CN103272563B - A kind of preparation method of aluminum hydroxide film - Google Patents
A kind of preparation method of aluminum hydroxide film Download PDFInfo
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Abstract
The invention discloses a kind of based on sodium aluminate and for the preparation and application of the aluminum hydroxide film of adsorbing Cr (VI): first, dense HCl is added in sodium aluminate solution, form stable aluminum hydroxide sol particle precipitation, and be hydrolyzed certain hour at a certain temperature; Subsequently, add peptizing agent peptization, make sol particles dispersed, add coalescents polyvinyl alcohol (PVA) further, form stable gel through ageing certain hour, film obtains aluminum hydroxide film.This method has the advantages such as cheaper starting materials, mild condition and technique are simple, prepared aluminum hydroxide film has good absorption property to the hypertoxic pollutant Cr (VI) in water body, especially has obvious advantage in adsorbent separation and regeneration cycle use.
Description
Technical field
The present invention relates to the technical field of the Synthesis and applications of fine chemicals aluminium oxide, is exactly a kind of preparation method for the aluminum hydroxide film of hypertoxic pollutant heavy metal Cr (VI) and application thereof.
Background technology
Along with the fast development of economy, heavy-metal pollution has become the focus of people's growing interest, and chromium, cadmium and mercury etc. are common heavy metal contaminants.For chromium, it pollutes and is mainly derived from the industrial wastewater of mining, chemical industry, plating, printing and dyeing, leather etc. and percolate etc.By the impact of the conditions such as Organic substance in water, redox materials, temperature and hardness, the valence state that chromium exists in water environment is Cr (III) and Cr (VI) mainly, wherein maximum with the toxicity of Cr (VI), it is general with Cr in water environment
2o
4 2-, Cr
2o
7 2-and HCrO
4 -three kinds of anionic forms exist, and have strong impulse and corrosivity.Cr (VI) is easily absorbed by the body and at body body accumulation, people knows from experience because its too high levels is carcinogenic, teratogenesis, mutagenesis.In addition, the Cr (VI) in water can not directly be decomposed, and can produce very large negative effect equally after being discharged into water body to environment, publilc health and development.Therefore, the process containing Cr (VI) waste water is of great practical significance.
The processing method of Cr (VI) waste water is a lot, mainly comprise oxidation precipitation, ion-exchange, microorganism, counter-infiltration and absorption method etc., wherein absorption method has that processing cost is low, removal effect good, the advantage such as selective height and highly versatile, receives and pays close attention to widely.The people such as Mor [MorS, RavindraK, BishnoiNR.Adsorptionofchromiumfromaqueoussolutionbyactiv atedaluminaandactivatedcharcoal.BioresourceTechnology, 2007,98 (4), 954-957.] have studied the absorption property of activated alumina to Cr (VI), research finds that its absorption property is at room temperature best, but saturation capacity is only 7.4mg/g.CN101348297A discloses a kind of processing method of effluent containing heavy metal ions, utilize the heavy metal ion in the magnetic particle absorption waste water containing tri-iron tetroxide, adsorbance can reach 36mg/g, utilize oxidation reaction to be separated the chromium ion of micro-property magnetic grain and absorption subsequently, but there is the shortcomings such as complex disposal process.In addition, the patent reported is separated more difficult with the adsorbent Cr (VI) mentioned in document afterwards, about the research of its circulation absorption performance also rarely has report.
The good characteristics such as inoranic membrane has that good heat resistance, chemistry are high with mechanical stability, is easily separated after adsorption fouling thing, have started in many fields such as the Large area electronics such as FPD, separation and membrane catalytic reactions to apply.CN102787309A discloses a kind of preparation method relating to the aluminum oxide film of field of thin film transistors, by precursor solution coating film forming on coated face, obtains aluminum oxide film through heat treatment process; And with it for gate dielectric layer prepares ZTO semiconductor layer, prepare source, drain electrode thereon, obtain thin film transistor (TFT) through encapsulation.The people such as Soma [SomaC, RumeauM, SergentC.Useofmineralmembrancesinthetreatmentoftextileef fluents.Proc.1
stinternationalConferenceofInorganicMembrances.Montpellier, France, 1989,523-526.] utilize the pellumina treatment of dyeing and printing of 0.2 μm, its clearance is more than 98%; The people such as Cumming [CummingIW, TurnerAD.OptimitionofanUFpilotplantforthetreatmentofradi oactivewaste.Proc.FutureInd.ProspectsMembersProc.Conf.Br ussels, Belgium, 1988,163.] employing aperture is the waste water of the zirconium oxide film of 2nm and the pellumina process low-activity of 0.2 μm, clearance is 5 times of common iron flucculation process, realizes industrialization.To sum up, the inoranic membranes such as pellumina are existing application in the field such as dyeing waste water and radioactive wastewater, but also rarely has report in the application in the heavy metal adsorption fields such as Cr (VI).
To sum up, develop a kind of cheaper starting materials, preparation condition gentle, to hypertoxic pollutant Cr (VI), there is excellent absorption property, be easily separated, reclaim and important scientific meaning and good application prospect can be had by the inoranic membrane that uses of circular regeneration.
Summary of the invention
Technical problem to be solved by this invention is: provide that a kind of cheaper starting materials, wide material sources, preparation method are easy, to be easily separated after mild condition, absorption Cr (VI) pollutant and can the preparation and application of aluminum hydroxide film that uses of circular regeneration, prepared product has excellent absorption property to the hypertoxic pollutant Cr (VI) in water body.
The present invention solves its technical problem and adopts following technical scheme:
The preparation method of aluminum hydroxide film provided by the invention, it comprises the following steps:
(1) first sodium aluminate is dissolved in distilled water, obtains the sodium aluminate solution that concentration is 40-200g/L, add hydrochloric acid subsequently, under agitation form the suspension of aluminum hydroxide sol particle precipitation, then this suspension is transferred in water-bath the reaction that is hydrolyzed;
(2) gained hydrolysis product is cooled, add the aqueous solution of peptizing agent and film forming agent polyvinyl alcohol (PVA), after stirring, obtain colloidal sol;
(3) by film, the drying after ageing 12-72h at 80-90 DEG C of gained colloidal sol, described aluminum hydroxide film is obtained.
The pH of described aluminum hydroxide sol particle precipitation suspension can be 4-8.
The technological parameter of described hydrolysis can be: reaction temperature is 60-90 DEG C, and the reaction time is 6-12h.
Described peptizing agent can be any one in hydrochloric acid, acetic acid and nitric acid, and its addition is: (H
+): n (Al
3+)=0.07-0.25.
The present invention can adopt PVA to assist film forming, and the addition of PVA is: m
pVA: m
al2O3=0-0.8.
Aluminum hydroxide film prepared by the inventive method is for adsorbing Cr (VI) solution that pH is 2-6.
The present invention can by the aluminum hydroxide film sodium carbonate desorption after absorption Cr (VI), and the aluminum hydroxide film after desorption recycles.
The fundamental reaction principle of foundation of the present invention is: sodium aluminate solution is after concentrated hydrochloric acid adjust ph, form stable aluminum hydroxide precipitation, form stable aluminum hydroxide sol particle after being hydrolyzed certain hour at a certain temperature, after adding peptizing agent, mutually repel between particle and form stable colloidal sol; Make the dispersion of micelle reach balance as early as possible with gathering through aging again, form single domain size distribution; Subsequently, add the viscosity that appropriate PVA regulates colloidal sol, make whole gel network have the structure of bridge joint between organic/inorganic, enhance the elasticity of network, suppress film cracking, formed and there is certain flexible inoranic membrane.In acid condition, during isoelectric point lower than nano aluminium oxide, nano alumina surface is positively charged because absorption H+ ion for this film, the metallate ion existed with anionic form under thus can adsorbing low pH.
The present invention, compared with the technology of preparing of existing porous C r (VI) adsorbent, has following major advantage:
1) cheaper starting materials and convenient sources, sodium aluminate is the intermediate product that Bayer process prepares in metallurgical-grade aluminum oxide process, comparatively metal alkoxide and other inorganic aluminates cheap.
2) the simple and mild condition of technique, adopt sol-gel process, drying film forming, do not relate to roasting process, thus energy consumption significantly reduces.
3) aluminum hydroxide film prepared by has excellent absorption property to Cr (VI), and not only adsorbance is large, the rate of adsorption fast, the more important thing is and can regeneration cycle use.
Accompanying drawing explanation
Fig. 1-Fig. 7 is respectively the SEM picture of aluminum hydroxide film prepared by embodiment 1-7;
Fig. 8 prepared by embodiment 1-7 aluminum hydroxide film at room temperature to the curve of adsorption kinetics of Cr (VI);
Fig. 9 certain boehmite that aluminum hydroxide film and Shandong Aluminum Plant produce prepared by embodiment 4 at room temperature uses the comparison of adsorbance to continuous four regeneration cycle of Cr (VI).
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, and these embodiments are only the descriptions to the better implementation method of the present invention, but are not limited to described content below.
Embodiment 1:
Taking 1g sodium aluminate is dissolved in 40ml distilled water, stirs the sodium aluminate solution forming 40g/L, add appropriate dense HCl and regulate its pH value to be 4, then transfer them in water-bath, under the water bath condition of 60 ° of C, react 12h under moderate strength.Product, through being cooled to room temperature, adding a certain amount of acetic acid and carries out peptization, n (H
+): n (Al
3+)=0.25, after peptization certain hour, does not add PVA, i.e. m
pVA: m
al2O3=0, after stirring certain hour, carry out centrifugation, by product ageing 72h at 80 DEG C, on the slide after film to ultrasonic cleaning, obtain product after drying, Fig. 1 is shown in by its SEM picture.
The potassium bichromate solution of preparation 100ml, 100mg/L, the HCl solution of the pH 1mol/L of solution is adjusted to 2, add the above-mentioned sample of 400mg subsequently, after at room temperature stirring 4h, sampling is separated and analyzes filtrate composition with ultraviolet-visible spectrophotometer, curve of adsorption kinetics is shown in that the adsorbance of Fig. 8 embodiment 1, Cr (VI) is 4.7mg/g.
Embodiment 2:
Taking 4g sodium aluminate is dissolved in 40ml distilled water, and under moderate strength, stir the sodium aluminate solution forming 100g/L, adding appropriate dense HCl adjust ph is 6, then transfers them in water-bath, under the water bath condition of 85 ° of C, react 8h.Product, through being cooled to room temperature, adding a certain amount of concentrated hydrochloric acid and carries out peptization, n (H
+): n (Al
3+)=0.2, after peptization certain hour, adds a certain amount of PVA, and its addition is m
pVA: m
al2O3=0.1, after stirring certain hour, centrifugation, ageing 12h at 90 DEG C, on the slide after film to ultrasonic cleaning, drying and film forming, Fig. 2 is shown in by its SEM picture.
The potassium bichromate solution of preparation 100ml, 100mg/L, the HCl solution of the pH 1mol/L of solution is adjusted to 3, add the above-mentioned sample of 400mg subsequently, after at room temperature stirring 4h, sampling is separated and analyzes filtrate composition with ultraviolet-visible spectrophotometer, curve of adsorption kinetics is shown in that the adsorbance of Fig. 8 embodiment 2, Cr (VI) is 12.6mg/g.
Embodiment 3:
Taking 4g sodium aluminate is dissolved in 40ml distilled water, and under moderate strength, stir the sodium aluminate solution forming 100g/L, adding appropriate dense HCl adjust ph is 6, then transfers them in water-bath, under the water bath condition of 85 ° of C, react 8h.Product, through being cooled to room temperature, adding a certain amount of concentrated hydrochloric acid and carries out peptization, n (H
+): n (Al
3+)=0.2, after peptization certain hour, adds a certain amount of PVA, and its addition is m
pVA: m
al2O3=0.3, after stirring certain hour, centrifugation, ageing 48h at 85 DEG C, on the slide after film to ultrasonic cleaning, drying and film forming, Fig. 3 is shown in by its SEM picture.
The potassium bichromate solution of preparation 100ml, 100mg/L, the HCl solution of the pH 1mol/L of solution is adjusted to 3, add the above-mentioned sample of 400mg subsequently, after at room temperature stirring 4h, sampling is separated and analyzes filtrate composition with ultraviolet-visible spectrophotometer, curve of adsorption kinetics is shown in that the adsorbance of Fig. 8 embodiment 3, Cr (VI) is 15.2mg/g.
Embodiment 4:
Taking 4g sodium aluminate is dissolved in 40mL distilled water, and under moderate strength, stir the sodium aluminate solution forming 100g/L, adding appropriate dense HCl adjust ph is 6, then transfers them in water-bath, under the water bath condition of 80 ° of C, react 10h.Product, through being cooled to room temperature, adding a certain amount of concentrated hydrochloric acid and carries out peptization, n (H
+): n (Al
3+)=0.2, after peptization certain hour, adds a certain amount of PVA, and its addition is m
pVA: m
al2O3=0.5, after stirring certain hour, centrifugation, ageing 24h at 90 DEG C, on the slide after film to ultrasonic cleaning, drying and film forming, Fig. 4 is shown in by its SEM picture.
The potassium bichromate solution of preparation 100ml, 100mg/L, the HCl solution of the pH 1mol/L of solution is adjusted to 4, add the above-mentioned sample of 400mg subsequently, after at room temperature stirring 4h, sampling is separated and analyzes filtrate composition with ultraviolet-visible spectrophotometer, curve of adsorption kinetics is shown in that the adsorbance of Fig. 8 embodiment 4, Cr (VI) is 26.9mg/g.
Embodiment 5:
Taking 4g sodium aluminate is dissolved in 40ml distilled water, and under moderate strength, stir the sodium aluminate solution forming 100g/L, adding appropriate dense HCl adjust ph is 6, then transfers them in water-bath, under the water bath condition of 85 ° of C, react 8h.Product, through being cooled to room temperature, adding a certain amount of concentrated hydrochloric acid and carries out peptization, n (H
+): n (Al
3+)=0.2, after peptization certain hour, adds a certain amount of PVA, and its addition is m
pVA: m
al2O3=0.8, after stirring certain hour, centrifugation, ageing 48h at 85 DEG C, on the slide after film to ultrasonic cleaning, drying and film forming, Fig. 5 is shown in by its SEM picture.
The potassium bichromate solution of preparation 100ml, 100mg/L, the HCl solution of the pH 1mol/L of solution is adjusted to 3, add the above-mentioned sample of 400mg subsequently, after at room temperature stirring 4h, sampling is separated and analyzes filtrate composition with ultraviolet-visible spectrophotometer, curve of adsorption kinetics is shown in that the adsorbance of Fig. 8 embodiment 5, Cr (VI) is 15.6mg/g.
Embodiment 6:
Taking 6g sodium aluminate is dissolved in 40ml distilled water, and under moderate strength, stir the sodium aluminate solution forming 150g/L, adding appropriate dense HCl adjust ph is 6, then transfers them in water-bath, under the water bath condition of 85 ° of C, react 8h.Product, through being cooled to room temperature, adding a certain amount of red fuming nitric acid (RFNA) and carries out peptization, n (H
+): n (Al
3+)=0.15, after peptization certain hour, adds a certain amount of PVA, and its addition is m
pVA: m
al2O3=0.5, after stirring certain hour, centrifugation, ageing 48h at 85 DEG C, on the slide after film to ultrasonic cleaning, drying and film forming, Fig. 6 is shown in by its SEM picture.
The potassium bichromate solution of preparation 100ml, 100mg/L, the HCl solution of the pH 1mol/L of solution is adjusted to 6, add the above-mentioned sample of 400mg subsequently, after at room temperature stirring 4h, sampling is separated and analyzes filtrate composition with ultraviolet-visible spectrophotometer, curve of adsorption kinetics is shown in that the adsorbance of Fig. 8 embodiment 6, Cr (VI) is 21.2mg/g.
Embodiment 7:
Taking 8g sodium aluminate is dissolved in 40ml distilled water, and under moderate strength, stir the sodium aluminate solution forming 200g/L, adding appropriate dense HCl adjust ph is 8, then transfers them in water-bath, under the water bath condition of 90 ° of C, react 6h.Product, through being cooled to room temperature, adding a certain amount of red fuming nitric acid (RFNA) and carries out peptization, n (H
+): n (Al
3+)=0.07, after peptization certain hour, adds a certain amount of PVA, and its addition is m
pVA: m
al2O3=0.5, after stirring certain hour, centrifugation, ageing 12h at 90 DEG C, on the slide after film to ultrasonic cleaning, drying and film forming, Fig. 7 is shown in by its SEM picture.
The potassium bichromate solution of preparation 100ml, 100mg/L, the HCl solution of the pH 1mol/L of solution is adjusted to 2, add the above-mentioned sample of 400mg subsequently, after at room temperature stirring 4h, sampling is separated and analyzes filtrate composition with ultraviolet-visible spectrophotometer, curve of adsorption kinetics is shown in that the adsorbance of Fig. 8 embodiment 7, Cr (VI) is 16.9mg/g.
Embodiment 8:
The impact of aluminum hydroxide film on Cr (VI) rate of adsorption is prepared under investigating different condition, done again " embodiment 1-7 " prepared aluminium hydroxide membrane sample to the curve of adsorption kinetics of Cr (VI), the preparation process of sample is as described in " embodiment 1-7 ".The adsorption kinetic data process is as follows:
The potassium bichromate solution of preparation 100ml, 100mg/LCr (VI), the pH hydrochloric acid solution of solution is adjusted to 3, add the above-mentioned sample of 400mg subsequently, sample when 0,0.5,1,2,4 and 8h respectively and measure the concentration (see figure 8) of Cr in filtrate (VI).
Fig. 8 shows, and different hydro pellumina reaches the time slightly difference of Cr (VI) adsorption equilibrium, roughly between 1-4h, has adsorption dynamics adsorption kinetics faster.
Embodiment 9:
Ability is used in order to investigate the circular regeneration after prepared aluminum hydroxide film absorption Cr (VI), further for the aluminium hydroxide membrane sample prepared by " embodiment 4 ", comparative study itself and Shandong Aluminum Plant's business boehmite are to the circular regeneration absorption property of Cr (VI).Circular regeneration adsorption experiment process is as follows:
The potassium bichromate solution two parts of preparation 100ml, 100mg/L, the pH hydrochloric acid solution of solution is adjusted to 3.0, add the aluminum hydroxide film prepared by 0.4g " embodiment 4 " and Shandong Aluminum Plant's business boehmite subsequently respectively, adsorption equilibrium is reached after 4h, sampling is separated and analyzes filtrate composition with ultraviolet-visible spectrophotometer, calculates its adsorbance.
Be separated respectively after completing adsorption process and reclaim above-mentioned adsorbent, in above-mentioned adsorbent, adding the Na of 150ml, 0.1mol/L further respectively
2cO
3solution, resolves completely by adsorbed Cr (VI), by adsorbent separation, dry rear recovery, repeats above-mentioned adsorption process.Adsorb 4 times according to above-mentioned Adsorption-desorption processes continuous circulation, working sample is at every turn to the adsorbance (Fig. 9) that Cr (VI) adsorbs.After 4 absorption, the rate of recovery of inoranic membrane is 93%, and the rate of recovery of Shandong Aluminum Plant's business boehmite is only 48%.
Fig. 9 shows, the adsorbance of original aluminum hydroxide film to Cr (VI) is 15.3mg/g, lower than Shandong Aluminum Plant's business boehmite to the adsorbance 16.1mg/g of Cr (VI), after circulation primary, the adsorbance of aluminum hydroxide film increases substantially to 28.1mg/g, higher than the adsorbance 16.1mg/g of this boehmite, after circulation second time, the adsorbance of aluminum hydroxide film and boehmite tends towards stability.Visible, when aluminum hydroxide film repeatedly recycles to the adsorbance of Cr (VI) apparently higher than certain business boehmite.
In above-described embodiment 1 ~ embodiment 9, before and after absorption at room temperature, the concentration of Cr (VI) adopts diphenyl carbazide spectrophotometry to measure, and ultraviolet-uisible spectrophotometer used is Japanese Shimadzu UVmini-1240 type.
It is important to emphasize, above-described embodiment is only used to the citing clearly illustrating that the present invention does, and the restriction completely not to embodiment.Those of ordinary skill in the field can also make other multi-form variation on the basis of the above description; here cannot also without the need to providing embodiment to all embodiments, but thus the apparent variation of amplifying out be still in protection scope of the present invention.
Claims (2)
1. a preparation method for aluminum hydroxide film, it is characterized in that a kind of based on sodium aluminate, for the absorption of Cr (VI) solution and the preparation method of the aluminum hydroxide film that can recycle, its step comprises:
(1) first sodium aluminate is dissolved in distilled water, obtains the sodium aluminate solution that concentration is 40-200g/L, add hydrochloric acid subsequently, under agitation form the suspension of aluminum hydroxide sol particle precipitation, then this suspension is transferred in water-bath the reaction that is hydrolyzed; The pH of described aluminum hydroxide sol particle precipitation suspension is 4-8;
(2) gained hydrolysis product is cooled, add the aqueous solution of peptizing agent and film forming agent polyvinyl alcohol (PVA), after stirring, obtain colloidal sol; The technological parameter of described hydrolysis is: reaction temperature is 60-90 DEG C, and the reaction time is 6-12h; Described peptizing agent is any one in hydrochloric acid, acetic acid and nitric acid, and its addition is: n (H
+): n (Al
3+)=0.07-0.25; Adopt PVA to assist film forming, the addition of PVA is mPVA:mAl
2o
3ratio for being greater than 0, being less than or equal to 0.8;
(3) by film, the drying after ageing 12-72h at 80-90 DEG C of gained colloidal sol, described aluminum hydroxide film is obtained.
2. the preparation method of aluminum hydroxide film according to claim 1, is characterized in that prepared aluminum hydroxide film is for adsorbing Cr (VI) solution that pH is 2-6; To adsorb the aluminum hydroxide film sodium carbonate desorption after Cr (VI), the aluminum hydroxide film after desorption recycles.
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| CN104741007A (en) * | 2015-04-16 | 2015-07-01 | 柳州豪祥特科技有限公司 | Preparation method of membrane separation layer for water treatment |
| CN105107486A (en) * | 2015-10-09 | 2015-12-02 | 武汉理工大学 | Preparation method of pseudo-boehmite composite film for adsorbing toxic Cr (VI) |
| CN109833851B (en) * | 2019-03-21 | 2021-11-30 | 陕西科技大学 | Nanofiber adsorption film prepared from vinasse and preparation method and application thereof |
| CN110064358B (en) * | 2019-05-08 | 2022-04-15 | 广州大学 | SiO for adsorbing toxic Cr (VI)2Gamma-AlOOH composite film and preparation method and application thereof |
| CN113979788B (en) * | 2021-11-23 | 2023-10-03 | 亚细亚建筑材料股份有限公司 | Self-cleaning super-hydrophilic ceramic material and preparation method thereof |
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| CN1868885A (en) * | 2006-05-12 | 2006-11-29 | 广西民族大学 | Self-dispersion type nanometer gamma A100H and its preparation method and use |
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| JPH03285079A (en) * | 1990-03-30 | 1991-12-16 | Teika Corp | Formation of alumina film on inorganic substrate of metal, glass, ceramics or the like |
| EP2361885A1 (en) * | 2008-10-29 | 2011-08-31 | Kawaken Fine Chemicals Co., Ltd. | Porous alumina free-standing film, alumina sol and methods for producing same |
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| Title |
|---|
| "SORPTION OF CHROMIUM(VI) AND CHROMIUM(III) ON ALUMINIUM HYDROXIDE";S. MUSIC;，et al;《Journal of Radioanalytical and Nuclear Chemistry》;19861231;第100卷(第1期);第187页第2段-第188页第1段，图1 * |
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