CN103738967A - Method for production of sodium fluosilicate from fluorine-containing acidic wastewater - Google Patents
Method for production of sodium fluosilicate from fluorine-containing acidic wastewater Download PDFInfo
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- CN103738967A CN103738967A CN201310602976.1A CN201310602976A CN103738967A CN 103738967 A CN103738967 A CN 103738967A CN 201310602976 A CN201310602976 A CN 201310602976A CN 103738967 A CN103738967 A CN 103738967A
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Abstract
The invention discloses a method for production of sodium fluosilicate from fluorine-containing acidic wastewater. The method includes: taking fluorine-containing acidic wastewater as a raw material, adding a proper amount of diatomite and a sodium carbonate solution, controlling the reaction temperature and reaction time, filtering the solution at the end of reaction, and drying the filter cake, thus obtaining a sodium fluosilicate product. The added sodium carbonate and the acidic wastewater are in a mass ratio of 2.0%-2.2%, the added diatomite and the acidic wastewater are in a mass ratio of 1.0%-1.5%, the reaction temperature is 50DEG C-70DEG C, and the reaction time is 2h-3h. With the method provided by the invention, the fluorine content of the acidic wastewater is reduced to 0.1%-0.2% after treatment, and the phosphorus content is almost unchanged. Meanwhile, after deep defluorination, the treated water can be used for production of feed grade calcium hydrogen phosphate, thus realizing recycling of phosphorus, fluorine, and silicon resources. The method provided reduces the production cost, realizes recycling of resources, and has great economic benefits and environmental protection benefits.
Description
Technical field
The present invention relates to Wet-process Phosphoric Acid Production technical field.Be specifically related to a kind of acidic fluoride-containing waste water and produce the method for Sodium Silicofluoride.
Background technology
At present, chemical enterprise is faced with severe environmental protection pressure, in Large-scale Phosphorus Chemical Manufacture enterprise, has a large amount of acidic fluoride-containing waste water, how to make good use of these waste water, and the recycling that realizes waste resource is to need the problem of solution badly.It is generally to utilize phosphoric acid fluorinated tail gas in composite fertilizer's production process or the silicofluoric acid that produces in Phosphoric Acid Concentration process reacts and produces with sodium sulfate or sodium-chlor that Sodium Silicofluoride is produced, and Chinese patent CN101972584, CN102153091 have the production method of mentioning about Sodium Silicofluoride.
The acidic fluoride-containing waste water producing for present phosphorous chemical industry enterprise, is mainly in acid waste water, to add lime to process, and the liquid phase after processing is discharged after reaching industrial discharge standard, not only improves production cost, and causes the waste of resource.Along with the development of fine chemistry industry, the utilization of fluorine resource will more and more come into one's own.
Summary of the invention
Main purpose of the present invention is to be devoted to the materials such as fluorine in recovered acid wastewater, silicon to produce Sodium Silicofluoride product, is characterized in adding sodium carbonate and diatomite by acidic fluoride-containing waste water, at suitable temperature, reacts and produces Sodium Silicofluoride.
The present invention adopts following technical measures to realize, and concrete steps are: take acidic fluoride-containing waste water as raw material, add appropriate diatomite and sodium carbonate solution, control temperature of reaction and reaction times, after having reacted, solution is filtered, filter cake is dried, and obtains Sodium Silicofluoride product.
The main component of acidic fluoride-containing waste water is,
| Index | P | F | SiO 2 | SO 4 |
| Content (%) | 1.6~1.9 | 0.75~0.95 | 0.16~0.20 | 0.2~0.3 |
The add-on of sodium carbonate and the mass ratio of acid waste water are: 2.0% ~ 2.2%, and the mass ratio of diatomaceous add-on and acid waste water is: 1.0% ~ 1.5%.
Temperature of reaction is: 50 ℃ ~ 70 ℃, the reaction times is: 2h ~ 3h.
Beneficial effect of the present invention: acid waste water after treatment, fluorine content in water is reduced to 0.1% ~ 0.2%, phosphorus content is almost constant, can be for the production of calcium hydrophosphate fodder after water after simultaneously processing carries out degree of depth defluorinate again, realize the recycling of phosphorus, fluorine, silicon resource, reduce production costs, realize the recycle of resource, there is larger economic benefit and environmental benefit.
Embodiment
By specific embodiment, further illustrate the present invention below, but be not used for limiting the scope of the invention.
Embodiment 1:
A kind of acidic fluoride-containing waste water is produced the method for Sodium Silicofluoride, take 1000g acidic fluoride-containing waste water, its main component is, fluorine content is 0.92%, silicon-dioxide is 0.18%, sulfate radical is 0.22%, phosphorus is 1.7%, then to adding 20g sodium carbonate, add 10g diatomaceous, temperature of reaction is for being controlled at 50 ℃.Reaction times is 2h, after having reacted, solution is filtered, and filter cake is dried, and obtains Sodium Silicofluoride product.In product, the content of Sodium Silicofluoride reaches more than 95%.In acid waste water after processing, the content of fluorine is 0.16%, the content of phosphorus is 1.6%, silicon-dioxide is 0.07%, sulfate radical content is 0.19%, and the water after processing returns to calcium hydrophosphate fodder device and uses as raw materials for production.
Embodiment 2:
A kind of acidic fluoride-containing waste water is produced the method for Sodium Silicofluoride, take 1000g acidic fluoride-containing waste water, its main component is, fluorine content is 0.78%, silicon-dioxide is 0.20%, sulfate radical is 0.20%, phosphorus is 1.9%, then to adding 22g sodium carbonate, add 15g diatomaceous, temperature of reaction is for being controlled at 60 ℃.Reaction times is 2.5h, after having reacted, solution is filtered, and filter cake is dried, and obtains Sodium Silicofluoride product.In product, the content of Sodium Silicofluoride reaches 92%.In acid waste water after processing, the content of fluorine is 0.11%, the content of phosphorus is 1.8%, silicon-dioxide is 0.10%, sulfate radical content is 0.20%, and the water after processing returns to calcium hydrophosphate fodder device and uses as raw materials for production.
Embodiment 3:
A kind of acidic fluoride-containing waste water is produced the method for Sodium Silicofluoride, take 1000g acidic fluoride-containing waste water, its main component is, fluorine content is 0.85%, silicon-dioxide is 0.20%, sulfate radical is 0.19%, phosphorus is 1.9%, then to adding 20g sodium carbonate, add 1,5g diatomaceous, temperature of reaction is for being controlled at 70 ℃.Reaction times is 2h, after having reacted, solution is filtered, and filter cake is dried, and obtains Sodium Silicofluoride product.In product, the content of Sodium Silicofluoride reaches more than 97%.In acid waste water after processing, the content of fluorine is 0.09%, the content of phosphorus is 1.7%, silicon-dioxide is 0.06%, sulfate radical content is 0.20%, and the water after processing returns to calcium hydrophosphate fodder device and uses as raw materials for production.
Claims (1)
1. acidic fluoride-containing waste water is produced a method for Sodium Silicofluoride, it is characterized in that: take acidic fluoride-containing waste water as raw material, add appropriate diatomite and sodium carbonate solution, control temperature of reaction and reaction times, after having reacted, solution is filtered, filter cake is dried, and obtains Sodium Silicofluoride product; The quality percentage composition of the main component of acidic fluoride-containing waste water is,
The add-on of sodium carbonate and the mass ratio of acid waste water are: 2.0% ~ 2.2%, and the mass ratio of diatomaceous add-on and acid waste water is: 1.0% ~ 1.5%, temperature of reaction is: 50 ℃ ~ 70 ℃, the reaction times is: 2 h ~ 3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310602976.1A CN103738967A (en) | 2013-11-26 | 2013-11-26 | Method for production of sodium fluosilicate from fluorine-containing acidic wastewater |
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| CN201310602976.1A CN103738967A (en) | 2013-11-26 | 2013-11-26 | Method for production of sodium fluosilicate from fluorine-containing acidic wastewater |
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| CN103738967A true CN103738967A (en) | 2014-04-23 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104555962A (en) * | 2015-01-05 | 2015-04-29 | 云南铜业胜威化工有限公司 | Method for increasing defluorination rate of high-impurity concentrated phosphoric acid |
| CN109761238A (en) * | 2019-03-22 | 2019-05-17 | 盛隆资源再生（无锡）有限公司 | A method of utilizing fluorine-containing phosphorous devil liquor recovery prodan and phosphoric acid |
| CN114349570A (en) * | 2022-02-11 | 2022-04-15 | 瓮福（集团）有限责任公司 | Preparation method of calcium silicon fertilizer |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624203A (en) * | 2009-08-03 | 2010-01-13 | 中昊晨光化工研究院 | Method for preparing calcium fluoride from waste water containing fluorine |
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2013
- 2013-11-26 CN CN201310602976.1A patent/CN103738967A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101624203A (en) * | 2009-08-03 | 2010-01-13 | 中昊晨光化工研究院 | Method for preparing calcium fluoride from waste water containing fluorine |
Non-Patent Citations (1)
| Title |
|---|
| 陈献桃: "以Na2SiF6固相形式回收钙镁磷肥厂含氟废水中的氟", 《岳阳师范学院学报（自然科学版）》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104555962A (en) * | 2015-01-05 | 2015-04-29 | 云南铜业胜威化工有限公司 | Method for increasing defluorination rate of high-impurity concentrated phosphoric acid |
| CN109761238A (en) * | 2019-03-22 | 2019-05-17 | 盛隆资源再生（无锡）有限公司 | A method of utilizing fluorine-containing phosphorous devil liquor recovery prodan and phosphoric acid |
| CN109761238B (en) * | 2019-03-22 | 2021-04-06 | 盛隆资源再生（无锡）有限公司 | Method for recovering sodium fluosilicate and phosphoric acid by using fluorine-containing and phosphorus-containing waste liquid |
| CN114349570A (en) * | 2022-02-11 | 2022-04-15 | 瓮福（集团）有限责任公司 | Preparation method of calcium silicon fertilizer |
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Application publication date: 20140423 |