CN103613181A - Method for treating phosphogypsum slag dump pool water by using low-grade lime - Google Patents
Method for treating phosphogypsum slag dump pool water by using low-grade lime Download PDFInfo
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- CN103613181A CN103613181A CN201310628403.6A CN201310628403A CN103613181A CN 103613181 A CN103613181 A CN 103613181A CN 201310628403 A CN201310628403 A CN 201310628403A CN 103613181 A CN103613181 A CN 103613181A
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Abstract
The invention relates to a method for treating phosphogypsum slag dump pool water by using low-grade lime. The method comprises the following steps: slaking lime; grading the lime; purifying the phosphogypsum slag dump pool water by using coarse sand; treating the purified liquid by using fine lime milk to prepare phosphorus-containing slag, wherein treatment on the phosphogypsum slag dump pool water by the lime is divided into primary, secondary and tertiary precipitation reactions to respectively precipitate fluorine and phosphorus in the pool water and deeply purify the pool water. By utilizing the method, the low-grade lime can be slaked completely, so calcium carbonate of the lime is completely used for treating the pool water, the using amount of the lime is reduced by about 30 percent and the cost is reduced; the lime is utilized in a grading mode, and the fine lime milk containing few impurities and the pool water subjected to defluorination purification treatment generate precipitation reaction to obtain the available phosphorus-containing slag with high grade and few impurities, so the phosphorus resources are recovered and a good economic benefit is achieved; the discharge slag after pool water treatment is reduced by about 70 percent, the occupied land for stockpiling treatment and the maintenance cost of a stock dump are reduced, damage to the environment is reduced, and the environment-friendly benefit is significant.
Description
Technical field
The present invention relates to phosphorous chemical industry field of waste water treatment, relate in particular to the method for the low-grade lime treatment phosphogypsum slag field Chi Shui of a kind of use.
Background technology
China's Wet Phosphoric Acid Plant mainly adopts wet phosphoric acid by dihydrate explained hereafter phosphoric acid, produces every year a large amount of by product phosphogypsums, and these phosphogypsums generally adopt wet-process deslagging mode (wet basis, moisture approximately 23%), by the defeated pulp pump of phosphoric acid plant, deliver to phosphogypsum slag field.Phosphogypsum is stored up in process in slag field, in phosphogypsum wet basis, water and rainwater form phosphogypsum slag field Chi Shui in slag field, in water, contain the plurality of impurities such as phosphorus fluorine calcium sulphur magnesium-aluminum-iron, this pond water part is delivered to production equipment cocycle and is used, and a part is carried out recycle and reuse or qualified discharge after sewage disposal.
The milk of lime that during the general employing of water treatment of China's phosphogypsum slag field Chi Shui adds, low-quality lime slaking forms is processed through I and II chemical precipitation, supernatant liquor recycle and reuse or qualified discharge, the precipitating sludge thickening filtration of I and II settling tank obtains sewage slag.Owing to adopting, the lime grade for the treatment of pond water is not high contains a large amount of impurity, and the process characteristic for the treatment of pond water, although cause the sewage slag obtaining to contain a large amount of phosphor resources, but foreign matter content is many, in sewage slag, the content of Vanadium Pentoxide in FLAKES, generally at 18%-24%, does not reach the requirement of 28%-31% on current Wet Phosphoric Acid Plant, and Mg content mostly exceeds standard, so sewage slag is generally deposited processing as slag dump, taken land resources, and caused certain environmental pollution.
The present invention processes phosphogypsum slag field Chi Shui by low-grade lime classification utilization, obtains the high and available phosphorus throw out of phosphorus content, reduces lime usage quantity, reclaims phosphor resource, meets the requirement of green economy and recycling economy.Through retrieval, there is no up to now the patent application that phosphogypsum slag field Chi Shui is processed in low-grade lime classification utilization, there is no relevant bibliographical information yet.
Summary of the invention
The method that the object of the invention is to overcome above-mentioned shortcoming and the low-grade lime treatment phosphogypsum slag field Chi Shui of a kind of use is provided, the method has the lime of reduction usage quantity, reclaims phosphor resource, economic benefit and environmental benefit outstanding feature.
For achieving the above object, the technical solution used in the present invention is: the method for the low-grade lime treatment phosphogypsum slag field Chi Shui of a kind of use, comprises the following steps:
(1), lime slaking: be that 45%-65%, calcium carbonate quality percentage composition are that 10%-25%, calcium sulfate quality percentage composition are that 0-15%, silicon-dioxide quality percentage composition are 5%-15%, all the other add the water digestion 0.5h-3h of 40 ℃-70 ℃ for the low-grade lime of other impurity by effective CaO quality percentage composition, the 2-6 that water add-on is lime quality doubly;
(2), lime classification: the thick milk of lime of gained after digestion is passed through to the separated classification of spinning liquid, the heavy material of gained is calcium carbonate, calcium sulfate, silicon-dioxide and the high coarse sand of other foreign matter content, the material that gained proportion is little is the refined lime breast that calcium carbonate, calcium sulfate, silicon-dioxide and other foreign matter content are low, and the butt mass ratio of gained coarse sand and refined lime breast is 1:1-2;
(3), coarse sand purifying treatment phosphogypsum slag field Chi Shui: the coarse sand of gained is joined in the water of pond, phosphogypsum slag field and carries out primary sedimentation reaction, stirring reaction 0.5h～2h at 25 ℃～50 ℃, controlling reaction end pH value is 2.0～2.5, has reacted rear filtration, is purified liquid and fluorine-containing slag;
(4), refined lime breast treatment and purification liquid is prepared phosphorus bearing slag: the refined lime breast of gained is joined and in scavenging solution, carries out secondary sedimentation reaction, stirring reaction 0.5h～2h at 25 ℃～50 ℃, controlling reaction end pH value is 5.5～6.5, has reacted rear filtration, and filter cake is in butt P
2o
5quality percentage composition is the phosphorus bearing slag of 30%-34%, filtrate continuation add refined lime breast to carry out three precipitin reaction to be neutralized to pH value be 8～10 rear filtrations, a filtered liquid part is returned to phosphoric acid systemic circulation and is used, a part is returned to milk of lime preparation system and is used.
Above-mentioned phosphogypsum slag field Chi Shui is 1%-6% containing Vanadium Pentoxide in FLAKES quality percentage composition, and fluorine-containing quality percentage composition is 0.3%-1.5%.
The present invention becomes one, two, three precipitin reaction by pond, lime treatment phosphogypsum slag field moisture, respectively for the fluorine in settling tank water, phosphorus and deep purifying Chi Shui, mainly for reclaim this phosphor resource of phosphorus phosphorus bearing slag of high grade and that impurity is few when secondary sedimentation is reacted.Spinning liquid after low-grade lime slaking is classified into two portions, and a part is calcium carbonate, calcium sulfate, silicon-dioxide and the high coarse sand of other foreign matter content, and another part is the refined lime breast that calcium carbonate, calcium sulfate, silicon-dioxide and other foreign matter content are low.Coarse sand is for primary sedimentation reaction, and while reacting due to primary sedimentation, the acidity of phosphogypsum slag field Chi Shui is relatively strong, can react comparatively completely with the calcium carbonate in coarse sand, and the calcium carbonate taking full advantage of in former lime carrys out treating pond water; Secondly, the calcium sulfate in former lime and other are also discharged by fluorine-containing slag as the impurity that gangue and so on react with Chi Shui hardly after primary sedimentation reacts.Refined lime breast is due to impure less, carrying out secondary sedimentation with the Chi Shui of process defluorinate purifying treatment reacts, by controlling pH value, obtain the phosphorus bearing slag that phosphorus grade is higher and impurity is few, this phosphorus bearing slag has higher economic worth, can with phosphorus concentrate equally for phosphoric acid by wet process produce or for the preparation of containing phosphatic manure.
With respect to pond, existing lime treatment phosphogypsum slag field water technology, tool of the present invention has the following advantages:
(1) by the present invention, can make low-grade lime slaking abundant, and utilize more fully the calcium carbonate in lime to carry out treating pond water, make lime usage quantity reduce approximately 30%, reduced the cost that uses lime.
(2) the present invention utilizes lime classification, impure less refined lime breast and the Chi Shui that passes through defluorinate purifying treatment carry out precipitin reaction obtain phosphorus grade compared with high, impurity is few, available phosphorus bearing slag, has reclaimed phosphor resource, good in economic efficiency.
(3) the present invention makes the discharge slag of pond water treatment reduce approximately 70%, has reduced and has stored up the land seizure amount of processing and the maintenance cost in stockyard, has reduced the harm to environment, and environmental benefit is obvious.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
For the ease of understanding the present invention, below examples of implementation set forth content of the present invention, content of the present invention is not limited only to the following examples.
embodiment 1
By effective CaO quality percentage composition be 52%, calcium carbonate quality percentage composition is 15%, calcium sulfate quality percentage composition is 8%, silicon-dioxide quality percentage composition is 10%, all the other stir digestion 1 hour for the low-grade lime 100kg of other impurity adds the water 350kg of 50 ℃.By the thick milk of lime of gained after digestion, by the separated classification of spinning liquid, the butt mass ratio of gained coarse sand and refined lime breast is 1:1.4.
The coarse sand of gained is joined to the phosphogypsum slag field Chi Shui (P of 1t
2o
5be that 4.0%, F is 0.9%) in carry out primary sedimentation reaction, stirring reaction 1h at 40 ℃, controlling reaction end pH value is 2.1, has reacted rear filtration, is purified liquid and fluorine-containing slag.
In scavenging solution, add refined lime breast to carry out secondary sedimentation reaction, stirring reaction 1.5h at 40 ℃, controlling reaction end pH value is 6.5, has reacted rear filtration, filter cake is phosphorus bearing slag, after being dried, obtains 106kg butt phosphorus bearing slag (P
2o
5quality percentage composition is 32.5%), filtrate continuation add refined lime breast to carry out three precipitin reaction to be neutralized to pH value be 8 rear filtrations, a filtered liquid part is returned to phosphoric acid systemic circulation and is used, a part is returned to milk of lime preparation system and is used.
embodiment 2
By effective CaO quality percentage composition be 45%, calcium carbonate quality percentage composition is 25%, calcium sulfate quality percentage composition is 12%, silicon-dioxide quality percentage composition is 13%, all the other stir digestion 3 hours for the low-grade lime 30kg of other impurity adds the water 60kg of 40 ℃.By the thick milk of lime of gained after digestion, by the separated classification of spinning liquid, the butt mass ratio of gained coarse sand and refined lime breast is 1:1.
The coarse sand of gained is joined to the phosphogypsum slag field Chi Shui (P of 1t
2o
5be that 1.0%, F is 0.3%) in carry out primary sedimentation reaction, stirring reaction 2h at 25 ℃, controlling reaction end pH value is 2.5, has reacted rear filtration, is purified liquid and fluorine-containing slag.
In scavenging solution, add refined lime breast to carry out secondary sedimentation reaction, stirring reaction 2h at 25 ℃, controlling reaction end pH value is 5.5, has reacted rear filtration, filter cake is phosphorus bearing slag, after being dried, obtains 28kg butt phosphorus bearing slag (P
2o
5quality percentage composition is 30%), filtrate continuation add refined lime breast to carry out three precipitin reaction to be neutralized to pH value be 9 rear filtrations, a filtered liquid part is returned to phosphoric acid systemic circulation and is used, a part is returned to milk of lime preparation system and is used.
embodiment 3
By effective CaO quality percentage composition be 65%, calcium carbonate quality percentage composition is 10%, calcium sulphate content is 0, silicon-dioxide quality percentage composition is 15%, all the other stir digestion 0.5 hour for the low-grade lime 122kg of other impurity adds the water 732kg of 70 ℃.By the thick milk of lime of gained after digestion, by the separated classification of spinning liquid, the butt mass ratio of gained coarse sand and refined lime breast is 1:2.
The coarse sand of gained is joined to the phosphogypsum slag field Chi Shui (P of 1t
2o
5be that 6.0%, F is 1.1%) in carry out primary sedimentation reaction, stirring reaction 0.5h at 50 ℃, controlling reaction end pH value is 2.0, has reacted rear filtration, is purified liquid and fluorine-containing slag.
In scavenging solution, add refined lime breast to carry out secondary sedimentation reaction, stirring reaction 0.5h at 50 ℃, controlling reaction end pH value is 5.7, has reacted rear filtration, filter cake is phosphorus bearing slag, after being dried, obtains 159kg butt phosphorus bearing slag (P
2o
5quality percentage composition is 31.7%), filtrate continuation add refined lime breast to carry out three precipitin reaction to be neutralized to pH value be 10 rear filtrations, a filtered liquid part is returned to phosphoric acid systemic circulation and is used, a part is returned to milk of lime preparation system and is used.
embodiment 4
By effective CaO quality percentage composition be 55%, calcium carbonate quality percentage composition is 20%, calcium sulfate quality percentage composition is 15%, silicon-dioxide quality percentage composition is 5%, all the other stir digestion 1 hour for the low-grade lime 125kg of other impurity adds the water 375kg of 55 ℃.By the thick milk of lime of gained after digestion, by the separated classification of spinning liquid, the butt mass ratio of gained coarse sand and refined lime breast is 1:1.2.
The coarse sand of gained is joined to the phosphogypsum slag field Chi Shui (P of 1t
2o
5be that 5.2%, F is 1.5%) in carry out primary sedimentation reaction, stirring reaction 1.5h at 37 ℃, controlling reaction end pH value is 2.3, has reacted rear filtration, is purified liquid and fluorine-containing slag.
In scavenging solution, add refined lime breast to carry out secondary sedimentation reaction, stirring reaction 1.5h at 35 ℃, controlling reaction end pH value is 5.8, has reacted rear filtration, filter cake is phosphorus bearing slag, after being dried, obtains 125kg butt phosphorus bearing slag (P
2o
5quality percentage composition is 34%), filtrate continuation add refined lime breast to carry out three precipitin reaction to be neutralized to pH value be 10 rear filtrations, a filtered liquid part is returned to phosphoric acid systemic circulation and is used, a part is returned to milk of lime preparation system and is used.
embodiment 5
By effective CaO quality percentage composition be 49%, calcium carbonate quality percentage composition is 22%, calcium sulfate quality percentage composition is 11%, silicon-dioxide quality percentage composition is 12%, all the other stir digestion 50 minutes for the low-grade lime 88kg of other impurity adds the water 200kg of 45 ℃.By the thick milk of lime of gained after digestion, by the separated classification of spinning liquid, the butt mass ratio of gained coarse sand and refined lime breast is 1:1.3.
The coarse sand of gained is joined to the phosphogypsum slag field Chi Shui (P of 1t
2o
5be that 4.1%, F is 0.8 %) in carry out primary sedimentation reaction, at 45 ℃, stirring reaction is 1 hour 15 minutes, controlling reaction end pH value is 2.1, has reacted rear filtration, is purified liquid and fluorine-containing slag.
In scavenging solution, add refined lime breast to carry out secondary sedimentation reaction, at 45 ℃, stirring reaction is 1 hour 45 minutes, and controlling reaction end pH value is 6.2, has reacted rear filtration, and filter cake is phosphorus bearing slag, after being dried, obtains 107kg butt phosphorus bearing slag (P
2o
5quality percentage composition is 33%), filtrate continuation add refined lime breast to carry out three precipitin reaction to be neutralized to pH value be 10 rear filtrations, a filtered liquid part is returned to phosphoric acid systemic circulation and is used, a part is returned to milk of lime preparation system and is used.
The above, it is only preferred embodiment of the present invention, not the present invention is done to any pro forma restriction, any technical solution of the present invention content that do not depart from, any simple modification, equivalent variations and the modification above embodiment done according to technical spirit of the present invention, all still belong in the scope of technical solution of the present invention.
Claims (2)
1. by a method of low-grade lime treatment phosphogypsum slag field Chi Shui, it is characterized in that comprising the following steps:
(1), lime slaking: be that 45%-65%, calcium carbonate quality percentage composition are that 10%-25%, calcium sulfate quality percentage composition are that 0-15%, silicon-dioxide quality percentage composition are 5%-15%, all the other add the water digestion 0.5h-3h of 40 ℃-70 ℃ for the low-grade lime of other impurity by effective CaO quality percentage composition, the 2-6 that water add-on is lime quality doubly;
(2), lime classification: the thick milk of lime of gained after digestion is passed through to the separated classification of spinning liquid, the heavy material of gained is calcium carbonate, calcium sulfate, silicon-dioxide and the high coarse sand of other foreign matter content, the material that gained proportion is little is the refined lime breast that calcium carbonate, calcium sulfate, silicon-dioxide and other foreign matter content are low, and the butt mass ratio of gained coarse sand and refined lime breast is 1:1-2;
(3), coarse sand purifying treatment phosphogypsum slag field Chi Shui: the coarse sand of gained is joined in the water of pond, phosphogypsum slag field and carries out primary sedimentation reaction, stirring reaction 0.5h～2h at 25 ℃～50 ℃, controlling reaction end pH value is 2.0～2.5, has reacted rear filtration, is purified liquid and fluorine-containing slag;
(4), refined lime breast treatment and purification liquid is prepared phosphorus bearing slag: the refined lime breast of gained is joined and in scavenging solution, carries out secondary sedimentation reaction, stirring reaction 0.5h～2h at 25 ℃～50 ℃, controlling reaction end pH value is 5.5～6.5, has reacted rear filtration, and filter cake is in butt P
2o
5quality percentage composition is the phosphorus bearing slag of 30%-34%, filtrate continuation add refined lime breast to carry out three precipitin reaction to be neutralized to pH value be 8～10 rear filtrations, a filtered liquid part is returned to phosphoric acid systemic circulation and is used, a part is returned to milk of lime preparation system and is used.
2. according to the method for the described low-grade lime treatment phosphogypsum slag field Chi Shui of a kind of use of claim power, it is characterized in that phosphogypsum slag field Chi Shui is 1%-6% containing Vanadium Pentoxide in FLAKES quality percentage composition, fluorine-containing quality percentage composition is 0.3%-1.5%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528908A (en) * | 2014-12-12 | 2015-04-22 | 瓮福（集团）有限责任公司 | Method for removing fluorine in acidic wastewater by using lime serving as byproduct |
| CN104649724A (en) * | 2015-01-27 | 2015-05-27 | 瓮福（集团）有限责任公司 | Production method of calcium superphosphate |
| CN105000585A (en) * | 2015-06-12 | 2015-10-28 | 泰山石膏股份有限公司 | Ardealite neutralizing and purifying processing technology |
| CN105600992A (en) * | 2016-02-14 | 2016-05-25 | 瓮福（集团）有限责任公司 | Technology for preparing feed calcium from wastewater residues |
| CN105712529A (en) * | 2016-03-29 | 2016-06-29 | 瓮福（集团）有限责任公司 | Method for treating high-concentration acidic wastewater containing fluorine and phosphorus |
| CN106007051A (en) * | 2016-05-24 | 2016-10-12 | 瓮福（集团）有限责任公司 | Sewage treatment method for low-quality lime |
| 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 |
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| CN1283584A (en) * | 1999-08-04 | 2001-02-14 | 四川大学 | Process for preparing calcium hydrogen phosphate from middle-and low-grade phosphorus ore |
| CN101058414A (en) * | 2007-06-06 | 2007-10-24 | 四川绵竹新清华化工有限责任公司 | Reused process for waste water in calcium hydrogen orthophosphate production |
| CN102633384A (en) * | 2012-04-20 | 2012-08-15 | 瓮福（集团）有限责任公司 | Method for preparing phosphoric acid by recycling phosphorus from phosphorus-containing wastewater |
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| JPH10202271A (en) * | 1997-01-17 | 1998-08-04 | Kurita Water Ind Ltd | Treatment of waste water containing fluorine, phosphoric acid and organic matter |
| CN1283584A (en) * | 1999-08-04 | 2001-02-14 | 四川大学 | Process for preparing calcium hydrogen phosphate from middle-and low-grade phosphorus ore |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528908A (en) * | 2014-12-12 | 2015-04-22 | 瓮福（集团）有限责任公司 | Method for removing fluorine in acidic wastewater by using lime serving as byproduct |
| CN104649724A (en) * | 2015-01-27 | 2015-05-27 | 瓮福（集团）有限责任公司 | Production method of calcium superphosphate |
| CN105000585A (en) * | 2015-06-12 | 2015-10-28 | 泰山石膏股份有限公司 | Ardealite neutralizing and purifying processing technology |
| CN105000585B (en) * | 2015-06-12 | 2016-11-09 | 泰山石膏股份有限公司 | In ardealite and purification process technique |
| CN105600992A (en) * | 2016-02-14 | 2016-05-25 | 瓮福（集团）有限责任公司 | Technology for preparing feed calcium from wastewater residues |
| CN105712529A (en) * | 2016-03-29 | 2016-06-29 | 瓮福（集团）有限责任公司 | Method for treating high-concentration acidic wastewater containing fluorine and phosphorus |
| CN106007051A (en) * | 2016-05-24 | 2016-10-12 | 瓮福（集团）有限责任公司 | Sewage treatment method for low-quality lime |
| 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 |
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Application publication date: 20140305 |