CN104998599B - Production method of Friedel's salt modified red mud used as heavy metalflocculant-adsorbent - Google Patents
Production method of Friedel's salt modified red mud used as heavy metalflocculant-adsorbent Download PDFInfo
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- CN104998599B CN104998599B CN201510380363.7A CN201510380363A CN104998599B CN 104998599 B CN104998599 B CN 104998599B CN 201510380363 A CN201510380363 A CN 201510380363A CN 104998599 B CN104998599 B CN 104998599B
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Abstract
The invention discloses a production method of Friedel's salt modified red mud used as a heavy metal flocculant-adsorbent, and the mass ratio between the solid state red mud which is grinded into fine powder and a Frieders salt emulsion which contains Calcium and Aluminum whose mol ratio is 4:1 is 1:(0.2-0.9), and the red mud and theFriedel's salt emulsion are placed in a reactor and are mixed with water,and are subjected to intense stirring and mixing for reaction in a condition with normal temperature, normal pressure, apH value higher than 10 and a watersolid ratio which is 1-4:1, a mixture is obtained after continuous stirring lasting for 0.5-1.5 hours.The mixture ispermitted to stand for curing for more than or equal to 20 hours, solidsand a clarified liquid are separated, the sodium-freeFriedel's salt modified red mud with micro-nanoneedle-like and layer-like structures wrapped each other is obtained, and the modified red mud can be used as the heavy metal flocculation-adsorbent. The invention has the advantages of energy conservation and consumption reduction, low equipment corrosion, simple process, low cost and 'zero three waste (waste gas, waste water and industrial residue)'discharge, etc. The product provided by the invention is used for restoration of soil which is polluted by heavy metal, and effective deep purification of electroplating waste water and metal recovery waste water.
Description
Technical field
The present invention relates to a kind of use Fred salts changed red mud belongs to as the production method of heavy metal flocculation-adsorbent
Red mud is utilized and water purification agent and heavy-metal contaminated soil renovation agent production technical field.
Background technology
Red mud is the solid slag discharged in aluminum oxide production process, is contaminative waste residue with strong basicity, because containing a large amount of
Iron oxide takes on a red color and is referred to as red mud.China up to counts as big alumina producing state of the world the 4th, the red mud of annual discharge
Million tons.Due to the difference of the grade of ore, production method and technical merit, often produce one ton of aluminum oxide and will be about discharging 0.3-
2.5t red muds, with successively decreasing year by year for bauxite grade, produce the red mud discharge capacity of ton aluminum oxide also cumulative year after year.
The chemical composition of red mud is as shown in Table 1 below：
The chemical composition (wt%) of Pingguo Aluminium Industry Co., Guangxi's red mud of table 1
Fe2O3 Al2O3 CaO SiO2 TiO2 Na2O A/S N/S
42.10 16.11 14.80 8.61 8.06 3.53 1.87 0.41 2010 annual datas
35.6 17.3 14.14 10.8 3.0 5.70 1.60 0.53 2014 annual datas
According to incompletely statistics, only 2010 China's aluminum oxide yield has just reached 28,960,000 tons, common property life red mud
3537.4 ten thousand tons, i.e., often produce 1 ton of aluminum oxide and just produce more than 1.2 tons of red mud, wherein red mud from sintering process accounts for 18.1%, Bayer
Method red mud accounts for 81.9%.Compared with red mud from sintering process, the utilization difficulty of Bayer process red mud is bigger, and this is due to being given birth to using Bayer process
In producing alumina process, the key component of Bayer process red mud is alkali and oxidation in hydrated sodium aluminosilicate, therefore Bayer process red mud
Aluminium content is generally higher than red mud from sintering process, and higher alkali content increased the difficulty that it is applied in large industry in Bayer process red mud
Degree.At present, China's red mud comprehensive utilization ratio only 4%, accumulation volume of cargo in storage has reached several hundred million tons.Will more than the enterprise of domestic production aluminum oxide
Store up after red mud drying dehydration, not only occupy a large amount of soils, also create alkaline matter to subsurface wastewater infiltration system, cause body of groundwater
And soil pollution；The dust that exposed red mud is formed flies away with the wind, also can atmosphere pollution, the mankind and vegeto-animal existence are caused to bear
Face rings, and deteriorates ecological environment.Therefore, a large amount of red muds of aluminum oxide production process discharge how are processed, reducing environmental pollution is
Alumina industry urgent need to solve the problem.
Traditional Application way is to leach active ingredient aluminium, the iron in red mud under the conditions of high-temperature pressurizing with strong acid, but this
A little methods all have that high energy consumption, resource utilization be low, high cost.
Red mud contains the oxide of abundant iron, aluminium and calcium, and they are applied in water process as adsorbent and flocculant
Heavy metal ion, inorganic anion, organic dyestuff and the organic pollution that can effectively go in eliminating water etc..But directly using former
Shape red mud as adsorbent, its limited sorption capacity, people's preprocess method such as mainly take acid activation, heat treatment, iron modified
To improve its adsorption capacity, how to find cheap and efficient method of modifying is the important research side for advancing red mud application
To.
It is the focus and forward position neck for being modified research to red mud both at home and abroad at present using metal inorganic salt as activator
Domain, mainly by physics and chemical mode, changes the space structure of red mud and the composition and content of chemical composition.Such as China
Patent No. ZL200410067225.5, ZL200410073453.3 and ZL201110275030.X disclosed in patent document
Technical scheme in, in the first two patent document（The patent No.：ZL200410067225.5、ZL200410073453.3）Skill
In art scheme, red mud is mixed with alkaline earth oxide or hydroxide carries out roasting, forms bimetallic oxide, Ran Hougen
Hydrotalcite is generated according to " memory effect " with bimetallic oxide reaction with carbonate.And in latter patent document（Patent
Number：ZL201110275030.X）Then it is at a warm condition calcification to be carried out to red mud with white lime in disclosed process
Transition removing soda, is then passed through under an increased pressure CO2Reaction is separated with iron mineral and is separately recovered aluminium therein and iron.This is several
The technical scheme of individual patent is primarily present the not congruent subject matter of long flow path, high energy consumption, the utilization of resources；And in prior art its
His disclosed red mud is modified and reports the change for being simply related to its surface characteristic, it is difficult to meet the requirement of practical application.Therefore, it is existing
Have disclosed using red mud as material modification production waste cleanser or all not ideal enough as the method for soil-repairing agent, it is impossible to full
The needs that foot is used.
The content of the invention
The purpose of the present invention is：A kind of simple manufacture craft, low production cost are provided, industrial residue can be made full use of red
Life of the use Fred salts changed red mud of various active ingredients and strong operability in mud as heavy metal flocculation-adsorbent
Product method, to overcome the deficiencies in the prior art.
The technical scheme is that what is be achieved in that：
The present invention a kind of use Fred salts changed red mud be as the production method of heavy metal flocculation-adsorbent：With mill
Into the solid-state red mud of fine powder and containing Ca:Al mol ratios are 4:1 Fred salts emulsion is 1 in mass ratio:（0.2~amount 0.9)
It is placed in reactor and adds water to mix, is 1~4 in normal temperature and pressure and pH ＞ 10, water-solid ratio:Under conditions of 1, strong mixing is carried out
Hybrid reaction, obtains compound after persistently stirring 0.5~1.5 hour, compound is stood after displaying curing not less than 20 hours, will
Solid phase is separated with clarified solution, you can the removing sodium Fred salts changed red mud that the needle-like and stratiform for obtaining micro-nano structure is mutually wrapped up,
The changed red mud can be used as heavy metal flocculation-adsorbent and use.
Above-mentioned added Fred salts emulsion is both the effective flocculation-adsorption component in changed red mud and as red
The lytic agent of key component hydrated sodium aluminosilicate and discharge calcium oxide reaction of participating and generate calcium aluminosilicate hydrate phase and life in mud
Into Ca:Al mol ratios are 4:1-2:1 Fred salts phase.
Above-mentioned Fred salts emulsion used is using the Patent No. disclosed in Chinese patent literature
ZL200110048919.9, a kind of Fred salts emulsion of the method synthesis of entitled " method for producing Fred salts ".
Ca in above-mentioned Fred salts emulsion:Al mol ratios are less than 4:When 1, calcium oxide or calcium chloride are mended as auxiliary material
It is charged in Fred salts emulsion and obtains Fred salts mixed emulsion, and makes the Ca in the Fred salts mixed emulsion:Al mol ratios reach
To 4:After 1, you can use the Fred salts mixed emulsion as the Fred salts emulsion.
The key component of above-mentioned aluminium contained in gained changed red mud is calcium aluminosilicate hydrate by hydrated sodium aluminosilicate phase in version
Phase and Ca:Al mol ratios are 4:1-2:1 Fred salts phase.
Above-mentioned red mud mixes for the Bayer process red mud in Industry Waste red mud, red mud from sintering process or Bayer process with sintering process
Red mud.
As a result of above-mentioned technical proposal, applicable industry of the present invention give up red mud as a raw material, with Chinese patent
Fred salts synthesized by method disclosed in ZL200110048919.9 are used as modifying agent；The production technology of the present invention is in normal temperature
Carry out under normal pressure, process is simple；Reaction time is short, and unit-hour output is high.Whole products can be employed as sewage or polluted soil
Heavy metal flocculation-adsorbent；Technical process is discharged without " three wastes ", belongs to process for cleanly preparing.This aspect is reduced and produced into
This, has on the other hand greatly widened the application market of removing sodium Fred salts changed red mud.
The present inventor carries out in-depth study discovery by the structure to Fred salts and synthetic method：Meeting
Calcium aluminosilicate hydrate phase and Fred salts are mutually produced under the pH value precondition of precipitation, Gu even solid-liquid, solid-liquid-reaction system
In calcium ion also can react with aluminium ion, produce Al-Ca complex ion [Ca2Al(OH)6]+, thus constitute calcium aluminosilicate hydrate and not
Randt's salt cenotype is precipitated, Gu and the original solid phase, the high Ca that promote in solid-liquid, solid-liquid-reaction system:The Fred of Al mol ratios
Salt phase and hydrated sodium aluminosilicate phased soln, so as to difference Ca is obtained:The Fred salts of Al mol ratios.
The study find that, red mud is modified with the Fred salts with supramolecular structure so as in aluminum-containing mineral
Phase structure is thoroughly changed (confirmed by XRD and infrared spectrum detection), forms the micro-nano structure that needle-like is mutually wrapped up with stratiform（See
Electromicroscopic photograph）；The contents of many kinds of heavy metal ion in electroplating wastewater is removed as flocculation-adsorbent with Fred salts changed red mud, it is complete
GB is reached entirely（GB 21900-2008）The heavy metals emission standard of plating pollutant.Red mud is modified with Fred salts,
Domestic and foreign literature is showed no open report.Therefore, red mud is modified using Fred salts, has opened up a class changed red mud new
Product, utilizes, raising red mud has in wastewater treatment and its as the application of soil-repairing agent to solving red mud changing waste into resources
Significance.
The present invention has been carried out innovating and improved to existing red mud modification technology.It is of the invention compared with existing public technology
Innovation and be improved by it is following some：
1. solid-state Fred salts are reacted with solid-state red mud in aqueous slurry, formed hydroxyl mayenite intermediate, then this
A little intermediates again with system in anionic silicate and chlorion react and to form calcium aluminosilicate hydrate cenotype and Fred salts cenotype
Precipitation, simplifies synthesis technique.High Ca:Al mol ratio Fred salts emulsions be both effective flocculation-adsorption component in changed red mud,
It is again as the lytic agent of key component hydrated sodium aluminosilicate in red mud and discharges calcium oxide reaction of participating and generate relatively low Ca:
The Fred salts phase of Al mol ratios.
2. the key component of Bayer process red mud is that alkali and aluminum oxide in hydrated sodium aluminosilicate, therefore Bayer process red mud contains
Amount is generally higher than red mud from sintering process, but Bayer process red mud accounts for absolute majority in existing stacking red mud again, and it is red that this law processes Bayer process
Mud can be greatly lowered the soda content in changed red mud, thus widen product by heavy-metal contaminated soil reparation industry
Application.
3. compared with intensification pressuring method of the prior art, the operating condition of normal temperature and pressure of the present invention and alkaline environment,
Energy consumption, equipment corrosion etc. are all low than acid system；The present invention can effectively improve unit-hour output and the rate of recovery, lower production cost.
Removing sodium Fred salts changed red mud product obtained by present invention production can be directly used for industrial wastewater, town sewage
Heavy metals removal process.
Table 2 below and table 3 are respectively to carry out electroplating wastewater, hydrometallurgy waste water weight using product of the present invention dynamic flocculence
The using effect data of metal removal.
Table 2：Deep purifying (mg L of the Fred salts changed red mud to Nanning City's waste water from plating plant heavy metal-1)
Note：Fred salts changed red mud addition 0.2g L-1；Project Unit with underscore is μ g L-1
Table 3：Removal effect (μ g L of the Fred salts changed red mud to Hengyang metal recovery factory heavy metals-1)
| 28. Index | 29. Total Cr | 30.Cd | 31. Pb | 32. Hg | 33. Ni | 34.Cu | 35.Zn | 36.Mn |
| 37. Raw water | 38. 1.93 | 39. 79.5 | 40. 90.75 | 41. 20.12 | 42. 1378 | 43. 7.34 | 44. 463 | 45. 1.72 |
| 46. After changed red mud flocculation-absorption | 47. 2.03 | 48. 0.51 | 49. 2.85 | 50. ＜ 0.0 | 51. ＜ 0.0 | 52. 0.03 | 53. 0.865 | 54. 0.003 |
Note：Fred salts changed red mud addition 0.2g L-1；Project Unit with underscore is mg L-1
Knowable to data above, depth effectively can be carried out to electroplating wastewater using the Fred salts changed red mud of the present invention net
Change, be fully achieved GB（GB 21900-2008）The heavy metals emission standard of plating pollutant；And can be used as heavy metal recovery product
A kind of efficient, inexpensive flocculation-adsorbent of industry waste water.
Description of the drawings
Fig. 1 isThe present invention is rightThe X-ray diffracting spectrum contrast that Pingguo red mud is modified forward and backward；
Fig. 2 is the infrared spectrum contrast that the present invention is modified forward and backward to Pingguo red mud；
Fig. 3 is Pingguo red mud scanning electron microscope image before modified；
Effect drop Fig. 4 is the modified scanning electron microscope image of Pingguo red mud.
Specific embodiment
Below, in conjunction with the embodiments the present invention is described in further detail.
Embodiments of the invention：A kind of use Fred salts changed red mud of the present invention is used as heavy metal flocculation-adsorbent
Production method is：With finely disintegrated solid-state red mud and containing Ca:Al mol ratios are 4:1 Fred salts emulsion is 1 in mass ratio:
（0.2~amount 0.9) is placed in reactor and adds water to mix, and is 1~4 in normal temperature and pressure and pH ＞ 10, water-solid ratio:1 bar
Under part, strong mixing hybrid reaction is carried out, compound is obtained after persistently stirring 0.5~1.5 hour, compound is stood and displays curing not
After less than 20 hours, solid phase is separated with clarified solution, you can the removing sodium that the needle-like and stratiform for obtaining micro-nano structure is mutually wrapped up is not
Randt's salt changed red mud, the changed red mud can be used as heavy metal flocculation-adsorbent and use.
The Fred salts emulsion for being added is both the effective flocculation-adsorption component in changed red mud and as in red mud
The lytic agent of key component hydrated sodium aluminosilicate and discharge calcium oxide participate reaction generate calcium aluminosilicate hydrate phase and generate Ca:
Al mol ratios are 4:1-2:1 Fred salts phase；Fred salts emulsion used is using the patent disclosed in Chinese patent literature
Number for ZL200110048919.9, entitled " a kind of method for producing Fred salts " method synthesis Fred salts breast
Liquid；Ca in Fred salts emulsion used:Al mol ratios are less than 4:When 1, calcium oxide or calcium chloride are added to as auxiliary material
Fred salts mixed emulsion is obtained in Fred salts emulsion, and makes the Ca in the Fred salts mixed emulsion:Al mol ratios reach 4:1
Afterwards, you can use the Fred salts mixed emulsion as the Fred salts emulsion；The master of contained aluminium in gained changed red mud
Component is wanted to be calcium aluminosilicate hydrate phase and Ca by hydrated sodium aluminosilicate phase in version:Al mol ratios are 4:1-2:1 Fred salts phase；Institute
It is that Bayer process red mud in prior art in Industry Waste red mud, red mud from sintering process or Bayer process mix with sintering process with red mud
Red mud.
The several examples using the present invention are presented herein below：
Example 1：With containing Fe2O3、Al2O3、CaO、SiO2Content is respectively the Guangxi of 35.6 %, 17.3%, 14.14%, 10.8%
The mass parts of Pingguo Aluminium Industry Corp dam red mud 1000 are placed in enamel glass reactor, are disposably added under the conditions of normal agitation
The Fred salts of 200-450 mass parts are reacted, and continue to stir~1 hour and after curing 24 hours, you can be obtained containing aluminium
Key component is calcium aluminosilicate hydrate phase and Ca by hydrated sodium aluminosilicate phase in version:Al mol ratios are 4:1-2:1 Fred salts phase
Changed red mud.
Example 2：With containing Fe2O3、Al2O3、CaO、SiO2Content be respectively 8.35%, 24.38%, 16.95%, 19.95% it is expensive
The mass parts of 2 ﹟ dam mixing red mud of state Chinalco 1000 are placed in enamel glass reactor, disposable under the conditions of normal agitation
The Fred salts for adding 400-850 mass parts are reacted, and continue to stir~1 hour and after curing 24 hours, you can be obtained and contain
The key component of aluminium is calcium aluminosilicate hydrate phase and Ca by hydrated sodium aluminosilicate phase in version:Al mol ratios are 4:1-2:1 Fred
Salt phase changed red mud.
Claims (5)
1. a kind of use Fred salts changed red mud is characterized in that as the production method of heavy metal flocculation-adsorbent：It is thin with wearing into
The solid-state red mud of powder with contain Ca:Al mol ratios are 4:1 Fred salts emulsion is 1 in mass ratio:（0.2~amount 0.9) is placed in
In reactor and add water to mix, be 1~4 in normal temperature and pressure and pH ＞ 10, water-solid ratio:Under conditions of 1, strong mixing mixing is carried out
Reaction, obtains compound after persistently stirring 0.5~1.5 hour, compound is stood after displaying curing not less than 20 hours, by solid phase
Separate with clarified solution, you can the removing sodium Fred salts changed red mud that the needle-like and stratiform for obtaining micro-nano structure is mutually wrapped up, this changes
Property red mud can be used as heavy metal flocculation-adsorbent and use.
2. use Fred salts changed red mud according to claim 1 as heavy metal flocculation-adsorbent production method, its
It is characterized in that：The Fred salts emulsion for being added is both the effective flocculation-adsorption component in changed red mud and as main in red mud
Want the lytic agent of component hydrated sodium aluminosilicate and discharge calcium oxide and participate to react generation calcium aluminosilicate hydrate phase and generation Ca:Al
Mol ratio is 4:1-2:1 Fred salts phase.
3. use Fred salts changed red mud according to claim 1 as heavy metal flocculation-adsorbent production method, its
It is characterized in that：Ca in Fred salts emulsion:Al mol ratios are less than 4:When 1, calcium oxide or calcium chloride are added to as auxiliary material
Fred salts mixed emulsion is obtained in Fred salts emulsion, and makes the Ca in the Fred salts mixed emulsion:Al mol ratios reach 4:1
Afterwards, you can use the Fred salts mixed emulsion as the Fred salts emulsion.
4. use Fred salts changed red mud according to claim 1 as heavy metal flocculation-adsorbent production method, its
It is characterized in that：In gained changed red mud the key component of contained aluminium by hydrated sodium aluminosilicate phase in version be calcium aluminosilicate hydrate phase and
Ca:Al mol ratios are 4:1-2:1 Fred salts phase.
5. use Fred salts changed red mud according to claim 1 as heavy metal flocculation-adsorbent production method, its
It is characterized in that：The red mud be Bayer process red mud in Industry Waste red mud, red mud from sintering process or Bayer process mix with sintering process it is red
Mud.
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| US10766812B2 (en) * | 2016-03-15 | 2020-09-08 | Fluorchemie Gmbh Frankfurt | Composition containing modified chromate-deficient red mud and method for producing same |
| CN110668480B (en) * | 2019-11-07 | 2021-06-25 | 南通海星电子股份有限公司 | Method for producing Fred salt by using aluminum-containing waste hydrochloric acid and aluminum-containing sludge in electrode foil industry |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644508A (en) * | 2004-12-16 | 2005-07-27 | 浙江大学 | Production of acqueous talc from brine |
| CN102294351A (en) * | 2011-05-27 | 2011-12-28 | 章兴华 | Method for taking Fred salt as heavy metal cadmium-polluted soil remediation agent |
| CN102603027A (en) * | 2012-03-27 | 2012-07-25 | 湖南农业大学 | Method for treating manganese-containing waste water by utilizing modified red mud |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6115735A (en) * | 1984-06-29 | 1986-01-23 | Mitsui Alum Kogyo Kk | Preparation of red mud granular adsorbent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644508A (en) * | 2004-12-16 | 2005-07-27 | 浙江大学 | Production of acqueous talc from brine |
| CN102294351A (en) * | 2011-05-27 | 2011-12-28 | 章兴华 | Method for taking Fred salt as heavy metal cadmium-polluted soil remediation agent |
| CN102603027A (en) * | 2012-03-27 | 2012-07-25 | 湖南农业大学 | Method for treating manganese-containing waste water by utilizing modified red mud |
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