CN103739048B - Defluorination medicine and preparation method thereof - Google Patents
Defluorination medicine and preparation method thereof Download PDFInfo
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- CN103739048B CN103739048B CN201310569409.0A CN201310569409A CN103739048B CN 103739048 B CN103739048 B CN 103739048B CN 201310569409 A CN201310569409 A CN 201310569409A CN 103739048 B CN103739048 B CN 103739048B
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Abstract
The invention discloses a wastewater defluorination medicine. The defluorination medicine is characterized in that the defluorination medicine contains rare earth elements and also contains polyacrylamide. The defluorination principle of the medicine is characterized in that fluorinions are removed through an ion precipitation method, the fluorinions combine with rare earth element ions to form a fluorinated rare earth precipitate, fluorinated rare earth is insoluble in water, and the fluorinions in water is removed through an ion co-precipitation effect, so the medicine has a very good selectivity, and the generated fluorinated rare earth is recovered to realize rare earth smelting. The defluorination medicine is suitable for removing low concentration fluorinion pollution factors in wastewater, and has the advantages of good defluorination effect, stability and low processing cost, and the generated fluorinated rare earth is recoverable.
Description
Technical field
The present invention relates to a kind of fluoride waste process field, relate in particular to and be specifically related to FLUORIDE REMOVAL IN WASTEWATER medicament and the preparation method that rare-earth compound is main component.
Background technology
Fluorine is one of trace element of needed by human, and the suitable fluorine mass concentration of tap water is 0.5-1.0mg/L.When tap water lacks fluorine, easily suffer from dental caries; If but long-term drinking fluorine mass concentration is higher than the water of 1.0mg/L, can cause that dental fluorosis is sick; The water that long-term drinking fluorine mass concentration is 3-6mg/L, can cause osteofluorosis.China's Fluorine Containing Groundwater is widely distributed, especially in northwest arid area, approximately has 70,000,000 people to drink the water that fluorine content exceeds standard, and causes fluorosis in various degree.Industrial, in the waste water of the industry such as fluorine-containing ore extraction, Metal smelting, aluminium processing, coke, glass, electronics, plating, chemical fertilizer, agricultural chemicals discharge, often contain the fluorochemical of high density, cause environmental pollution.Defluorinating process research is the important topic of domestic and international environmental protection and health field always.
Fluoride waste, most domestic factory there is no perfect treatment facility at present, and the fluorine in wastewater content discharging surpasses discharging standards, serious environment pollution.According to national sewage comprehensive emission standard, fluorinion concentration should be less than 10mg/L, and in the emission standard of part industry standard or special discharge areas, fluorinion concentration should be less than 2mg/L, and drinking water standard requires fluorinion concentration to require below 1mg/L.Conventional FLUORIDE REMOVAL IN WASTEWATER medicament is roughly divided into two classes both at home and abroad at present, i.e. calcium salt precipitation method defluorination medicament and absorption method defluorination medicament.
Calcium salt mainly contains CaO, CaCl
2, Ca (OH)
2deng, by adding calcium salt, be main pharmaceutical chemicals, form that Calcium Fluoride (Fluorspan) precipitation or Calcium Fluoride (Fluorspan) are adsorbed in formed throw out and coprecipitation.The method is simple, processing is convenient, and expense is low, but lime solubleness is low, can only add with milk sap, and the CaF producing
2precipitation is wrapped in Ca (OH)
2the surface of particle, make it to be fully utilized, thereby consumption is large.Fluorine in wastewater content after processing generally can only drop to 20-50mg/L, can not reach the primary standard of stipulating in < < integrated wastewater discharge standard > >.And existing body refuse sedimentation slow, dehydration difficulty, processes the large volume exhaust thing cycle long, the shortcomings such as the inadaptable continuous blow-down of processing continuously.
Absorption method defluorination medicament mainly contains activated alumina, clinoptilolite, activated magnesia etc., in recent years, has also reported the higher sorbent materials of adsorption capacity of fluoride ion such as hydroxyapatite, zirconium white and cerous hydroxide.Conventional sorbent material is as less of 0.06-2.0mg/g in the fluorine adsorptive capacity of clinoptilolite and activated magnesia, and treatment effect is poor.The fluorine adsorptive capacity of calcium phosphate powder and activated magnesia reaches 3.5-10mg/g, but easily runs off in use procedure.And take rare earth element hydrous oxide and the rare earth salts that cerium and lanthanum be representative, the negatively charged ion such as the fluorine in water, arsenate are had to stronger avidity, thereby take the sorbent material that rare earth element is main adsorption component, because its adsorptive capacity is large, pollute the little and easy to operate concern both domestic and external that obtained.Rare earth element is to be caused by the relevant protonation reaction of its surface hydroxyl as the ion-exchange of sorbent material to adsorption property, and its defluorination mechanism is all coordinated water on metal ion and the F in solution
-exchange, and most rare earth as sorbent material be all by rare earth loaded on the fibrous material of high surface area, because Fibriform adsorbents has larger specific surface area and stronger physical strength, and the coordination ability of rare earth and F-is strong, so in conjunction with making rare-earth oxide there is higher loading capacity to the fluorion in water, stronger adsorption selectivity, sorbent material fluorine adsorptive capacity reaches 30mg/g.
Rare earth class sorbent material, protonation reaction is only surface adsorption and expensive, although can regenerate, regeneration effect is general, processing cost is high.The sorbent material of reporting in addition the carrier surface carrier band cerous hydroxides such as aluminium or titanium is better to fluorion adsorption effect, but which kind of absorption method no matter, rare earth compound is due to its unique fluorine affinity, not only can effectively remove fluorine excessive in water body, can improve traditional filter material surface tissue simultaneously, increase filter material surface adsorption potential, for the removal of other impurity in water, also there is good effect as heavy metal ion and part mineral ion, therefore all cannot carry out the selective adsorption of fluorion, the adsorption efficiency of sorbent material is lower, especially when waste water contains oily substance, during organic pollution materials, sorbent material can be saturated rapidly, almost cannot normally work.Therefore use sorbent material to carry out defluorination processing, cost is expensive, regeneration difficulty and be subject to the condition restriction of other pollution factor in waste water while using, and cannot in production reality, normally use.
Summary of the invention
For above-mentioned the deficiencies in the prior art, it is the defluorination medicament of main component that the object of the invention is to provide a kind of rare earth compound, with and preparation method thereof, be applicable in waste water, the removal of the low dose fluoride ionic soil factor, be characterized in that defluorination effect is good and stable, processing cost is low, and the rare earth fluoride of generation is recyclable.
The problem existing for solving above-mentioned prior art, reaches described object, and the technical scheme that the present invention takes is: a kind of FLUORIDE REMOVAL IN WASTEWATER medicament, it is characterized in that, and in described defluorination medicament, contain rare earth element.
Further, described rare earth element is rare earth chloride or carbonated rare earth.
Further, the defluorination medicament that described rare earth chloride forms is the aqueous solution, and rare earth chloride accounts for the 1-65% of defluorination medicament total mass, is preferably 5-10%, the preferred Lanthanum trichloride of described rare earth chloride, Cerium II Chloride, praseodymium chloride or Neodymium trichloride.
Further, the defluorination medicament that described carbonated rare earth forms is Powdered, and carbonated rare earth accounts for defluorination medicament total mass: be more than or equal to 80%, and be less than 100%, described carbonated rare earth is preferably Phosbloc, cerous carbonate, praseodymium carbonate or neodymium carbonate.
Further, in described defluorination medicament, also contain polyacrylamide, quality is 0.1 ‰-1 ‰ of defluorination medicament total mass.
Further, the addition of described polyacrylamide: massfraction is 0.1 ‰-0.2 ‰ in the defluorination medicament that contains rare earth chloride, the massfraction in the defluorination medicament that contains carbonated rare earth is 0.5 ‰-1 ‰.
The preparation method of the defluorination medicament that a kind of rare earth chloride forms is as follows:
(1) according to the massfraction preparation re chloride of 1-65%, and mix;
(2) in the re chloride described in step (1), by 0.1 ‰ of gross weight-0.2 ‰, add flocculation agent, mix, making rare earth chloride is the FLUORIDE REMOVAL IN WASTEWATER medicament of main component.
The preparation method of the defluorination medicament that a kind of carbonated rare earth forms is as follows:
The carbonated rare earth of described dosage ratio is mixed with polyacrylamide, stir.
The using method of the defluorination medicament that a kind of rare earth chloride forms: fluoride waste water inlet fluorinion concentration is lower than 50mg/L, pH value is controlled at neutral 7 left and right, according to the mass ratio 0.24-0.25 of fluorion and rare earth chloride, add rare earth chloride defluorination medicament, stir 30min, fully reaction, standing sedimentation 60min, the precipitation of formation is carried out solid-liquid separation after reclaiming, and is further used for rare-earth smelting.
The defluorination medicament using method that a kind of carbonated rare earth forms is as follows:
Fluoride waste fluorinion concentration is lower than 50mg/L, pH value is controlled at 2.5 left and right, according to the mass ratio 0.22-0.29 of fluorion and carbonated rare earth, add carbonated rare earth defluorination medicament, stir 30min, fully reaction, standing sedimentation 60min, carries out solid-liquid separation after the rare earth fluoride precipitation of formation reclaims, and is further used for rare-earth smelting.
Medicament of the present invention, its defluorination principle is to belong to ion precipitation method to remove fluorion, fluorion is combined with rare earth element ion and is formed rare earth fluoride precipitation, rare earth fluoride is water insoluble, by the coprecipitated effect of ion, remove the fluorion in water, therefore have good selectivity, the rare earth fluoride of generation reclaims for rare-earth smelting.Reactional equation is as follows:
F
-+Re
3+→ReF
3
Beneficial effect of the present invention is:
(1) routine of defluorination medicament of the present invention adds, can make waste water fluorinion concentration≤5mg/L after treatment, lower than the first discharge standard (10mg/L is following) of regulation in < < integrated wastewater discharge standard > > (GB8978-2002), lower than the special emission limit of stipulating in < < rare-earth industry pollutant emission standard > > (8 mg/L are following).
(2) slightly excessive the adding of defluorination medicament of the present invention, can make waste water fluorinion concentration≤2mg/L after treatment, lower than the special emission limit of fluorion (2 mg/L are following) (10mg/L is following) of regulation in < < copper, nickel, cobalt emission of industrial pollutants standard > > (GB25467-2010).
(3) defluorination medicament of the present invention has selectivity to the removal of fluorinion in waste water, can not be subject in waste water other pollution factor as the impact of the pollution factors such as oil, COD, SS, can realize the fluoride ion removing under non-strong alkaline condition.
(4) defluorination medicament of the present invention is to reach by the coprecipitated mode of ion the object of removing fluorion, rare earth element ion in medicament and fluorion form rare earth fluoride precipitation, rare earth fluoride precipitation is water insoluble, nitric acid, hydrochloric acid, sulfuric acid, and chemical property is highly stable; The rare earth fluoride throw out generating can be back to rare-earth smelting, again make the raw material that rare earth chloride is produced as defluorination medicament after solid-liquid separation, and rare earth element without running off, greatly reduces cost for wastewater treatment in defluorination process.
(5) defluorination medicament of the present invention is applied in FLUORIDE REMOVAL IN WASTEWATER process, when the rare earth fluoride purity that forms under certain waste water quality condition is higher, can be applicable to precursor and produces.
(6) precipitate particles of the formation of the fluorion in this defluorination medicament and waste water rare earth fluoride is thin, the settling time is longer, the present invention has added polyacrylamide as flocculation agent in defluorination medicament, avoid because using inorganic salts flocculation agent, be combined with fluorinion in waste water and form precipitation, cause in rare earth fluoride precipitation and carry a large amount of impurity secretly, be convenient to the recovery of rare earth fluoride, shortened the sedimentary settling time of rare earth fluoride, improved effect of settling, reduce the investment of defluorination precipitation apparatus.
(7) compared with prior art, defluorination medicament of the present invention, the rare earth fluoride precipitation that forms recoverable by rare earth element ion and fluorion is removed fluorion, guaranteeing on water outlet fluorion basis up to standard, can realize the recycling of fluorion, defluorination medicament rare earth elements, avoid usining rare-earth compound as difficult problems such as use cost costliness that sorbent material was brought, adsorbent reactivation weak effects.
Embodiment
Embodiment 1
Defluorination medicament preparation method of the present invention is as follows:
Raw material: lanthanum chloride solution (content 60%), polyacrylamide (particulate state, content 90%), pure water.
Preparation: the lanthanum chloride solution that (1) water is 60% by content is diluted to 5%, and mixes.
(2) in the lanthanum chloride solution of 5% described in step (1), 0.2 ‰ add polyacrylamide in proportion, mix, and stir 1h, and making Lanthanum trichloride is the FLUORIDE REMOVAL IN WASTEWATER medicament of main component.
Be applied to certain rare earth metallurgy degree of depth defluorination, water inlet fluorinion concentration is 48mg/L, and pH value is 7.14, and quantity discharged is 10m
3/ d, adds Lanthanum trichloride defluorination medicament 3.88kg/m
3, water outlet fluorinion concentration is 4.01mg/L, and water outlet pH value is 6.86, and the yield of lanthanum fluoride is 1.26kg/d, and the rate of recovery is 83.4%.
Embodiment 2
Raw material: solution of cerium chloride by oxidation (content 65%), polyacrylamide (particulate state, content 92%), pure water.
Preparation: the solution of cerium chloride by oxidation that (1) water is 65% by content is diluted to 10%, and mixes.
(2) in the solution of cerium chloride by oxidation of 10% described in step (1), 0.1 ‰ add polyacrylamide in proportion, mix, and stir 1h, and making Cerium II Chloride is the FLUORIDE REMOVAL IN WASTEWATER medicament of main component.
Be applied to certain rare earth metallurgy degree of depth defluorination, water inlet fluorinion concentration is 44mg/L, and pH is 7.02, and quantity discharged is 12m
3/ d, adds Cerium II Chloride defluorination medicament 1.73kg/m
3, water outlet fluorinion concentration is 3.91mg/L, and pH value is 6.72, and the yield of cerium fluoride is 1.344kg/d, and the rate of recovery is 83.6%.
Embodiment 3
Raw material: praseodymium chloride solution (content 56%), polyacrylamide (particulate state, content 88%), pure water.
Preparation: the praseodymium chloride solution dilution to 5% that (1) water is 65% by content, and mix.
(2) in the praseodymium chloride solution of 5% described in step (1), 0.1 ‰ add polyacrylamide in proportion, mix, and stir 1h, and making praseodymium chloride is the FLUORIDE REMOVAL IN WASTEWATER medicament of main component.
Be applied to certain waste gas containing fluoride absorption liquid defluorination, water inlet fluorinion concentration is 52mg/L, and pH is 6.89, and quantity discharged is 10m
3/ d, adds praseodymium chloride defluorination medicament 4.31kg/m
3, water outlet fluorinion concentration is 4.5mg/L, and pH value is 6.52, and the yield of praseodymium fluoride is 1.09kg/d, and the rate of recovery is 85.6%.
Embodiment 4
Raw material: neodymium chloride solution (content 66%), polyacrylamide (particulate state, content 90%), pure water.
Preparation: the neodymium chloride solution that (1) water is 66% by content is diluted to 10%, and mixes.
(2) in the neodymium chloride solution of 10% described in step (1), 0.2 ‰ add polyacrylamide in proportion, mix, and stir 1h, and making Neodymium trichloride is the FLUORIDE REMOVAL IN WASTEWATER medicament of main component.
Be applied to certain waste gas containing fluoride absorption liquid defluorination, water inlet fluorinion concentration is 56mg/L, and pH is 6.72, and quantity discharged is 8m
3/ d, adds Neodymium trichloride defluorination medicament 2.3kg/m
3, water outlet fluorinion concentration is 4.8mg/L, and pH value is 6.41, and the yield of neodymium fluoride is 1.17kg/d, and the rate of recovery is 81%.
Embodiment 5
Raw material: lanthanum chloride solution (content 60%), polyacrylamide (particulate state, content 90%), pure water.
Preparation: the lanthanum chloride solution that (1) water is 60% by content is diluted to 1%, and mixes.
(2) in the lanthanum chloride solution of 1% described in step (1), 0.1 ‰ add polyacrylamide in proportion, mix, and stir 1h, and making Lanthanum trichloride is the FLUORIDE REMOVAL IN WASTEWATER medicament of main component.
Be applied to certain rare earth metallurgy degree of depth defluorination, water inlet fluorinion concentration is 48mg/L, and pH value is 7.14, and quantity discharged is 10m
3/ d, adds Lanthanum trichloride defluorination medicament 19.4kg/m
3, water outlet fluorinion concentration is 4.21mg/L, and water outlet pH value is 6.92, and the yield of lanthanum fluoride is 1.21kg/d, and the rate of recovery is 80.3%.
Embodiment 6
Raw material: solution of cerium chloride by oxidation (content 65%), polyacrylamide (particulate state, content 92%), pure water.
Preparation: in described 65% solution of cerium chloride by oxidation, 0.2 ‰ add polyacrylamide in proportion, mixes, and stirs 1h, and making Cerium II Chloride is the FLUORIDE REMOVAL IN WASTEWATER medicament of main component.
Be applied to certain rare earth metallurgy degree of depth defluorination, water inlet fluorinion concentration is 44mg/L, and pH is 7.02, and quantity discharged is 12m
3/ d, adds Cerium II Chloride defluorination medicament 0.27kg/m
3, water outlet fluorinion concentration is 3.96mg/L, and pH value is 6.68, and the yield of cerium fluoride is 1.336kg/d, and the rate of recovery is 80.5%.
Embodiment 7
Raw material: Phosbloc (Powdered, 80%), polyacrylamide (particulate state, 90%)
Ratio according to 0.2 ‰ is mixed Phosbloc with polyacrylamide, stir.
Be applied to certain rare earth metallurgy degree of depth defluorination, water inlet fluorinion concentration is 48mg/L, and pH value is 2.56, and quantity discharged is 10m
3/ d, adds Phosbloc defluorination medicament 0.206kg/m
3, water outlet fluorinion concentration is 4.98mg/L, and water outlet pH value is 5.2, and the yield of lanthanum fluoride is 1.19kg/d, and the rate of recovery is 80.5%.
Embodiment 8
Raw material: cerous carbonate (Powdered, 92%), polyacrylamide (particulate state, 89%)
Ratio according to 0.1 ‰ is mixed cerous carbonate with polyacrylamide, stir.
Be applied to certain rare earth metallurgy degree of depth defluorination, water inlet fluorinion concentration is 44mg/L, and pH is 2.6, and quantity discharged is 12m
3/ d, adds cerous carbonate defluorination medicament 0.161kg/m
3, water outlet fluorinion concentration is 4.2mg/L, and pH value is 5.0, and the yield of cerium fluoride is 1.255kg/d, and the rate of recovery is 82%.
Embodiment 9
Raw material: praseodymium carbonate (Powdered, 99%), polyacrylamide (particulate state, 92%)
Ratio according to 0.1 ‰ is mixed praseodymium carbonate with polyacrylamide, stir.
Be applied to certain waste gas containing fluoride absorption liquid defluorination, water inlet fluorinion concentration is 52mg/L, and pH is 2.53, and quantity discharged is 10m
3/ d, adds praseodymium carbonate defluorination medicament 0.194kg/m
3, water outlet fluorinion concentration is 4.6mg/L, and pH value is 5.19, and the yield of praseodymium fluoride is 1.342kg/d, and the rate of recovery is 81.5%.
Embodiment 10
Raw material: neodymium carbonate (Powdered, 91%), polyacrylamide (particulate state, 90%)
Ratio according to 0.2 ‰ is mixed neodymium carbonate with polyacrylamide, stir.
Be applied to certain waste gas containing fluoride absorption liquid defluorination, water inlet fluorinion concentration is 56mg/L, and pH is 2.42, and quantity discharged is 8m
3/ d, adds Neodymium trichloride defluorination medicament 0.233kg/m
3, water outlet fluorinion concentration is 4.4mg/L, and pH value is 5.2, and the yield of neodymium fluoride is 1.19kg/d, and the rate of recovery is 81.8%.
Claims (1)
1. a using method for FLUORIDE REMOVAL IN WASTEWATER medicament, is characterized in that,
1) in described defluorination medicament, contain rare earth element; Described rare earth element be in lanthanum, cerium, praseodymium or neodymium any one or two or more; Described rare earth element is at least one in rare earth chloride or carbonated rare earth; The defluorination medicament that described rare earth chloride forms is the aqueous solution, and rare earth chloride accounts for the 1-65% of defluorination medicament total mass; The defluorination medicament that described carbonated rare earth forms is Powdered, and carbonated rare earth accounts for defluorination medicament total mass: be more than or equal to 80%, and be less than 100%; In described defluorination medicament, also contain polyacrylamide, the addition of described polyacrylamide: in the defluorination medicament forming at rare earth chloride, massfraction is 0.1 ‰-0.2 ‰, the massfraction in the defluorination medicament forming at carbonated rare earth is 0.5 ‰-1 ‰;
2) preparation method of described defluorination medicament:
The preparation method of the defluorination medicament that A. rare earth chloride forms is as follows:
(a) according to the massfraction preparation re chloride of 1-65%, and mix;
(b) in the re chloride described in step (a), by 0.1 ‰ of gross weight-0.2 ‰, add flocculation agent, mix, making rare earth chloride is the FLUORIDE REMOVAL IN WASTEWATER medicament of main component;
The preparation method of the defluorination medicament that B. carbonated rare earth forms is as follows: the carbonated rare earth of described dosage ratio is mixed with polyacrylamide, stir;
3) the use step of described defluorination medicament:
The using method of the defluorination medicament that A. rare earth chloride forms: pH value is controlled at neutral 7 left and right, according to the mass ratio 0.24-0.25 of fluorion and rare earth chloride, add rare earth chloride defluorination medicament, stir 30min, fully reaction, standing sedimentation 60min, the precipitation forming is carried out solid-liquid separation after reclaiming, and is further used for rare-earth smelting;
B. the defluorination medicament using method that carbonated rare earth forms is as follows: pH value is controlled at 2.5 left and right, according to the mass ratio 0.22-0.29 of fluorion and carbonated rare earth, add carbonated rare earth defluorination medicament, stir 30min, fully reaction, standing sedimentation 60min, after the rare earth fluoride precipitation forming reclaims, carry out solid-liquid separation, be further used for rare-earth smelting.
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| JP4525014B2 (en) * | 2002-07-08 | 2010-08-18 | 旭硝子株式会社 | By-product salt purification method, by-product salt and snow melting agent |
| KR20080058077A (en) * | 2006-12-21 | 2008-06-25 | 주식회사 포스코 | Method for treating wastewater including fluorine |
| CN102272061A (en) * | 2008-11-11 | 2011-12-07 | 莫利康普矿物有限责任公司 | Target material removal using rare earth metals |
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Inventor after: Han Siyu Inventor after: Han Zhengchang Inventor after: Ma Junjun Inventor after: Wu Chuanbao Inventor after: Zhang Shoubing Inventor after: Xia Jinlian Inventor after: Chai Huili Inventor after: Yu Lei Inventor before: Han Siyu Inventor before: Han Zhengchang Inventor before: Liu Dacai Inventor before: Ma Junjun Inventor before: Wang Zhilei Inventor before: Ling Ling |
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Application publication date: 20140423 Assignee: Yancheng Guotou Environmental Technology Co.,Ltd. Assignor: NANJING G+W ENVIRONMENT ENGINEERING Co.,Ltd. Contract record no.: X2021980001429 Denomination of invention: Application method of a kind of wastewater defluorination agent Granted publication date: 20141112 License type: Exclusive License Record date: 20210304 |