7. the technology of utilizing phosphorus-containing wastewater to prepare phosphate product as claimed in claim 1 or 2, it is characterized in that: the centrifugal and drying process in the steps d is as follows: it is centrifugal that fluidised form work in-process after the crystallization are passed to whizzer, extrude moisture content, when water content has 3%～5%, discharging approximately; Will be after the centrifugal discharge input drying machine drying or drying room oven dry, dry by the fire to the product water content be 0.2%～0.3%, be finished product.
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| CN 201110109878 CN102229454A (en) | 2011-04-29 | 2011-04-29 | Technology for preparing phosphate product with phosphorus-containing wastewater |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924148A (en) * | 2012-10-18 | 2013-02-13 | 大连碧城环保科技有限公司 | Process method for converting vegetable flower fertilizer by waste industrial phosphating solution |
| CN105967417A (en) * | 2016-05-19 | 2016-09-28 | 浙江永泉化学有限公司 | Treatment method of phosphorus-containing wastewater |
| CN106829897A (en) * | 2017-01-03 | 2017-06-13 | 浙江新化化工股份有限公司 | A kind of method that phosphate ester-containing and phosphite ester waste liquid prepare phosphate fertilizer |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1128477A (en) * | 1997-07-10 | 1999-02-02 | Kurita Water Ind Ltd | Phosphorus removing method |
| CN1597545A (en) * | 2004-08-20 | 2005-03-23 | 清华大学 | Phosphorus containing waste water treatment method and its application of recovered phosphorus product |
| CN101786744A (en) * | 2010-03-08 | 2010-07-28 | 昆明理工大学 | Method for directly utilizing waste liquor containing phosphoric acid and phosphorous acid |
| CN101798074A (en) * | 2010-03-12 | 2010-08-11 | 昆明理工大学 | Method for using yellow phosphorus-refined dearsenization waste liquid |
-
2011
- 2011-04-29 CN CN 201110109878 patent/CN102229454A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1128477A (en) * | 1997-07-10 | 1999-02-02 | Kurita Water Ind Ltd | Phosphorus removing method |
| CN1597545A (en) * | 2004-08-20 | 2005-03-23 | 清华大学 | Phosphorus containing waste water treatment method and its application of recovered phosphorus product |
| CN101786744A (en) * | 2010-03-08 | 2010-07-28 | 昆明理工大学 | Method for directly utilizing waste liquor containing phosphoric acid and phosphorous acid |
| CN101798074A (en) * | 2010-03-12 | 2010-08-11 | 昆明理工大学 | Method for using yellow phosphorus-refined dearsenization waste liquid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924148A (en) * | 2012-10-18 | 2013-02-13 | 大连碧城环保科技有限公司 | Process method for converting vegetable flower fertilizer by waste industrial phosphating solution |
| CN105967417A (en) * | 2016-05-19 | 2016-09-28 | 浙江永泉化学有限公司 | Treatment method of phosphorus-containing wastewater |
| CN106829897A (en) * | 2017-01-03 | 2017-06-13 | 浙江新化化工股份有限公司 | A kind of method that phosphate ester-containing and phosphite ester waste liquid prepare phosphate fertilizer |
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Application publication date: 20111102 |