CN104086019A - Industrial high-concentration phosphorus-containing wastewater treatment method - Google Patents
Industrial high-concentration phosphorus-containing wastewater treatment method Download PDFInfo
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- CN104086019A CN104086019A CN201410269701.5A CN201410269701A CN104086019A CN 104086019 A CN104086019 A CN 104086019A CN 201410269701 A CN201410269701 A CN 201410269701A CN 104086019 A CN104086019 A CN 104086019A
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Abstract
The invention discloses an industrial high-concentration phosphorus-containing wastewater treatment method. The method comprises the following steps: adding a fluorine removal agent to high-concentration acidic phosphorus-containing wastewater with the P by P2O5 content of 0.15-2.2%, the F content of 0.01-0.35% and the Ca content of 0.1-0.45% to adjust the pH value of the wastewater to 4.5-6.5, allowing obtained wastewater to stand, and discharging formed fluorine-containing sludge; continuously adding a precipitating agent to the obtained upper layer clear liquid to adjust the pH value of the wastewater to 8.0-9.0, converting P to a magnesium phosphate precipitate, flocculating the obtained clear liquid to realize standard reaching emission or factory reuse; and dissolving the magnesium phosphate precipitate in fertilizer-grade phosphoric acid to obtain a P and Mg-containing mixed liquid, and carrying out metric N source addition to make struvite. The fluorine removal agent is magnesium oxide, magnesium carbonate, magnesian marble or dolomite; and the precipitating agent is magnesium hydroxide or sodium hydroxide. The wastewater treatment method has the advantages of simple process flow, good fluorine and calcium effects, and maximal recovery of the P resource on the premise that standard reaching of emitted water is guaranteed.
Description
Technical field
The present invention relates to Chemical Engineering Technology and water treatment field, relate in particular to a kind of phosphorous chemical industry wastewater treatment and reclaim the method for phosphorus.
Background technology
As the raw material of sulphur dioxide of phosphor chemical industry, Rock Phosphate (72Min BPL) generally contains the fluorine of 3-4%, all can have the generation of fluorine in the links that phosphorous chemical industry is produced, and contains especially a large amount of fluorine in phosphogypsum waste water.Fluorine is a kind of to biological and all elements of toxic effect of physical environment, and therefore sulphur dioxide of phosphor chemical industry product has strict requirement to fluorine content.Meanwhile, contain a large amount of phosphorus in the waste water such as phosphogypsum, phosphorus is the requisite element of growth and development of plants and animals, does not have phosphorus just not have lived.Phosphorus is as a kind of Nonrenewable resources, and the dynamics of exploiting is in recent years excessive, data show China current phosphate rock resource only can exploit decades again, be about to face without phosphorus available crisis.Corresponding is the water body big area eutrophication being caused by nutritive elements such as phosphorus, seriously perplexs the normal productive life of the mankind.
Under so severe situation, for vegeto-animal primary demand and the mankind's Sustainable development, the recycling of Phosphorus From Wastewater becomes our inevitable choice.From high-concentration phosphorus-containing wastewater, refuse, reclaim phosphorus, can reduce pollution on the one hand, protection of the environment, can alleviate the pressure of phosphate rock resource exploitation on the other hand, can obtain certain economic profit simultaneously, reduces production cost, achieves many things at one stroke.
The common treatment process of fluoride waste has the precipitator method, absorption method, crystallization process and reverse osmosis method etc.The conventional lime of the precipitator method, as precipitation agent, makes fluorine form Calcium Fluoride (Fluorspan) precipitation, by solid-liquid separation, fluorine is removed, and its treatment process is simple, running cost is lower, is maximum method that uses at present.But for all waste water such as very high phosphogypsum of phosphorus, fluorine and calcium contents, there is some problems in current lime treatment method: lime usage quantity and to produce the quantity of slag all larger, and the solid waste forming after processing generally will carry out landfill disposal, easily causes secondary pollution; Most importantly herein in reason method, in waste water, a large amount of phosphorus is combined with calcium and is formed calcium phosphate, causes the significant wastage of phosphor resource.
Summary of the invention
The method of wastewater treatment that a kind of defluorination deliming is effective, technique is simple, running cost is low, phosphorus recovering effect is good that the object of the invention is to overcome the shortcoming of traditional method and provide.
The technical problem underlying that the present invention need to solve realizes by following scheme.
A treatment process for industry high-concentration phosphorus-containing wastewater, is characterized in that comprising the following steps:
Step 1, will be with P
2o
5meter phosphorus content is that 0.15-2.2%, fluorine content are that the high-concentration acidic wastewater phosphorus-containing wastewater that 0.01-0.35%, calcium contents are 0.1-0.45% adds in reactor, the temperature of controlling reactor is 30-60 DEG C, constantly under stirring action, adding defluorinating agent that the pH of waste water is adjusted to 4.5-6.5, after reaction 10-30min, stop stirring, leave standstill;
Step 2, reactor bottom is formed to fluorine-containing sludge after leaving standstill and discharge, then start stirring, add precipitation agent in supernatant liquor, regulation system pH is between 8.0-9.0, and reaction stops after 10-30min stirring, and leaves standstill;
Step 3, add the throw out generating after precipitation agent to discharge and collect from reactor bottom, the clear liquid finally forming adds flocculation agent, discharge after leaving standstill;
Step 4, the throw out fertilizer grade dilute phosphoric acid of collecting in step 3 dissolve, and obtain the mixing solutions containing P and Mg, are metered into N source and prepare struvite.
Described defluorinating agent is magnesium oxide, magnesiumcarbonate, magnesite or rhombspar.
When described magnesium oxide, magnesiumcarbonate, magnesite or rhombspar use as defluorinating agent, need to be ground to 200-300 object powder.
In use, 200-300 object powder need to be added water and be made into mass concentration is 10% pulpous state liquid to defluorinating agent.
The key of described defluorinating agent result of use is to ensure its solubleness in waste water: the acidity of (1) phosphorus-containing wastewater promotes to dissolve; (2) temperature of reactor further improves the solubleness of defluorinating agent; (3) defluorinating agent is levigate and be made into pulpous state and can to a certain degree improve solubleness.
Described precipitation agent is magnesium hydroxide or sodium hydroxide.Need to be before use milled to 200-300 order as the magnesium hydroxide of precipitation agent, and to be made into mass concentration be that 10% pulpous state liquid uses.
In processing, collected throw out is in the time dissolving with fertilizer grade dilute phosphoric acid, and the add-on of acid is taking just can be by complete resolution of precipitate for the best.
The flocculation agent using in step 3 is poly-aluminium or Polyferric Sulfate, gathers aluminium or Polyferric Sulfate and all buys from market.
In this technical finesse process, add defluorinating agent after system pH raise gradually, the Ca of self in waste water
2+and F
-preferentially react, the Mg being dissolved out in defluorinating agent
2+also can promote Ca
2+removal, work as Ca
2+while being removed to a certain degree, if also have F-, its meeting and Mg in system
2+react.When removing F-in this step, also can removal system in the Ca of the overwhelming majority
2+, principal reaction is as follows:
Mg
2++2F-＝MgF
2↓
Ca
2++2F-＝CaF
2↓
H
2SiF
6+Ca
2+＝CaSiF
6↓+2H
+
2HF+Ca
2+＝CaF
2↓+2H
+
After adding precipitation agent, system mainly reacts:
3Mg
2++2PO
4 3-＝Mg
3(PO
4)
2↓
The primary product forming while adding precipitation agent in system is trimagnesium phosphate, and some undissolved magnesium hydroxide (along with pH raises, precipitation agent solvability variation), is a kind of mixture simultaneously.This mixture adds after fertilizer grade dilute phosphoric acid, can dissolve the mixing solutions becoming containing Mg and P, then supplements N source and prepares struvite, and reaction equation is as follows:
Mg
2++NH
4 ++PO
4 3-+6H
2O＝MgNH
4PO
4·6H
2O↓
Mg
2++NH
4 ++HPO
4 2-+6H
2O＝MgNH
4PO
4·6H
2O↓+H
+
Mg
2++NH
4 ++H
2PO
4 -+6H
2O＝MgNH
4PO
4·6H
2O↓+2H
+
Method of wastewater treatment technical process of the present invention is simple, and defluorination and calcium effective ensureing, under water outlet prerequisite up to standard, to reclaim to greatest extent phosphor resource.
Embodiment
Embodiment 1
(1) be 0.15% (with P by phosphorus content
2o
5meter, lower with), fluorine content is 0.01%, calcium contents is 0.1%, pH is that 2.86 phosphorus-containing wastewater 2L adds in reactor, the temperature of controlling reactor is 30 DEG C, under continuous stirring action, adding mass concentration is that 10% magnesium oxide pulpous state liquid is adjusted to 4.5 by the pH of waste water, after reaction 10min, stop stirring, leave standstill;
(2) reactor bottom is formed to fluorine-containing sludge after leaving standstill and discharge, then start stirring, in supernatant liquor, adding mass concentration is 10% magnesium hydroxide pulpous state liquid, regulation system pH to 8.0, and reaction stops after 10min stirring, and leaves standstill;
(3) add the final clear liquid addition polymerization aluminium after precipitation agent to stir rear leaving standstill, measure by analysis, after processing, clear liquid is 1.8ppm containing P content, F content is 3.2ppm, Ca content is 14.3ppm, can meet the up-to-date emission standard of phosphorous chemical industry and carry out qualified discharge, what obtain prepares struvite containing supplementing N source after P, the dissolving of Mg throw out, and the rate of recovery of phosphorus reaches 91%.
Embodiment 2
(1) the phosphogypsum slag field phosphorus-containing wastewater 3L that by phosphorus content be 0.94%, fluorine content is 0.052%, calcium contents is 0.22%, pH is 2.45 adds in reactor, the temperature of controlling reactor is 40 DEG C, under continuous stirring action, adding mass concentration is that 10% magnesite pulpous state liquid is adjusted to 5.0 by the pH of waste water, after reaction 15min, stop stirring, leave standstill;
(2) reactor bottom is formed to fluorine-containing sludge after leaving standstill and discharge, then start stirring, in supernatant liquor, adding mass concentration is 10% magnesium hydroxide pulpous state liquid, and regulation system pH is 8.2, after reaction 15min, stops stirring, and leaves standstill;
(3) add final clear liquid after precipitation agent to add after Polyferric Sulfate stirs and leave standstill, measure by analysis, after processing, clear liquid is 3.2ppm containing P content, and F content is 3.9ppm, and Ca content is 22.5ppm, can meet the up-to-date emission standard of phosphorous chemical industry and carry out qualified discharge.What obtain prepares struvite containing supplementing N source after P, the dissolving of Mg throw out, and the rate of recovery of phosphorus reaches 87%.
Embodiment 3
(1) the phosphogypsum washes 2L that by phosphorus content be 1.64%, fluorine content is 0.12%, calcium contents is 0.28%, pH is 2.12 adds in reactor, the temperature of controlling reactor is 50 DEG C, under continuous stirring action, adding mass concentration is that 10% magnesiumcarbonate pulpous state liquid is adjusted to 5.5 by the pH of waste water, after reaction 30min, stop stirring, leave standstill;
(2) reactor bottom is formed to fluorine-containing sludge after leaving standstill and discharge, then start stirring, in supernatant liquor, adding mass concentration is 10% sodium hydroxide solution, and regulation system pH is 8.5, after reaction 30min, stops stirring, and leaves standstill;
(3) add rear the leaving standstill of final clear liquid addition polymerization aluminium stirring after precipitation agent, measure by analysis, it is 5.3ppm that the rear clear liquid of processing contains P content, and F content is 5.8ppm, and Ca content is 31.6ppm, can meet the up-to-date emission standard of phosphorous chemical industry and carry out qualified discharge.What obtain prepares struvite containing supplementing N source after P, the dissolving of Mg throw out, and the rate of recovery of phosphorus reaches 84%.
Embodiment 4
(1) the phosphorus-containing wastewater 3L that by phosphorus content be 2.2%, fluorine content is 0.35%, calcium contents is 0.45%, pH is 1.41 adds in reactor, the temperature of controlling reactor is 60 DEG C, under continuous stirring action, adding mass concentration is that 10% rhombspar pulpous state liquid is adjusted to 6.5 by the pH of waste water, after reaction 30min, stop stirring, leave standstill;
(2) reactor bottom is formed to fluorine-containing sludge after leaving standstill and discharge, then start stirring, in supernatant liquor, adding mass concentration is 10% magnesium hydroxide pulpous state liquid and sodium hydroxide solution, and regulation system pH is 9.0, after reaction 30min, stops stirring, and leaves standstill;
(3) add final clear liquid after precipitation agent to add after Polyferric Sulfate stirs and leave standstill, measure by analysis, after processing, clear liquid is 7.4ppm containing P content, and F content is 6.5ppm, and Ca content is 47.7ppm, can meet the up-to-date emission standard of phosphorous chemical industry and carry out qualified discharge.What obtain prepares struvite containing supplementing N source after P, the dissolving of Mg throw out, and the rate of recovery of phosphorus reaches 79%.
Claims (8)
1. a treatment process for industry high-concentration phosphorus-containing wastewater, is characterized in that comprising the following steps:
Step 1, will be with P
2o
5meter phosphorus content is that 0.15-2.2%, fluorine content are that the high-concentration acidic wastewater phosphorus-containing wastewater that 0.01-0.35%, calcium contents are 0.1-0.45% adds in reactor, the temperature of controlling reactor is 30-60 DEG C, constantly under stirring action, adding defluorinating agent that the pH of waste water is adjusted to 4.5-6.5, after reaction 10-30min, stop stirring, leave standstill;
Step 2, reactor bottom is formed to fluorine-containing sludge after leaving standstill and discharge, then start stirring, add precipitation agent in supernatant liquor, regulation system pH is between 8.0-9.0, and reaction stops after 10-30min stirring, and leaves standstill;
Step 3, add the throw out generating after precipitation agent to discharge and collect from reactor bottom, the clear liquid finally forming adds flocculation agent, discharge after leaving standstill;
Step 4, the throw out fertilizer grade dilute phosphoric acid of collecting in step 3 dissolve, and obtain the mixing solutions containing P and Mg, are metered into N source and prepare struvite.
2. the treatment process of a kind of industry high-concentration phosphorus-containing wastewater as claimed in claim 1, is characterized in that: described defluorinating agent is magnesium oxide, magnesiumcarbonate, magnesite or rhombspar.
3. the treatment process of a kind of industry high-concentration phosphorus-containing wastewater as claimed in claim 2, is characterized in that: when described magnesium oxide, magnesiumcarbonate, magnesite or rhombspar use as defluorinating agent, need to be ground to 200-300 object powder.
4. the treatment process of a kind of industry high-concentration phosphorus-containing wastewater as claimed in claim 3, is characterized in that: in use, 200-300 object powder need to be added water and be made into mass concentration is 10% pulpous state liquid to defluorinating agent.
5. the treatment process of a kind of industry high-concentration phosphorus-containing wastewater as claimed in claim 1, is characterized in that: described precipitation agent is magnesium hydroxide or sodium hydroxide.
6. the treatment process of a kind of industry high-concentration phosphorus-containing wastewater as claimed in claim 5, is characterized in that: need to be before use milled to 200-300 order as the magnesium hydroxide of precipitation agent, and to be made into mass concentration be that 10% pulpous state liquid uses.
7. the treatment process of a kind of industry high-concentration phosphorus-containing wastewater as claimed in claim 1, is characterized in that: in processing, collected throw out is in the time dissolving with fertilizer grade dilute phosphoric acid, and the add-on of acid is taking just can be by complete resolution of precipitate for the best.
8. the treatment process of a kind of industry high-concentration phosphorus-containing wastewater as claimed in claim 1, is characterized in that: the flocculation agent using in step 3 is poly-aluminium or Polyferric Sulfate.
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Cited By (17)
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| 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 |
| CN104841365A (en) * | 2015-04-29 | 2015-08-19 | 长沙清能环保科技有限公司 | Composite fluorine removal agent and preparation method |
| CN104944561A (en) * | 2015-06-16 | 2015-09-30 | 景德镇陶瓷学院 | Wastewater nitrogen and phosphorus removing method based on magnesite |
| CN106000277A (en) * | 2016-05-23 | 2016-10-12 | 安徽建筑大学 | Preparation method and use method of in-situ transformed phosphorus recovery material |
| CN106698730A (en) * | 2015-07-28 | 2017-05-24 | 江苏吉华化工有限公司 | Phosphorus chemical wastewater treatment method |
| CN108751152A (en) * | 2018-05-30 | 2018-11-06 | 湖北三宁化工股份有限公司 | The method for improving the pH value of the industrial monoammonium phosphate of Wet-process Phosphoric Acid Production |
| CN109607869A (en) * | 2018-12-31 | 2019-04-12 | 中北大学 | A kind of nitrophosphate fertilizer wastewater treatment method |
| CN109912076A (en) * | 2019-03-28 | 2019-06-21 | 江西中江环保股份有限公司 | A kind of processing method of Combined waste water efficient dephosphorization |
| CN110317115A (en) * | 2019-08-02 | 2019-10-11 | 中化重庆涪陵化工有限公司 | A method of composite slow-release fertilizer is produced using phosphorous chemical industry production waste water |
| CN110563198A (en) * | 2019-09-04 | 2019-12-13 | 广西长润环境工程有限公司 | Chemical fertilizer wastewater treatment method and treatment equipment |
| CN110759514A (en) * | 2019-08-16 | 2020-02-07 | 上海世渊环保科技有限公司 | High-concentration phosphorus-containing wastewater treatment method and treatment system for phenolic resin enterprises |
| CN110950314A (en) * | 2019-11-25 | 2020-04-03 | 中南民族大学 | Artificial struvite, preparation method thereof and citrate soluble fertilizer |
| CN111995104A (en) * | 2020-07-21 | 2020-11-27 | 森田新能源材料（张家港）有限公司 | Dephosphorization and defluorination process for industrial wastewater |
| CN112520891A (en) * | 2020-11-25 | 2021-03-19 | 华中师范大学 | Advanced treatment method of comprehensive wastewater of phosphorus chemical industry |
| CN112811740A (en) * | 2021-01-28 | 2021-05-18 | 关向辉 | Method for removing fluorine and hardness from industrial wastewater |
| CN113461202A (en) * | 2021-06-24 | 2021-10-01 | 宜都兴发化工有限公司 | Resource treatment method for high phosphorus, high calcium and high magnesium |
| CN113788558A (en) * | 2021-09-08 | 2021-12-14 | 武汉工程大学 | Method for removing fluorine in phosphogypsum leachate by using reverse osmosis membrane |
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| CN104445730B (en) * | 2014-11-21 | 2017-02-08 | 贵州开磷集团股份有限公司 | Comprehensive utilization method of wastewater containing phosphorus and fluorine |
| 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 |
| CN104841365A (en) * | 2015-04-29 | 2015-08-19 | 长沙清能环保科技有限公司 | Composite fluorine removal agent and preparation method |
| CN104944561A (en) * | 2015-06-16 | 2015-09-30 | 景德镇陶瓷学院 | Wastewater nitrogen and phosphorus removing method based on magnesite |
| CN104944561B (en) * | 2015-06-16 | 2017-11-24 | 景德镇陶瓷大学 | A kind of denitrogenation of waste water phosphorus removing method based on magnesite |
| CN106698730A (en) * | 2015-07-28 | 2017-05-24 | 江苏吉华化工有限公司 | Phosphorus chemical wastewater treatment method |
| CN106000277A (en) * | 2016-05-23 | 2016-10-12 | 安徽建筑大学 | Preparation method and use method of in-situ transformed phosphorus recovery material |
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| CN109912076A (en) * | 2019-03-28 | 2019-06-21 | 江西中江环保股份有限公司 | A kind of processing method of Combined waste water efficient dephosphorization |
| CN110317115A (en) * | 2019-08-02 | 2019-10-11 | 中化重庆涪陵化工有限公司 | A method of composite slow-release fertilizer is produced using phosphorous chemical industry production waste water |
| CN110759514A (en) * | 2019-08-16 | 2020-02-07 | 上海世渊环保科技有限公司 | High-concentration phosphorus-containing wastewater treatment method and treatment system for phenolic resin enterprises |
| CN110563198A (en) * | 2019-09-04 | 2019-12-13 | 广西长润环境工程有限公司 | Chemical fertilizer wastewater treatment method and treatment equipment |
| CN110950314A (en) * | 2019-11-25 | 2020-04-03 | 中南民族大学 | Artificial struvite, preparation method thereof and citrate soluble fertilizer |
| CN110950314B (en) * | 2019-11-25 | 2021-04-23 | 中南民族大学 | Artificial struvite, preparation method thereof and citrate soluble fertilizer |
| CN111995104A (en) * | 2020-07-21 | 2020-11-27 | 森田新能源材料（张家港）有限公司 | Dephosphorization and defluorination process for industrial wastewater |
| CN112520891A (en) * | 2020-11-25 | 2021-03-19 | 华中师范大学 | Advanced treatment method of comprehensive wastewater of phosphorus chemical industry |
| CN112811740A (en) * | 2021-01-28 | 2021-05-18 | 关向辉 | Method for removing fluorine and hardness from industrial wastewater |
| CN113461202A (en) * | 2021-06-24 | 2021-10-01 | 宜都兴发化工有限公司 | Resource treatment method for high phosphorus, high calcium and high magnesium |
| CN113461202B (en) * | 2021-06-24 | 2023-10-27 | 宜都兴发化工有限公司 | High-phosphorus and high-calcium magnesium recycling treatment method |
| CN113788558A (en) * | 2021-09-08 | 2021-12-14 | 武汉工程大学 | Method for removing fluorine in phosphogypsum leachate by using reverse osmosis membrane |
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Application publication date: 20141008 |