CN105600992A - Technology for preparing feed calcium from wastewater residues - Google Patents
Technology for preparing feed calcium from wastewater residues Download PDFInfo
- Publication number
- CN105600992A CN105600992A CN201610084460.6A CN201610084460A CN105600992A CN 105600992 A CN105600992 A CN 105600992A CN 201610084460 A CN201610084460 A CN 201610084460A CN 105600992 A CN105600992 A CN 105600992A
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- reaction
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- slag
- wastewater
- calcium
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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
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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
- 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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a technology for preparing feed calcium from wastewater residues. A traditional wastewater treatment technology and feed calcium production are combined so as to optimize the current production technology. Compared with traditional one-level, two-level and three-level methods for neutralizing wastewater by adding lime milk, according to the technology, a new four-level neutralizing method is adopted, the control point of the pH value in wastewater is regulated with wastewater residues and lime milk in the first-level defluorination stage and the second-level defluorination stage respectively, fluoride in wastewater is removed to the maximum, the interference of fluoride in wastewater on the removing rate of phosphate radicals in the later stage is relieved, a feed calcium product is prepared in the third-level neutralization stage, a large amount of phosphate and fluorine in wastewater are removed in the fourth-level neutralization stage so that outer drainage water can meet the drainage standard, and meanwhile the reaction time of all the stages is regulated. By means of the technology, wastewater residues obtained in traditional wastewater neutralization treatment are fully recycled, the recycling rate of the phosphate resource in wastewater residues is increased, feed-grade calcium hydrophosphate is the product, and economic benefits are achieved while the environment-protection pressure of stacking of wastewater residues is relieved.
Description
Technical field
The present invention relates to phosphate fertilizer industry phosphorus fluorine wastewater processing technology, specifically a kind of sewage system is raised the technique of calcium.
Background technology
In the processing procedure of high concentration phosphorus, fluoric acid wastewater, according to Phosphorus From Wastewater fluorine concentration difference, can adopt respectively at presentOne-level neutralization and flocculent precipitation, secondary neutralization and the two-stage precipitation method, three grades of neutralizations and three grades of flocculent precipitations etc. Above-mentioned three kindsTechnique in process of production by produce a large amount of sewage slags, owing to containing a large amount of calcirm-fluoride, calcium silicates, alkali calcium phosphate etc.,Make in slag phosphorus content on the low side, do not reach reuse effect, can only adopt slag dam landfill or become phosphorus stone with phosphogypsum slag hybrid processCream building block is used in building trade. But these methods all efficiently do not use sewage slag, and contained in the slag that run offSome phosphor resources.
Current defluorination reaction of raising calcium production does not carry out classification defluorinate, will certainly shadow at the defluorination residues that the reaction later stage accumulatesThe selective precipitation of phonolite ash to fluoride, has weakened the removal ability of fluorine, affects the quality of overflowing liquid. In addition, after neutralization reactionClear liquid there is no at present good whereabouts, phosphor resource wherein is not recycled, simultaneously at environmental protection standard increasingly stringentSituation under, the whereabouts of this water and use be must consider.
Summary of the invention
The object of the invention is to, the sewage slag that allows traditional waste water treatment process produce is turned waste into wealth, and alleviates slag field and stores upPressure, is applied to sewage slag to raise calcium production, optimizes the part operation stage of original device, and the high efficiente callback of reaching phosphor resource is outerThe qualified discharge of draining, the new technology of reduction cost of water treatment.
Sewage slag system of the present invention is raised the technique of calcium, comprises the following steps:
(1) the slag field Chi Shui of sewage-treatment plant and sewage slag being carried out to first order defluorination reaction, pH controls index and is 2.25～2.60, the reaction time is controlled at 10 minutes, and temperature is not less than 40 DEG C, and reaction finishes rear clarification naturally 10 minutes, removes bottom slagSlurry is got clear liquid, adds milk of lime to carry out secondary defluorination reaction, and the reaction time is not low 30 minutes, and pH controls index and is 2.70～3.30, temperature is not less than 40 DEG C;
(2) slip of defluorination reaction adds Flokal B to carry out after 10 minutes clarifying treatment, and clear liquid carries out third level limeBreast neutralization reaction, it is 5.70～6.20 that pH controls index, after this elementary reaction, in water, fluorine ion, lower than 30ppm, is follow-up waterThe efficient removal of middle phosphorus fluorine lays the first stone, and the reaction time is controlled at more than 50 minutes, and water temperature is not less than 30 DEG C, and reaction finishes laggardRow Separation of Solid and Liquid;
(3) clear liquid of third level reaction carries out the reaction of fourth stage lime slurry neutralization, and it is 9.70～10.50 that pH controls index, reactionTime is controlled at more than 40 minutes, and water temperature is not less than 30 DEG C, adds flocculant to carry out sedimentation after having reacted, and the time is 30 pointsClock, can drain and account for more than 1/2 moisture of cumulative volume, and the level Four slag slurry of bottom returns to neutralization reaction and recycles.
In described step (1), through two-stage defluorinate, fluoride (F meter) lower than 100ppm, phosphate (P meter) content is1.0%～1.30%。
In described step (1), after defluorination reaction, the whereabouts of defluorination residues is the gypsum stock tank again that enters phosphoric acid after starching again,Deliver to slag field, the phosphorus in its liquid phase enters in the reaction system of technique by Chi Shui.
In described step (2), solid phase slag drying and processing post analysis after Separation of Solid and Liquid, fluoride (F meter) lower than 0.18%, phosphorusHydrochlorate (P meter) content can reach more than 16.5%, completely meets and raises calcium product quality standard, and liquid is made level Four neutralisation treatment.
In described step (3), after reaction in water fluoride (F meter) lower than 5ppm, phosphate (P meter) lower than 1ppm.
In described step (3), when the reuse of level Four slag, take two-stage to add slag method, first utilize in level Four slag slurry and defluorinate water, pHControl index for being less than 4.5, react 30 minutes, add afterwards milk of lime to continue reaction, it is 5.70～6.20 that pH controls index, anti-Between seasonable, it is 20 minutes.
The collocation method of described milk of lime, wherein: quick lime CaO content is more than 15%, milk of lime exceedes 30 setup timeMinute.
In described technique, the temperature of reaction slurry when requiring, fills into appropriate steam in slip.
The present invention compared with the prior art, not changing on the basis of sewage treatment process, has carried out sewage slag comprehensivelyRecycling, and optimized the defluorinate workshop section of raising calcium, in having carried out and water reuse, reduced the consumption cost of lime simultaneously.
Write in " phosphate fertilizer and compound fertilizer " in September, 2015 " recoverying and utilizing method of phosphor resource in phosphate fertilizer acid waste water "In (the 5th page of Vol.30No.9) literary composition, described similar technique, but the angle that this technique only reclaims from waste water slag resource is carried outSet forth, do not mention and the content of raising calcium explained hereafter and combining, compared with this article, the final products of flow process of the present invention are for raisingMaterial calcium hydrophosphate, and by the former defluorination reaction of calcium technique, the transformation that neutralization reaction has been carried out fractional order reaction, the number of reactive tank of raisingAmount setting has been made and having been clarified a plan, and reaction time and temperature and pH control index and be also optimized, and effluent index is better thanAforementioned technique.
The present invention has overcome traditional handicraft shortcoming, catches the double dominant of economy and the feature of environmental protection, makes sewage disposal and raisesCalcium technique organically combines, and is adapted to industrialized large production.
Brief description of the drawings
Fig. 1 is process chart of the present invention.
Detailed description of the invention
Sewage slag system is raised calcium new technology, comprises the following steps:
(1) the slag field Chi Shui of sewage-treatment plant and sewage slag being carried out to first order defluorination reaction, pH controls index and is 2.20～2.50, the reaction time is controlled at 10 minutes, and temperature is not less than 40 DEG C, after finishing, reaction in first grade subsides groove, clarifies 10 minutes,Remove bottom slag slurry, clear liquid overflow, to secondary defluorinate groove (secondary defluorinate groove is set to 3), adds milk of lime to carry out secondary defluorinateReaction, it is 2.70～3.30 that pH controls index, and the reaction time is not less than 30 minutes, and temperature is not less than 40 DEG C, described milk of limeCollocation method, wherein: quick lime CaO content is 10%～15%, milk of lime more than 30 minutes setup time. The main removal of this step given upA large amount of fluorides in water, avoid the impact of a large amount of fluorides on phosphate radical clearance in subsequent reactions water, are divided into two-stage defluorinate, areOn the basis of originally raising calcium device defluorinate workshop section, be optimized, the removal of one-level defluorination residues is conducive to effectively entering of secondary defluorinateOK, through two-stage defluorinate, fluoride (F meter) is 1% left and right lower than 100ppm, phosphate (P meter) content. The whereabouts of defluorination residues isAfter starching, enter the gypsum stock tank again of phosphoric acid again, deliver to slag field, the phosphorus in its liquid phase still can enter the anti-of technique by Chi ShuiAnswer in system.
(2) slip of defluorination reaction adds appropriate Flokal B to enter secondary subsider to carry out 10 minutes clarifying treatmentAfter, clear liquid carries out third level lime slurry neutralization reaction (neutralization reaction groove is set to 5), and it is 5.70～6.20 that pH controls index,After this elementary reaction, in water, fluorine ion is lower than 30ppm, and for the efficient removal of phosphorus fluorine in follow-up water lays the first stone, the reaction time is controlledBuilt in more than 50 minutes, water temperature is not less than 30 DEG C, and reaction finishes rear slip and enters Neutralization settlement groove and carry out Separation of Solid and Liquid, solid phase slagDrying and processing post analysis, fluoride (F meter) lower than 0.18%, phosphate (P meter) content can reach more than 16.5%, completely meet and raise calciumTarget level of product quality, liquid is made level Four neutralisation treatment.
(3) clear liquid of third level neutralization reaction carries out the reaction of fourth stage lime slurry neutralization (level Four neutralization reaction groove is made as 5Individual), pH control index be 9.70～10.50, after this elementary reaction in water fluoride (F meter) lower than 5ppm, phosphate (P meter)Lower than 1ppm, the reaction time is controlled at more than 40 minutes, and water temperature is not less than 30 DEG C, adds appropriate flocculant four after having reactedIn level subsider, carry out sedimentation, the time is 30 minutes, can drain and account for more than 1/2 moisture of cumulative volume, and the level Four slag of bottom is starchedReturn to three grades of neutralization reactions and recycle, while having the reuse of level Four slag, take two-stage to add slag method, first utilize the neutralization of level Four slag slurryDefluorinate water, pH controls index for being less than 4.5, reacts 30 minutes, adds afterwards milk of lime to continue reaction, and it is 5.70 that pH controls index～6.20, the reaction time is 20 minutes. The recovery of level Four slag is reclaimed the phosphorus in slag again, and has reduced lime consumptionCost.
Claims (8)
1. sewage slag system is raised a technique for calcium, it is characterized in that, comprises the following steps:
(1) pond, phosphogypsum slag field water leading indicator is pH≤1.7, P2O5>=2.5%, F≤1.1%, by the slag field of sewage-treatment plantChi Shui and sewage slag carry out first order defluorination reaction, pH control index be 2.25～2.60, the reaction time be controlled at 10 minutes withIn, temperature is not less than 40 DEG C, and reaction finishes rear clarification naturally 10 minutes, removes bottom slag slurry and gets clear liquid, adds milk of lime to carry outSecondary defluorination reaction, it is 2.70～3.30 that pH controls index, the reaction time, temperature was not less than 40 DEG C in order to be not less than 30 minutes;
(2) slip of defluorination reaction carries out after 20 minutes clarifying treatment, and clear liquid carries out the reaction of third level lime slurry neutralization, and pH controlsIndex is 5.70～6.20, after this elementary reaction in water fluorine ion lower than 30ppm, for the efficient removal of phosphorus fluorine in follow-up water is beatenLower basis, the reaction time is controlled at more than 50 minutes, and water temperature is not less than 30 DEG C, after reaction finishes, carries out Separation of Solid and Liquid;
(3) clear liquid of third level reaction carries out the reaction of fourth stage lime slurry neutralization, and it is 9.70～10.50 that pH controls index, reactionTime is controlled at more than 40 minutes, and water temperature is not less than 30 DEG C, adds flocculant to carry out sedimentation after having reacted, and the time is 30 pointsClock, can drain and account for more than 1/2 moisture of cumulative volume, and the level Four slag slurry of bottom returns to neutralization reaction and recycles.
2. sewage slag system as claimed in claim 1 is raised the technique of calcium, it is characterized in that, in described step (1), de-through two-stageFluorine, fluoride is in F, and lower than 100ppm, phosphate, in P, content is 1%～1.3%.
3. sewage slag system as claimed in claim 1 is raised the technique of calcium, it is characterized in that, in described step (1), de-after defluorination reactionThe whereabouts of fluorine slag is the gypsum stock tank again that enters phosphoric acid after starching again, delivers to slag field, and the phosphorus in its liquid phase enters by Chi ShuiIn the reaction system of technique.
4. sewage slag system as claimed in claim 1 is raised the technique of calcium, it is characterized in that, in described step (2), after Separation of Solid and LiquidSolid phase slag drying and processing post analysis, fluoride is in F, and lower than 0.18%, phosphate is in P, content can reach more than 16.5%, completelyMeet and raise calcium product quality standard, liquid is made level Four neutralisation treatment.
5. sewage slag system as claimed in claim 1 is raised the technique of calcium, it is characterized in that, in described step (3), and fluorine in water after reactionCompound is in F, lower than 5ppm, phosphate in P, lower than 1ppm.
6. sewage slag system as claimed in claim 1 is raised the technique of calcium, it is characterized in that, in described step (3), and the reuse of level Four slagTime, take two-stage to add slag method, first utilize in level Four slag slurry and defluorinate water, pH controls index for being less than 4.5, reacts 30 minutes, itAfter add milk of lime continue reaction, pH control index be 5.70～6.20, the reaction time is 20 minutes.
7. sewage slag system as claimed in claim 1 is raised the technique of calcium, it is characterized in that, and the collocation method of described milk of lime, wherein:Quick lime CaO content is 10%～15%, milk of lime more than 30 minutes setup time.
8. the sewage slag system as described in claim 1-7 any one is raised the technique of calcium, it is characterized in that, the temperature of reaction slurry lower thanWhen requirement, in slip, fill into appropriate steam.
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| CN201610084460.6A CN105600992A (en) | 2016-02-14 | 2016-02-14 | Technology for preparing feed calcium from wastewater residues |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105884077A (en) * | 2016-04-13 | 2016-08-24 | 四川绵竹市盘龙矿物质有限责任公司 | Method for realizing total-closed wastewater circulation in feed-grade calcium hydrophosphate production process |
| CN106744771A (en) * | 2017-02-21 | 2017-05-31 | 瓮福（集团）有限责任公司 | A kind of phosphorus-containing wastewater produces the defluorination method of calcium hydrophosphate fodder |
| CN109205854A (en) * | 2018-10-29 | 2019-01-15 | 贵州川恒化工股份有限公司 | The new method of the synchronous deep phosphorous removal fluorine of the inorganic sewage of phosphorous chemical industry |
| CN110078039A (en) * | 2019-06-04 | 2019-08-02 | 瓮福（集团）有限责任公司 | A kind of low-concentration phosphorus-containing wastewater step produces the method and device of calcium hydrophosphate fodder |
| CN110526450A (en) * | 2019-09-24 | 2019-12-03 | 瓮福（集团）有限责任公司 | A kind of acid phosphorus fluorine waste water treatment process of the low slag rate of efficient dephosphorization fluorine |
| CN115974595A (en) * | 2022-12-29 | 2023-04-18 | 瓮福（集团）有限责任公司 | Process for preparing phosphorus-magnesium-calcium composite long-acting fertilizer by treating phosphorus-fluorine-containing wastewater |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105884077A (en) * | 2016-04-13 | 2016-08-24 | 四川绵竹市盘龙矿物质有限责任公司 | Method for realizing total-closed wastewater circulation in feed-grade calcium hydrophosphate production process |
| CN106744771A (en) * | 2017-02-21 | 2017-05-31 | 瓮福（集团）有限责任公司 | A kind of phosphorus-containing wastewater produces the defluorination method of calcium hydrophosphate fodder |
| CN109205854A (en) * | 2018-10-29 | 2019-01-15 | 贵州川恒化工股份有限公司 | The new method of the synchronous deep phosphorous removal fluorine of the inorganic sewage of phosphorous chemical industry |
| CN110078039A (en) * | 2019-06-04 | 2019-08-02 | 瓮福（集团）有限责任公司 | A kind of low-concentration phosphorus-containing wastewater step produces the method and device of calcium hydrophosphate fodder |
| CN110078039B (en) * | 2019-06-04 | 2023-09-22 | 瓮福（集团）有限责任公司 | Method and device for preparing feed-grade calcium hydrophosphate in low-concentration phosphorus-containing wastewater step manner |
| CN110526450A (en) * | 2019-09-24 | 2019-12-03 | 瓮福（集团）有限责任公司 | A kind of acid phosphorus fluorine waste water treatment process of the low slag rate of efficient dephosphorization fluorine |
| CN115974595A (en) * | 2022-12-29 | 2023-04-18 | 瓮福（集团）有限责任公司 | Process for preparing phosphorus-magnesium-calcium composite long-acting fertilizer by treating phosphorus-fluorine-containing wastewater |
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