CN104226278B - A kind of preparation method of thallium adsorbent and purposes - Google Patents
A kind of preparation method of thallium adsorbent and purposes Download PDFInfo
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- CN104226278B CN104226278B CN201410452028.9A CN201410452028A CN104226278B CN 104226278 B CN104226278 B CN 104226278B CN 201410452028 A CN201410452028 A CN 201410452028A CN 104226278 B CN104226278 B CN 104226278B
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Abstract
The preparation method and the purposes that the present invention relates to a kind of thallium adsorbent, comprise the following steps: S10, and get column chromatography polyamide materials and join in dilute hydrochloric acid solution, under room temperature, mix and soak 20-24 hour; S20, adds potassium ferrocyanide to the solution system in step S10, stirs and filters after standing 20-24 hour; S30, gets the solid matter after filtration, adds in ferric chloride solution, and on solid matter, appearance blueness precipitation, stirs 40-60 minute, till extremely blueness precipitates while no longer increasing; S40, the solidliquid mixture of filtration step S30, obtaining load has blue sedimentary solid, and cleans with clear water, obtains hygrometric state thallium adsorbent. This law preparation technology is simple, practical, and cost of material is cheap, is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to sewage treatment area, particularly a kind of preparation method of thallium adsorbent and purposes.
Background technology
Thallium is the slightly nattier blue silvery white ductile metal of one, and water insoluble and aqueous slkali, is soluble in acid.Conventionally being present in iron, zinc sulfides ore deposit with trace, is the rare dispersion of the typical case unit that occurring in nature existsElement is also a kind of hypertoxic heavy metal element simultaneously. It is only second to methyl mercury to people and mammiferous toxicity,Much larger than mercury, lead and arsenic, main manifestations is neurotoxicity, make people and mammiferous central nervous system,There is pathology in the position such as gastrointestinal system and kidney.
Along with thallium is in the extensive use of agricultural, industry and high-technology field, a large amount of thalliums and compound thereof enterEnter surrounding medium, as, give up containing the mine Weathering And Leaching in thallium mineral deposit, nonferrous metallurgical process, smeltingWater discharges etc., continue to increase the thallium entering in water body and soil, cause on the one hand environmental pollution, anotherBy food chain enrichment, serious threat human body and animal body health, particularly to drinking water supply on the one handSafety causes very big harm. Due to its high poison, thallium and compound thereof are listed in preferential control by China and are pollutedThing blacklist. How effectively preventing, control and administer thallium has very heavy to the pollution of water, soil environmentThe meaning of wanting.
At present, the improvement method of thallium polluted-water is few, especially lacks the effective technology of advanced treating. BeautifulState EPA recommends the activated alumina method of purification and ion-exchange, still, in actual applications, in waterCalcium, magnesium plasma background concn larger, these two kinds of methods are unsatisfactory to the removal effect of low concentration thallium.The industrial wastewater high to thallium concentration, by adding oxidant and alkaline matter, as lime etc., makes monovalence thalliumBe oxidized to trivalent thallium, generate precipitation and remove, but this method belong to primary treatment, residual thallium is still inclined to one sideHigh. In the emergency processing of recent year generation river thallium contamination accident, utilize thallium easily by " sponge inhalesAttached body " character of absorption, in contaminated water body, add the adsorbents such as manganese dioxide solid, reduce thalliumActivity rate also makes its precipitation or adds potassium permanganate and other medicaments, by oxidation, precipitation and absorptionReduce the concentration of thallium, but often will add a large amount of chemical drugs in order to make concentration drop to acceptable levelAgent, no matter and be to be suspended in water containing the precipitation of thallium, be still settled down to bed mud, remain potential prestigeThe side of body.
Summary of the invention
The object of the present invention is to provide a kind of cheap, thallium adsorbent that technique is simple, practicalPreparation method and purposes.
The present invention proposes a kind of preparation method of thallium adsorbent, and it comprises the following steps:
S10, gets column chromatography polyamide materials and joins in dilute hydrochloric acid solution, under room temperature, mixes and soaks20-24 hour;
S20, adds potassium ferrocyanide to the solution system in step S10, stirs and leaves standstillAfter 20-24 hour, filter;
S30, gets the solid matter after filtration, adds in ferric chloride solution, on described solid matter, occursBlueness precipitation, stirs 40-60 minute, till extremely blueness precipitates while no longer increasing;
S40, the solidliquid mixture of filtration step S30, obtaining load has blue sedimentary solid, andClean with clear water, obtain hygrometric state thallium adsorbent.
Preferably, also comprise step S50, the hygrometric state thallium adsorbent making is dried to moisture content littleIn 4%.
Preferably, described dry concrete steps are: the hygrometric state thallium adsorbent making is turned by Turnover BoxEnter in drying room, and by heated-air circulation oven, hygrometric state thallium adsorbent is dried, and at whole drying courseIn, bake out temperature is controlled at 45 DEG C-55 DEG C.
Preferably, the polyamide materials described in step S10 is polyamide or Fypro.
Preferably, the concentration of watery hydrochloric acid described in step S10 is 0.5mol/L, described polyamide materials and saltThe mass ratio of acid solution is 1:20.
Preferably, in step S20, add potassium ferrocyanide to the solution system in step S10, described AsiaThe concentration of the potassium ferricyanide is 0.1mol/L.
Preferably, in step S30, described ferric chloride concn is 0.01mol/L, and after described filtrationSolid matter and ferric chloride solution mass ratio are 1:20.
The present invention also proposes a kind of method of removing thallium in waste water, and it comprises the following steps:
S11, adopts wet method dress post, and the preparation method as described in claim 1 to 7 any one is preparedThallium adsorbent pack adsorption column into, blade diameter length ratio is 1:8-10;
S12, regulates the pH value of waste water to acid, flows through adsorption column with the flow velocity of 2-4BV/h.
Preferably, further comprising the steps of:
S13, the upon adsorption dose of leakage point that reaches capacity, gets the saturated potassium chloride containing 0.1mol/L hydrochloric acid solutionFor eluent, flow through adsorption column with the flow velocity of 1BV/h and carry out wash-out, and circulate 3-6 time, obtain eluent;
S14, toward eluent adding calcium hydroxide described in step S13 to solution PH > 7, adds vulcanized sodium,After reaction, filter, and the sediment of gained is pressed to dangerous disposition of solid waste.
The preparation method of the thallium adsorbent that the present invention proposes, technique is simple, practical, and cost of material is lowHonest and clean, be suitable for large-scale industrial production; And the adsorbent making has the effect of special efficacy exchange adsorption to thallium, can beIn the larger situation of calcium, magnesium, sulfate radical, chlorine plasma background concn, low concentration in Adsorption waterThallium, makes it reach standards for drinking water quality (GB5749-2006).
Detailed description of the invention
Should be appreciated that specific embodiment described herein is only in order to explain the present invention, not for limitFixed scope of the present invention.
The preparation method who the invention provides a kind of thallium adsorbent, it comprises the following steps:
S10, gets column chromatography polyamide materials and joins in dilute hydrochloric acid solution, under room temperature, mixes and soaks20-24 hour;
In practical operation, polyamide materials can first add water and wash away dust and powder, selects bulk or graininessMaterial material. Preferably, described polyamide materials is polyamide or Fypro.
S20, adds potassium ferrocyanide to the solution system in step S10, stirs and leaves standstillAfter 20-24 hour, filter;
It should be noted that after the filtrate of filtering gained is optionally supplemented hydrochloric acid and potassium ferrocyanide and can carry outReuse.
S30, gets the solid matter after filtration, adds in ferric chloride solution, occurs blue on solid matterPrecipitation, stirs 40-60 minute, till extremely blueness precipitates while no longer increasing;
In practical operation, the solid matter after filtration is polyamide granules or Fypro.
S40, the solidliquid mixture of filtration step S30, obtaining load has blue sedimentary solid, andClean with clear water, obtain hygrometric state thallium adsorbent.
Preferably, in order to be convenient for carrying and to preserve, the hygrometric state thallium adsorbent making also will be dried to and containWater rate is less than 4%. Particularly, described hygrometric state thallium adsorbent proceeds in drying room by Turnover Box, and logicalCross heated-air circulation oven wet granular is dried, and in whole drying course, bake out temperature is controlled at 45 DEG C-55 DEG C. After measured, this adsorbent is 56mg/g (butt particle) and 73 to the saturated adsorption capacity of thalliumMg/g (butt fiber).
The preparation method of the thallium adsorbent that the present invention proposes is using polyamide materials as carrier, under room temperatureBe immersed in 20-24 hour in dilute hydrochloric acid solution, in hydrochloric acid medium, the acid amides matrix in polyamide structureSonization is positively charged; While processing with potassium ferrocyanide solution, the amide groups absorption Fe (CN) of positive charge6 4-Anion; Again with ferric chloride solution processing, Fe (CN)6 4-Fe in ion and ferric chloride solution3+Reaction, fastFast-growing au bleu sediment-Prussian blue, and be attached in polyamide materials. Reaction equation is:
3Fe(CN)6 4-+4Fe3+→Fe4[Fe(CN)6]3↓
Having the sedimentary polyamide materials of this blueness to filter load cleans, obtains thallium adsorbent. This absorptionAgent has the effect of special efficacy exchange adsorption to thallium, can be larger at calcium, magnesium, sulfate radical, chlorine plasma background concnSituation under, the thallium of low concentration in Adsorption water, makes it reach standards for drinking water quality(GB5749-2006), and preparation technology is simple, practical, and cost of material is cheap, is suitable for large ruleMould industrial production.
The present invention also proposes a kind of method of removing thallium in waste water, and it comprises the following steps:
S11, adopts wet method dress post, packs the thallium adsorbent of preparing by above-mentioned preparation method into adsorption column,Blade diameter length ratio is 1:8-10;
S12, regulates the pH value of waste water to acid, flows through adsorption column with the flow velocity of 2-4BV/h.
What the present invention proposed utilizes thallium adsorbent to remove the method for thallium in waste water, packs thallium adsorbent into absorptionPost, in the time that waste water containing thallium flows through adsorption column, forms insoluble substance after the replaceable iron on Prussian blue of thalliumTIFe[Fe(CN)6, be attached on the adsorbent in adsorption column, thereby TI replaced to separation from waste waterOut.
Preferably, for adsorbent is reused, also to carry out finishing drilling to displacing the adsorbent of thalliumDo:
S13, the upon adsorption dose of leakage point that reaches capacity, gets the saturated potassium chloride containing 0.1mol/L hydrochloric acid solutionFor eluent, flow through adsorption column with the flow velocity of 1BV/h and carry out wash-out, and circulate 3-6 time, obtain eluent;
S14, toward adding calcium hydroxide in the eluent obtaining in step S13 to solution PH > 7, then addsVulcanized sodium, filters after reaction, and supernatant is integrated with to waste water, and the sediment of gained is discarded by dangerous solidThing is disposed.
Reach absorption saturated after, through containing the saturated potassium chloride of 0.1mol/L hydrochloric acid solution be eluent repeatedlyRinse, obtain the eluent containing thallium, this eluent is under alkali condition, taking vulcanized sodium as precipitating reagent, rawBecome thallium sulfide precipitation. By Separation of Solid and Liquid, obtain the sediment of Containing Sulfur thallium, useless by dangerous solidGurry is disposed; (, according to the regulation of " Chinese people's republicanism order prevention and control of environmental pollution by solid wastes method "It is collected and is under lock and key, and specify the hazardous waste disposal company of State Bureau of Environmental Protection's accreditation to enterRow is disposed. ) supernatant is directly incorporated into wastewater treatment.
Embodiment 1:
S10, gets 14～30 order column chromatography polyamides, at room temperature adds by 1:20 (weight ratio)Enter 0.5mol/LHCl solution, soak 20 hours.
S20, adds potassium ferrocyanide to making potassium ferrocyanide solution in the solution system in step S10Concentration is 0.1mol/L, stirs, and soaks after 24 hours and filters.
S30, gets the polyamide granules after filtration, adds 0.01mol/LFeCl by 1:20 (mass ratio)3In solution, occur blue precipitation on polyamide granules, continue low rate mixing 60min, extremely blue precipitation is notTill increasing again.
S40, filters and cleans with clear water, obtains hygrometric state thallium adsorbent.
Embodiment 2:
S10, gets 14～30 order column chromatography Fypros, at room temperature adds by 1:20 (weight ratio)Enter in 0.5mol/LHCl solution, soak 23 hours.
S20, adds potassium ferrocyanide to making potassium ferrocyanide solution in the solution system in step S10Concentration is 0.1mol/L, stirs, and leaves standstill after 20 hours and filters.
S30, gets the Fypro after filtration, adds 0.01mol/LFeCl by 1:20 (mass ratio)3In solution, occur blue precipitation on Fypro, continue low rate mixing 50min, extremely blue precipitation is notTill increasing again.
S40, filters and cleans with clear water, obtains hygrometric state thallium adsorbent.
Embodiment 3:
S10, gets 14～30 order column chromatography polyamides, at room temperature adds by 1:20 (weight ratio)Enter in 0.5mol/LHCl solution, soak 24 hours.
S20, adds potassium ferrocyanide to making potassium ferrocyanide solution in the solution system in step S10Concentration is 0.1mol/L, stirs, and leaves standstill after 22 hours and filters.
S30, gets the polyamide granules after filtration, adds 0.01mol/LFeCl by 1:20 (mass ratio)3In solution, occur blue precipitation on polyamide granules, continue low rate mixing 40min, extremely blue precipitation is notTill increasing again.
S40, filters and cleans with clear water, obtains hygrometric state thallium adsorbent.
Embodiment 4:
S11, adopts wet method dress post, packs the thallium adsorbent of preparing by above-mentioned preparation method into adsorption column,Blade diameter length ratio is 1:10.
S12, the water outlet taking certain smeltery after multi-grade chemical precipitation process is handling object, this water outlet containsHeavy metal ion especially containing a large amount of calcium ions, and is 0.24mg/L through surveying thallium content. Regulate this waste waterPH value to 4, flows through adsorption column with the flow velocity of 3BV/h.
Measure the thallium content in water outlet with ICP-MS method, result is lower than method detection limit 0.00005mg/L,Lower than the concentration limit of standards for drinking water quality (GB5749-2006).
S13, saturated reaching after leakage point upon adsorption, gets the saturated potassium chloride containing 0.1mol/L hydrochloric acid solutionFor eluent, flow through adsorption column with the flow velocity of 1BV/h the thallium adsorbent through step S20 is carried out to wash-out,And circulate 3-6 time, obtain eluent;
S14, toward adding calcium hydroxide in the eluent obtaining in step S30 to solution PH > 7, then addsVulcanized sodium, filtered after a period of time, and supernatant is integrated with to waste water, and the sediment of gained is by dangerous solidWaste disposal.
Embodiment 5:
S11, adopts wet method dress post, packs the thallium adsorbent of preparing by above-mentioned preparation method into adsorption column,Blade diameter length ratio is 1:8.
S12 is right as processing taking the embodiment water outlet of 4 Zhong Mou smelteries after multi-grade chemical precipitation process equallyResemble (containing thallium 0.24mg/L), regulate the pH value to 5.5 of this waste water, flow through adsorption column with the flow velocity of 4BV/h.
Measure the thallium content in water outlet with ICP-MS method, result is lower than method detection limit 0.00005mg/L,Lower than the concentration limit of standards for drinking water quality (GB5749-2006).
Embodiment 6:
S11, adopts wet method dress post, packs the thallium adsorbent of preparing by above-mentioned preparation method into adsorption column,Blade diameter length ratio is 1:9.
S12, the same water outlet after multi-grade chemical precipitation process with embodiment 4 Zhong Mou smelteries is (containing thallium0.24mg/L) be handling object, regulate the pH value to 5 of this waste water, flow through absorption with the flow velocity of 2BV/hPost.
Measure the thallium content in water outlet with ICP-MS method, result is lower than method detection limit 0.00005mg/L,Lower than the concentration limit of standards for drinking water quality (GB5749-2006).
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, not all in the present inventionSpirit and principle within, any amendment of doing, be equal to replacement, improvement etc., all should be included in thisWithin bright protection domain.
Claims (9)
1. a preparation method for thallium adsorbent, is characterized in that, comprises the following steps:
S10, gets column chromatography polyamide materials and joins in dilute hydrochloric acid solution, under room temperature, mixes and soaks20-24 hour;
S20, adds potassium ferrocyanide to the solution system in step S10, stirs and leaves standstillAfter 20-24 hour, filter;
S30, gets the solid matter after filtration, adds in ferric chloride solution, on described solid matter, occursBlueness precipitation, stirs 40-60 minute, till extremely blueness precipitates while no longer increasing; Described ferric chloride solutionConcentration be 0.01mol/L, and solid matter and ferric chloride solution mass ratio after described filtration is1：20；
S40, the solidliquid mixture of filtration step S30, obtaining load has blue sedimentary solid, andClean with clear water, obtain hygrometric state thallium adsorbent.
2. the preparation method of thallium adsorbent as claimed in claim 1, is characterized in that, also comprises stepS50, is dried to moisture content by the hygrometric state thallium adsorbent making and is less than 4%.
3. the preparation method of thallium adsorbent as claimed in claim 2, is characterized in that, described dryConcrete steps are: the hygrometric state thallium adsorbent making is proceeded in drying room by Turnover Box, and pass through hot blastCirculation baking oven is dried hygrometric state thallium adsorbent, and in whole drying course, bake out temperature is controlled at 45 DEG C-55℃。
4. the preparation method of thallium adsorbent as claimed in claim 1, is characterized in that, in step S10Described polyamide materials is polyamide or Fypro.
5. the preparation method of the thallium adsorbent as described in any one in claim 1 to 4, is characterized in that,The concentration of watery hydrochloric acid described in step S10 is 0.5mol/L, the quality of described polyamide materials and hydrochloric acid solutionThan being 1: 20.
6. the preparation method of the thallium adsorbent as described in any one in claim 1 to 4, is characterized in that,In step S20, add potassium ferrocyanide to the solution system in step S10, described potassium ferrocyanide denseDegree is 0.1mol/L.
7. the thallium adsorbent that the preparation method as described in claim 1 to 6 any one prepares is goingExcept the application of thallium in waste water.
8. a method of removing thallium in waste water, is characterized in that, it comprises the following steps:
S11, adopts wet method dress post, and the preparation method as described in claim 1 to 6 any one is preparedThallium adsorbent pack adsorption column into, blade diameter length ratio is 1: 8-10;
S12, regulates the pH value of waste water to acid, flows through adsorption column with the flow velocity of 2-4BV/h.
9. the method for thallium in removal waste water as claimed in claim 8, is characterized in that, also comprises followingStep:
S13, the upon adsorption dose of leakage point that reaches capacity, gets the saturated potassium chloride containing 0.1mol/L hydrochloric acid solutionFor eluent, flow through adsorption column with the flow velocity of 1BV/h and carry out wash-out, and circulate 3-6 time, obtain eluent;
S14, in the described eluent obtaining toward step S13, adding calcium hydroxide, to solution PH > 7, adds sulphurChange sodium, after reaction, filter, and the sediment of gained is pressed to dangerous disposition of solid waste.
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| CN106082502B (en) * | 2016-08-16 | 2019-06-18 | 华南理工大学 | A kind of method of thallium in removal waste water |
| CN110252270B (en) * | 2019-07-05 | 2022-04-19 | 生态环境部华南环境科学研究所 | Desorption recycling method and device for thallium-containing titanium peroxide |
| CN111186887B (en) * | 2020-01-19 | 2021-09-03 | 中南大学 | Method for removing and recovering thallium from industrial wastewater |
| CN115947432A (en) * | 2023-01-17 | 2023-04-11 | 中国科学院生态环境研究中心 | Method for removing trace thallium ions in water |
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| DE69608820T2 (en) * | 1996-03-08 | 2000-11-16 | Minnesota Mining & Mfg | ADSORPTION AGENT FOR CAESUMIONS AND METHOD FOR THEIR PRODUCTION |
| CN102836693B (en) * | 2012-09-19 | 2014-05-14 | 清华大学 | Magnetic-nucleus coated type inorganic ion adsorbent used for removing Cs ions in radioactive wastewater, and preparation method of same |
| CN103406097B (en) * | 2013-07-29 | 2015-05-20 | 中国科学院东北地理与农业生态研究所 | Magnetic Prussian blue carbon nano composite material and manufacturing method and application thereof |
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| CN101279249A (en) * | 2008-05-23 | 2008-10-08 | 清华大学 | Preparation of potassium zirconium hexacyanoferrate using pellet silica-gel as carrier |
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