CN103880143B - Red mud is utilized to prepare the technique of arsenic removal composite - Google Patents
Red mud is utilized to prepare the technique of arsenic removal composite Download PDFInfo
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- CN103880143B CN103880143B CN201410140102.3A CN201410140102A CN103880143B CN 103880143 B CN103880143 B CN 103880143B CN 201410140102 A CN201410140102 A CN 201410140102A CN 103880143 B CN103880143 B CN 103880143B
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Abstract
The invention discloses a kind of technique utilizing red mud to prepare arsenic removal composite, it is characterized in that, is raw material with red mud, comprises the steps: that (1) gets red mud slurry, adds hydrochloric acid dilute solution, stirs after being warming up to 80 DEG C ~ 90 DEG C; (2) after stirring, mixture being cooled, by filtering the red mud solid after obtaining pickling and filtrate, then red mud solid being washed; (3) in the red mud solid through washing in described (2), adding reductive agent, filtration after reduction reaction completes, obtaining described arsenic removal composite.This technique is with industrial red mud waste residue for raw material, and economical environment-protective, preparation technology is convenient and swift, is conducive to scale operation, and gained matrix material effect of removing arsenic is excellent.
Description
Technical field
The present invention relates to material engineering field, particularly a kind of technique utilizing industrial red mud waste residue to prepare arsenic removal composite.
Background technology
Arsenic and compound thereof are one of principal pollutant in trade effluent, the reveal any symptoms of arsenic acute poisoning for can have Metallic Flavour in Nausea and vomiting, mouth, abdomen severe pain, etc., comparatively severe one can produce dizziness, sural spasm, cyanosis so that shock, there is nervus centralis paralysis symptom in severe patient, limbs pain spasm, consciousness disappear.
The contaminative waste residue of discharging when red mud is Aluminium industry extraction aluminum oxide, average often produces 1 ton of aluminum oxide, incidentally produces 1.0 ~ 2.0 tons of red muds.China is as large alumina producing state of the world the 4th, and the red mud of annual discharge is up to millions of tons.A large amount of red muds can not fully effectively utilize, and large-area stockyard can only be relied on to stack, occupy a large amount of soil, also cause serious pollution to environment.The a large amount of red mud of safe storage has very large challenge.The red mud leakage accident of 10 people's death that causes of Hungary's generation in 2010 embodies the difficulty of safe handling red mud.It is existing that to utilize red mud to remove the technology of arsenic be adopt ferric oxide/silicon-dioxide in red mud as matrix material, its working mechanism mainly activates red mud surface and realizes adsorbing arsonium ion, this technology does not relate to the redox reaction of arsonium ion, and adsorption efficiency is not high.And face the risk of the desorption again of arsonium ion under condition of different pH.
The another kind of technology of removing arsenic is administered by nano zero valence iron particle, and this technology mainly improves the governance efficiency of arsenic by the redox reaction of arsonium ion and Zero-valent Iron.Metallic arsenic or the pentavalent arsenic of oxidation or reduction are deposited on iron particle, reduce the risk of arsenic desorption.But iron has ferromegnetism, when not having carrier, nano iron particles can be assembled, and reduces reaction specific surface area, thus reduces the governance efficiency of arsenic.In addition in the prior art, need to buy the starting material such as molysite, the preparation cost of nano iron particles is all higher, is unfavorable for its promotion and application in the middle of arsenic removal field.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the invention provides a kind of technique utilizing industrial red mud waste residue to prepare arsenic removal composite, this technique with industrial red mud waste residue for raw material, economical environment-protective, preparation technology is convenient and swift, be conducive to scale operation, gained matrix material effect of removing arsenic is excellent.
The technique utilizing red mud to prepare arsenic removal composite provided by the invention, is be raw material with red mud, comprises the steps:
(1), get red mud slurry, add hydrochloric acid dilute solution, stir after being warming up to 80 DEG C ~ 90 DEG C;
(2), stir after mixture is cooled, obtaining the red mud solid after pickling and filtrate by filtering, then again filtering after the washing of red mud solid;
(3), in the red mud solid through washing in described (2) adding reductive agent, filtration after reduction reaction completes, obtaining described arsenic removal composite.
Preferably, every 10g red mud slurry joins the hydrochloric acid that 55-65ml concentration is 1mol/L.
Preferably, described reductive agent is sodium borohydride.
Preferably, the solid that every 10g red mud slurry obtains after pickling is the sodium borohydride solution reduction of 1mol/L by 90-110ml concentration.
Preferably, the time of stirring in described step (1) is 30-40 minute.
Preferably, the arsenic removal composite that this technique also comprises obtaining in described step (3) is washed, and washing times is 2-4 time.
Preferably, the filtrate in described step (2) can be used for extracting metallic aluminium.
The technique utilizing red mud to prepare arsenic removal composite provided by the invention, has following beneficial effect:
(1), activation and the ferric oxide reduced in red mud obtain zero-valent iron particle, obtained nano zero valence iron particulate load is on the silicon-dioxide in red mud, under avoiding carrier free situation, nano iron particles is assembled, while the specific surface area keeping red mud and nano iron particles, by the redox reaction of nano zero valence iron particle in arsonium ion and silica supports to improve the governance efficiency of arsenic, make the utilization that each composition in red mud obtains comprehensively, coordinates.
(2), utilize industrial red mud waste residue for raw material, turn waste into wealth, reduce red mud and pollute, achieve many things at one stroke.
(3), be rich in the light metal alloy such as aluminium in the filtrate of red mud after pickling, therefrom can extract metallic aluminium, make spent pickle liquor obtain recycling, economic environmental protection.
(4) technique quickness and high efficiency, cost is low, is conducive to large-scale production, promotion and application.
Embodiment
In order to make those skilled in the art person understand technical scheme of the present invention better, below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
Pickling: take out 37% hydrochloric acid 10 milliliters, adds 110 ml distilled waters and is diluted to 3% solution (1 mol/L).Take out red mud slurry 10 grams, add the hydrochloric acid dilute solution of 60 milliliter 3%, adding distil water to 500 milliliter, be heated to 90 degree, fully stir after 30 minutes and be cooled to room temperature.By filtering to isolate red mud solid and filtrate.Isolated filtrate picks and places that to be cooled to room temperature in the container of 500 milliliters stand-by.Isolated red mud solid distillation washing three times, stand-by after filtering.
Reduction: take out sodium borohydride 3.8 grams, add 100 ml distilled waters and be diluted to 38 grams per liter solution (1 mol/L).In the isolated stand-by red mud solid of upper step, add the iron in the sodium borohydride solution reduction solid of 50 milliliter of 1 mol/L.Isolate solid and liquid after filtration, isolated solid distillation washing three times, namely obtains the arsenic removal composite 5g of nano-sized iron oxide particulate load on silicon-dioxide.
Test example 1. composition and particle form detect
In embodiment 1, SEM test display red mud particle is micron particles, and EDS analyzes and shows that red mud main component is iron, aluminium, silicon, sodium and titanium.After persalt washing, most of aluminium and sodium separate out red mud, and aluminium manufacturer can reclaim the output that these lyes increase aluminium, and concrete recovery and extracting method are conventionally known to one of skill in the art, repeat no more in the application.After pickling, the main component of red mud is iron, silicon and titanium.Zero-valent Iron prepared by the ferric oxide that sodium borohydride can reduce in red mud, obtains nano zero valence iron/silicon dioxide composite material.
The arsenic removal of test example 2. matrix material is tested
Get the clean centrifuge tube of 50 milliliters, 35ppm sodium metaarsenate solution prepared by metarsenic acid (NaAsO2) reference liquid adding 36 ml distilled waters and 9 milliliters.Label is that sample A0 is as standard.
The stand-by arsenic removal composite finally obtained in embodiment 1, adding 36 ml distilled waters obtains in red mud water mixture, add the mixture that 9 milliliters of sodium metaarsenate (NaAsO2) solution prepare 35ppm sodium metaarsenate solution and arsenic removal composite again, label is sample A1.Sample A0, A1 are put on gyrator and rock.
Sample A0 gets 3 milliliters, adds the nitric acid of 1 mol/L, surveys arsenious concentration as benchmark with ICP.
After 1 hour, sample A1 is centrifugal, gets 3 milliliters of supernatant liquors, adds the nitric acid of 11 mol/L, survey arsenious concentration with ICP.Sample A1, with hand even, is put back on gyrator.
After 2 hours, sample A1 is centrifugal, gets 3 milliliters of supernatant liquors, adds the nitric acid of 11 mol/L, survey arsenious concentration with ICP.Sample A1, with hand even, is put back on gyrator.
After 3 hours, sample A1 is centrifugal, gets 3 milliliters of supernatant liquors, adds the nitric acid of 11 mol/L, survey arsenious concentration with ICP.
ICP test result sees the following form 1.
Table 1.ICP test result
ICP test shows that the arsenic removal composite provided by the invention after reducing adsorbs the most of trivalent arsenic of also redox, and the arsonium ion more than 80% was adsorbed and redox by matrix material in 3 hours.
Above the technique utilizing red mud to prepare arsenic removal composite provided by the present invention is described in detail.Apply specific case herein to set forth principle of the present invention and embodiment, the explanation of above embodiment just understands core concept of the present invention for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, some improvement and modification can also be carried out to the present invention.These improve and modify and also should fall in the protection domain of the claims in the present invention.
Claims (6)
1. utilize red mud to prepare the technique of arsenic removal composite, it is characterized in that, be raw material with red mud, comprise the steps:
(1), get red mud slurry, add hydrochloric acid dilute solution, stir after being warming up to 80 DEG C ~ 90 DEG C;
(2), stir after mixture is cooled, obtaining the red mud solid after pickling and filtrate by filtering, then red mud solid being washed;
(3), in the red mud solid through washing in described (2) adding reductive agent, filtration after reduction reaction completes, obtaining described arsenic removal composite; Described reductive agent is sodium borohydride.
2. the technique utilizing red mud to prepare arsenic removal composite according to claim 1, is characterized in that, every 10g red mud slurry joins the hydrochloric acid that 55-65mL concentration is 1mol/L.
3. the technique utilizing red mud to prepare arsenic removal composite according to claim 1, is characterized in that, the solid that every 10g red mud slurry obtains after pickling, is the sodium borohydride solution reduction of 1mol/L by 90-110mL concentration.
4. the technique utilizing red mud to prepare arsenic removal composite according to claim 1, is characterized in that, the time of stirring in described step (1) is 30-40 minute.
5. the technique utilizing red mud to prepare arsenic removal composite according to claim 1, is characterized in that, the arsenic removal composite also comprised obtaining in described step (3) is washed, and washing times is 2-4 time.
6. the technique utilizing red mud to prepare arsenic removal composite according to claim 1, is characterized in that, the filtrate in described step (2) can be used for extracting metallic aluminium.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1981921A (en) * | 2005-12-14 | 2007-06-20 | 中国科学院生态环境研究中心 | High-activity mud adsorbent and its production |
| CN101176840A (en) * | 2006-11-09 | 2008-05-14 | 中国科学院生态环境研究中心 | Application method of iron modified red mud arsenic-removing adsorption agent |
| CN103464091A (en) * | 2013-10-08 | 2013-12-25 | 武汉科技大学 | Modified bentonite load nanometer iron material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1981921A (en) * | 2005-12-14 | 2007-06-20 | 中国科学院生态环境研究中心 | High-activity mud adsorbent and its production |
| CN101176840A (en) * | 2006-11-09 | 2008-05-14 | 中国科学院生态环境研究中心 | Application method of iron modified red mud arsenic-removing adsorption agent |
| CN103464091A (en) * | 2013-10-08 | 2013-12-25 | 武汉科技大学 | Modified bentonite load nanometer iron material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Arsenic removal from aqueous solution using ferrous based red mud sludge;Yiran Li等;《Journal of Hazardous Materials》;20091204;第177卷;131-137 * |
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Inventor after: Zheng Tongli Inventor after: Guo Xiaogang Inventor after: Hao Jinglin Inventor after: Zheng Tonghua Inventor before: Zheng Tonghua |
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Effective date of registration: 20200423 Address after: 073000 No.03, district yg-2, high standard industrial park, North (Dingzhou) renewable resources industrial base, Dingzhou City, Baoding City, Hebei Province Patentee after: Beihong kedingzhou New Material Technology Co.,Ltd. Address before: 100070 Beijing Fengtai District Branch Road No. 7 room 616 Patentee before: NORTH HUAYUAN (BEIJING) TECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20230620 Address after: 101300 West Yard of Grain Depot, Yanhe Village, Liqiao Town, Shunyi District, Beijing Patentee after: BEIJING AIWUERDE TECHNOLOGY DEVELOPMENT Co.,Ltd. Address before: No. 03, Zone YG-2, Gaobiao Industrial Park, North (Dingzhou) Renewable Resources Industrial Base, Dingzhou, Baoding, Hebei, 073000 Patentee before: Beihong kedingzhou New Material Technology Co.,Ltd. |