CN104628086A - Novel phosphorus removal method for alkaline leaching solution containing molybdenum and vanadium - Google Patents
Novel phosphorus removal method for alkaline leaching solution containing molybdenum and vanadium Download PDFInfo
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- CN104628086A CN104628086A CN201510004158.0A CN201510004158A CN104628086A CN 104628086 A CN104628086 A CN 104628086A CN 201510004158 A CN201510004158 A CN 201510004158A CN 104628086 A CN104628086 A CN 104628086A
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- resin
- immersion liquid
- neutral
- washing
- molybdenum vanadium
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Abstract
The invention discloses a novel phosphorus removal method for an alkaline leaching solution containing molybdenum and vanadium. The novel phosphorus removal method comprises the following steps: resin pretreatment: a, cleaning resin with deionized water until no turbid color, b, soaking with low-concentration NaOH, stirring, and washing to be neutral, c, soaking with HCl, stirring and washing to be neutral, d, soaking with NaOH, stirring so as to convert resin into OH- type, and e, washing the resin with deionized water to be neutral, and packing into an ion exchange column; resin adsorption: adsorbing phosphorus in the molybdenum-vanadium alkaline leaching solution with the pretreated resin; resin analysis: eluting the resin with aqueous ammonia, and simultaneously finishing regeneration of the resin; and concentrating and crystallizing the generated ammonium phosphate solution for later use in preparation of a phosphate fertilizer. The technology system is simple, energy-saving, environment-friendly, and free of pollution; resources can be recycled; and the problems that the molybdenum-vanadium alkaline leaching solution is not thorough in phosphorus removal, large in dephosphorization slag amount and low in cost, and environmental pollution is easily caused are effectively solved.
Description
Technical field
The present invention relates to a kind of phosphorus removing method, particularly a kind of containing molybdenum vanadium alkali immersion liquid Novel dephosphorization method.
Background technology
Dephosphorization technique has multiple, be applied to the dephosphorization mainly chemical precipitation method containing the immersion liquid of molybdenum vanadium alkali at present, according to the basis that chemical precipitating is reacted, in order to generate phosphate compounds, for chemical agent mainly metal-salt medicament and the calcium hydroxide (white lime) of chemical dephosphorization.After in many high volence metal ion adding of agents to solution, all can generate the compound of insoluble with the dissolved phosphorus ionic bond in solution.For economic reasons, for the metal-salt medicament mainly Fe of phosphorus precipitating
3+, Al
3+and Mg
2+salt and lime.These medicaments use with solution and suspension.Reaction formula is as follows:
Ca
2++PO
4 3-→Ca
3(PO
4)
2
Al
3++PO
4 3-→AlPO
4↓pH=6～7
Fe
3++PO
4 3-→FePO
4↓pH=5～5.5
Mg
2++PO
4 3-→Ca
3(PO
4)
2。
Shortcoming is with not enough: precipitator method dephosphorization is large by doses, and processing costs is high, produces a large amount of chemical sludge, conducts oneself well to comprehend cause environmental pollution as improper, and phosphor-removing effect can only reach 20ppm containing the immersion liquid of molybdenum vanadium alkali.
Summary of the invention
The object of this invention is to provide a kind ofly save that material, cost are low, environmental protection, phosphor-removing effect are good containing molybdenum vanadium alkali immersion liquid Novel dephosphorization method, overcome the deficiencies in the prior art.
Of the present invention containing molybdenum vanadium alkali immersion liquid Novel dephosphorization method, step is as follows:
(1) resin pre-treatment:
A. with deionized water, resin is cleaned extremely without muddy look;
B. soak with lower concentration NaOH and stir, washing is to neutral;
C. soak with HCl and stir, washing is to neutral;
D. soak with NaOH and stir, making resin be converted to OH
-type;
E. with deionized water, resin wash is become neutral, load ion exchange column;
(2) resin absorption, adsorbs phosphorus in the immersion liquid of molybdenum vanadium alkali with pretreated resin;
(3) resin is resolved, resin ammonia soln drip washing, and resin completes regeneration simultaneously; Condensing crystal is carried out to the ammonium phosphate solution generated.
Described resin is the gel-type anion exchange resin of the phosphate radical in the immersion liquid of alternative absorption molybdenum vanadium alkali.
Described resin absorption condition is: the pH value of feeding liquid is 6.5 ~ 8.5, and flow velocity is 0.2 ~ 2 times of column volume, and control feed liquid and resin contact time are 30 ~ 300 minutes, when effluent liquid phosphorus content reaches 2ppm, stops absorption.
Ammonia soln concentration used resolved by described resin is 4% ~ 5%.
Method process system of the present invention is simple, and technical process is ingenious, compares with traditional molybdenum vanadium alkali immersion liquid dephosphorizing technology, energy-saving and environmental protection, pollution-free, can resource circulation utilization.Efficiently solve containing molybdenum vanadium immersion liquid dephosphorization not thorough, the dephosphorization quantity of slag is large, easily causes environmental pollution, the problem that cost is high.
Embodiment
The resin applied in method of the present invention is gel-type anion exchange resin, can exchange containing phosphonium ion a small amount of in the immersion liquid of molybdenum vanadium alkali and molybdenum vanadium metal ion isolation, resolve with ammonia soln spray, generate ammonium phosphate solution, after desorbed solution reaches finite concentration, condensing crystal, production phosphate fertilizer for subsequent use, simultaneously resin completes regeneration.Ion-exchange dephosphorization resin adopts sorbing material vinylbenzene SG resin being made to phosphorus.Outward appearance; The opaque particle of oyster white.Wet true density is 1.05 ~ 1.10g/L, and complete exchange capacity is greater than 2.5mmol/g, mean pore size 100nm.The scope of application: containing the immersion liquid of molybdenum vanadium metal ion alkali.Its dephosphorization process is as follows:
(1) resin pre-treatment:
A. with deionized water, resin is cleaned extremely without muddy look;
B. soak with lower concentration NaOH and stir, washing is to neutral;
C. soak with HCl and stir, washing is to neutral;
D. soak with NaOH and stir, making resin be converted to OH
-type;
E. with deionized water, resin wash is become neutral, load ion exchange column.
(2) resin absorption, adsorbs phosphorus in the immersion liquid of molybdenum vanadium alkali with pretreated resin.
(3) resin is resolved, resin ammonia soln drip washing, and resin completes regeneration simultaneously.After ammonium phosphate solution reaches finite concentration, condensing crystal, production phosphate fertilizer for subsequent use.
Specific embodiment is as follows:
Embodiment 1
Utilize a collection of 500L of process of the present invention containing the immersion liquid of molybdenum vanadium alkali, wherein phosphorus concentration 1.87g/L.
1, resin pre-treatment
First by step, resin is carried out pre-treatment:
A. with deionized water, resin is cleaned extremely without muddy look;
B. soak with lower concentration NaOH and stir, washing is to neutral;
C. soak with HCl and stir, washing is to neutral;
D. soak with NaOH and stir, making resin be converted to OH
-type;
E. with deionized water, resin wash is become neutral, load ion exchange column.
2, resin absorption
Adopt five resin column series connection, wherein four absorption, a drip washing, utilize pretreated resin to adsorb containing phosphorus in the immersion liquid of molybdenum vanadium alkali.Regulate immersion liquid pH value to be 6.5, control material inlet valve and make flow velocity be 0.2 times of column volume, after testing, feed liquid and resin contact are after 265 minutes, and effluent liquid phosphorus content reaches more than 2ppm (wearing a little), and resin absorption is saturated, stop absorption immediately.
3, regeneration resolved by resin
The ammonia soln drip washing with 4% resolved by resin, and resin completes regeneration simultaneously.After the ammonium phosphate solution generated reaches finite concentration, condensing crystal, production phosphate fertilizer for subsequent use.
Be 0.0009g/L containing the phosphorus concentration after molybdenum vanadium alkali immersion liquid dephosphorization, clearance is 99.95%.Whole process does not have dephosphorized slag to produce, and does not pollute environment.
Embodiment 2
Utilize a collection of 1700L of process of the present invention containing the immersion liquid of molybdenum vanadium alkali, wherein phosphorus concentration 2.22g/L.
1 resin pre-treatment
First by step, resin is carried out pre-treatment:
A. with deionized water, resin is cleaned extremely without muddy look;
B. soak with lower concentration NaOH and stir, washing is to neutral;
C. soak with HCl and stir, washing is to neutral;
D. soak with NaOH and stir, making resin be converted to OH
-type;
E. with deionized water, resin wash is become neutral, load ion exchange column.
2, resin absorption
Adopt five resin column series connection, wherein four absorption, a drip washing, utilize pretreated resin to adsorb containing phosphorus in the immersion liquid of molybdenum vanadium alkali.Regulate immersion liquid pH value to be 7, control material inlet valve and make flow velocity be 0.5 times of column volume, after testing, feed liquid and resin contact are after 190 minutes, and effluent liquid phosphorus content reaches more than 2ppm (wearing a little), and resin absorption is saturated, stop absorption immediately.
3, regeneration resolved by resin
The ammonia soln drip washing with 4.2% resolved by resin, and resin completes regeneration simultaneously.After finite concentration is reached to the ammonium phosphate solution generated, condensing crystal, production phosphate fertilizer for subsequent use.
Be 0.0011 g/L containing the phosphorus concentration after molybdenum vanadium alkali immersion liquid dephosphorization, clearance is 99.95%.Whole process does not have dephosphorized slag to produce, and does not pollute environment.
Embodiment 3
Utilize a collection of 2800L of process of the present invention containing the immersion liquid of molybdenum vanadium alkali, wherein phosphorus concentration 2.10g/L.
1 resin pre-treatment
First by step, resin is carried out pre-treatment:
A. with deionized water, resin is cleaned extremely without muddy look;
B. soak with lower concentration NaOH and stir, washing is to neutral;
C. soak with HCl and stir, washing is to neutral;
D. soak with NaOH and stir, making resin be converted to OH
-type;
E. with deionized water, resin wash is become neutral, load ion exchange column.
2, resin absorption
Adopt five resin column series connection, wherein four absorption, a drip washing, utilize pretreated resin to adsorb containing phosphorus in the immersion liquid of molybdenum vanadium alkali.Regulate immersion liquid pH value to be 7.5, control material inlet valve and make flow velocity be 1 times of column volume, after testing, feed liquid and resin contact are after 160 minutes, and effluent liquid phosphorus content reaches more than 2ppm (wearing a little), and resin absorption is saturated, stop absorption immediately.
3, regeneration resolved by resin
The ammonia soln drip washing with 4.4% resolved by resin, and resin completes regeneration simultaneously.After finite concentration is reached to the ammonium phosphate solution generated, condensing crystal, production phosphate fertilizer for subsequent use.
Be 0.0008 g/L containing the phosphorus concentration after molybdenum vanadium alkali immersion liquid dephosphorization, clearance is 99.96%.Whole process does not have dephosphorized slag to produce, and does not pollute environment.
Embodiment 4
Utilize a collection of 4000L of process of the present invention containing the immersion liquid of molybdenum vanadium alkali, wherein phosphorus concentration 1.89g/L.
1 resin pre-treatment
First by step, resin is carried out pre-treatment:
A. with deionized water, resin is cleaned extremely without muddy look;
B. soak with lower concentration NaOH and stir, washing is to neutral;
C. soak with HCl and stir, washing is to neutral;
D. soak with NaOH and stir, making resin be converted to OH
-type;
E. with deionized water, resin wash is become neutral, load ion exchange column.
2, resin absorption
Adopt five resin column series connection, wherein four absorption, a drip washing, utilize pretreated resin to adsorb containing phosphorus in the immersion liquid of molybdenum vanadium alkali.Regulate immersion liquid pH value to be 8, control material inlet valve and make flow velocity be 1.5 times of column volumes, after testing, feed liquid and resin contact are after 110 minutes, and effluent liquid phosphorus content reaches more than 2ppm (wearing a little), and resin absorption is saturated, stop absorption immediately.
3, regeneration resolved by resin
The ammonia soln drip washing with 4.7% resolved by resin, and resin completes regeneration simultaneously.After finite concentration is reached to the ammonium phosphate solution generated, condensing crystal, production phosphate fertilizer for subsequent use.
Be 0.0012 g/L containing the phosphorus concentration after molybdenum vanadium alkali immersion liquid dephosphorization, clearance is 99.94%.Whole process does not have dephosphorized slag to produce, and does not pollute environment.
Embodiment 5
Utilize a collection of 5000L of process of the present invention containing the immersion liquid of molybdenum vanadium alkali, wherein phosphorus concentration 1.97g/L.
1 resin pre-treatment
First by step, resin is carried out pre-treatment:
A. with deionized water, resin is cleaned extremely without muddy look;
B. soak with lower concentration NaOH and stir, washing is to neutral;
C. soak with HCl and stir, washing is to neutral;
D. soak with NaOH and stir, making resin be converted to OH
-type;
E. with deionized water, resin wash is become neutral, load ion exchange column.
2, resin absorption
Adopt five resin column series connection, wherein four absorption, a drip washing, utilize pretreated resin to adsorb containing phosphorus in the immersion liquid of molybdenum vanadium alkali.Regulate immersion liquid pH value to be 8.5, control material inlet valve and make flow velocity be 2 times of column volumes, after testing, feed liquid and resin contact are after 84 minutes, and effluent liquid phosphorus content reaches more than 2ppm (wearing a little), and resin absorption is saturated, stop absorption immediately.
3, regeneration resolved by resin
The ammonia soln drip washing with 5% resolved by resin, and resin completes regeneration simultaneously.After finite concentration is reached to the ammonium phosphate solution generated, condensing crystal, production phosphate fertilizer for subsequent use.
Be 0.0007 g/L containing the phosphorus concentration after molybdenum vanadium alkali immersion liquid dephosphorization, clearance is 99.96%.Whole process does not have dephosphorized slag to produce, and does not pollute environment.
Claims (4)
1., containing a molybdenum vanadium alkali immersion liquid Novel dephosphorization method, it is characterized in that: step is as follows:
(1) resin pre-treatment:
A. with deionized water, resin is cleaned extremely without muddy look;
B. soak with lower concentration NaOH and stir, washing is to neutral;
C. soak with HCl and stir, washing is to neutral;
D. soak with NaOH and stir, making resin be converted to OH
-type;
E. with deionized water, resin wash is become neutral, load ion exchange column;
(2) resin absorption, adsorbs phosphorus in the immersion liquid of molybdenum vanadium alkali with pretreated resin;
(3) resin is resolved, resin ammonia soln drip washing, and resin completes regeneration simultaneously.
2. as claimed in claim 1 containing molybdenum vanadium alkali immersion liquid Novel dephosphorization method, it is characterized in that: described resin is the gel-type anion exchange resin of the phosphate radical in the immersion liquid of alternative absorption molybdenum vanadium alkali.
3. as claimed in claim 1 or 2 containing molybdenum vanadium alkali immersion liquid Novel dephosphorization method, it is characterized in that: described resin absorption condition is: the pH value of feeding liquid is 6.5 ~ 8.5, flow velocity is 0.2 ~ 2 times of column volume, control feed liquid and resin contact time are 30 ~ 300 minutes, when effluent liquid phosphorus content reaches 2ppm, stop absorption.
4. as claimed in claim 3 containing molybdenum vanadium alkali immersion liquid Novel dephosphorization method, it is characterized in that: ammonia soln concentration used resolved by described resin is 4% ~ 5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510004158.0A CN104628086A (en) | 2015-01-06 | 2015-01-06 | Novel phosphorus removal method for alkaline leaching solution containing molybdenum and vanadium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510004158.0A CN104628086A (en) | 2015-01-06 | 2015-01-06 | Novel phosphorus removal method for alkaline leaching solution containing molybdenum and vanadium |
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ID=53207394
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|---|---|---|---|
| CN201510004158.0A Pending CN104628086A (en) | 2015-01-06 | 2015-01-06 | Novel phosphorus removal method for alkaline leaching solution containing molybdenum and vanadium |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104907108A (en) * | 2015-05-26 | 2015-09-16 | 安徽皖东树脂科技有限公司 | Pretreatment method of anion exchange resin |
| CN107500353A (en) * | 2017-09-19 | 2017-12-22 | 芜湖人本合金有限责任公司 | High-purity sodium metavanadate and preparation method thereof |
| CN115739209A (en) * | 2022-12-13 | 2023-03-07 | 山东省鲁洲食品集团有限公司 | Recovery method of anion exchange resin for starch sugar |
| CN115739209B (en) * | 2022-12-13 | 2024-04-30 | 山东省鲁洲食品集团有限公司 | Method for resuscitating starch sugar by using anion exchange resin |
Citations (4)
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|---|---|---|---|---|
| US20070246419A1 (en) * | 2006-04-20 | 2007-10-25 | Water Security Corporation | Compositions and methods for fluid purification |
| CN101254966A (en) * | 2008-04-14 | 2008-09-03 | 北京特斯顿新材料技术发展有限公司 | Recovery method of phosphate discharge liquid |
| CN101343093A (en) * | 2008-09-03 | 2009-01-14 | 南京大学 | Method for deeply purifying minim phosphor in water with composite resin |
| CN102774929A (en) * | 2012-07-06 | 2012-11-14 | 华南师范大学 | Method for recovering phosphor from eutrophic water |
-
2015
- 2015-01-06 CN CN201510004158.0A patent/CN104628086A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070246419A1 (en) * | 2006-04-20 | 2007-10-25 | Water Security Corporation | Compositions and methods for fluid purification |
| CN101254966A (en) * | 2008-04-14 | 2008-09-03 | 北京特斯顿新材料技术发展有限公司 | Recovery method of phosphate discharge liquid |
| CN101343093A (en) * | 2008-09-03 | 2009-01-14 | 南京大学 | Method for deeply purifying minim phosphor in water with composite resin |
| CN102774929A (en) * | 2012-07-06 | 2012-11-14 | 华南师范大学 | Method for recovering phosphor from eutrophic water |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104907108A (en) * | 2015-05-26 | 2015-09-16 | 安徽皖东树脂科技有限公司 | Pretreatment method of anion exchange resin |
| CN107500353A (en) * | 2017-09-19 | 2017-12-22 | 芜湖人本合金有限责任公司 | High-purity sodium metavanadate and preparation method thereof |
| CN115739209A (en) * | 2022-12-13 | 2023-03-07 | 山东省鲁洲食品集团有限公司 | Recovery method of anion exchange resin for starch sugar |
| CN115739209B (en) * | 2022-12-13 | 2024-04-30 | 山东省鲁洲食品集团有限公司 | Method for resuscitating starch sugar by using anion exchange resin |
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