CN103861571B - The preparation method of polyaniline composite titanium dioxide adsorbent, application and renovation process - Google Patents
The preparation method of polyaniline composite titanium dioxide adsorbent, application and renovation process Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of polyaniline composite titanium dioxide adsorbent, application and renovation process, this adsorbent is formed via polyaniline and titanium dioxide generation In-situ reaction, described preparation method comprises the following steps: utilize organic or inorganic titanium source to be raw material, adopts sol-gel process at 0 ~ 100 DEG C of obtained transparent titania sol; Under-20 ~ 80 DEG C of conditions, the TiO 2 sol of gained and aniline monomer are mixed mutually, adopt chemical oxidization method realize In-situ reaction, after filtration after drying polyaniline composite nano titanium dioxide adsorbent.This adsorbent effectively can adsorb the dyestuff in dye wastewater with high concentration, and the preparation method of adsorbent is simple, and operation is short, and reaction condition is gentle; Obtained adsorbent dosage in dye wastewater treatment process is little, reaches time of equilibrium adsorption short, and adsorbance is large, and can repeated regeneration Long-Time Service, and the adsorbent after regeneration still reveals very high absorption property to dye sheet.
Description
[technical field]
The invention belongs to technical field of chemical synthesis, be specifically related to a kind of preparation method of polyaniline composite titanium dioxide adsorbent, application and renovation process.
[background technology]
There is a large amount of waste water from dyestuff to be discharged in water body every year to go, there is the features such as the bioprocess in high concentration, dark colour, complicated component, easily interference water body, so serious water pollution can be caused due to this kind of waste water.Therefore, from water body, remove dyestuff and there is great environment and technical significance.
Dye waste water treatment method conventional at present has absorption method, flocculent precipitation, electrolysis, oxidizing process and biological degradation method etc.But the shortcomings such as it is high that some of them method has cost, and timeliness is short.And absorption method is owing to having the advantages such as simple to operate, energy consumption is low, cost is low, non-secondary pollution, be the effective ways removing this pollutant.In numerous adsorbents, the specific area of active carbon and adsorbance are all comparatively large, are desirable sorbing materials.But active carbon price comparison is expensive, and the absorption property after not easily regenerating or regenerating reduces greatly, limits it and uses widely.Therefore develop cheap, preparation is simple, adsorbent that is high, the easy regeneration of clearance becomes the focus of research.Titanium dioxide, as a kind of semi-conducting material of nontoxic, stable, low cost, becomes the focus of people's research.Through the composite titania material that high molecular polymer is modified, there is more excellent performance, but not yet have bibliographical information through conducting polymer modified composite titania material as dye sorbent.
[summary of the invention]
The object of the invention is to for deficiency of the prior art, provide a kind of preparation method of polyaniline composite titanium dioxide adsorbent, application and renovation process.
For achieving the above object, the present invention adopts following technical scheme:
The preparation method of polyaniline composite titanium dioxide adsorbent, comprises the following steps:
1) be (0.04 ~ 10) according to the volume ratio of titanium source and alcohol: 1, titanium source and alcohol are mixed with the alcoholic solution of titaniferous, under agitation, the alcoholic solution of titaniferous is added drop-wise to pH value is 0.5 ~ 6.0, temperature is be hydrolyzed in the salpeter solution of 0 ~ 100 DEG C, the volume ratio keeping water in titanium source and salpeter solution is 1:(0.1 ~ 60), and stir 3 ~ 24h at normal temperatures, obtain transparent or translucent TiO 2 sol;
2) be 1:(0.05 ~ 50 by the TiO 2 sol of gained and aniline monomer with mol ratio) be mixed to get mixture, then be 1:(0.1 ~ 3 by the mol ratio of oxidant and aniline monomer) in mixture, add oxidant, 2 ~ 48h is reacted at-20 ~ 80 DEG C, finally to product after filtration, dry, obtain polyaniline composite nano titanium dioxide adsorbent.
The present invention further improves and is, in step 1), described titanium source is one or more in titanium tetrachloride, tetrabutyl titanate, isopropyl titanate or metatitanic acid methyl esters.
The present invention further improves and is, in step 1), described alcohol is one or more in normal propyl alcohol, isopropyl alcohol, absolute ethyl alcohol, methyl alcohol, butanols or the tert-butyl alcohol.
The present invention further improves and is, step 2) in, oxidant is one or more in iron chloride, ammonium persulfate, potassium peroxydisulfate or potassium permanganate.
Another object of the present invention, the application of polyaniline composite titanium dioxide adsorbent in absorbing dye.
The present invention further improves and is, the dyestuff that polyaniline composite titanium dioxide adsorbent can adsorb comprises one or more in cationic dyes, anionic dyes or nonionic dye.
The present invention further improves and is, concrete technology step is: 1 ~ 120min is soaked in the acid of polyaniline composite titanium dioxide adsorbent or alkali, then add in the waste water containing dyestuff, the quantity of sorbent added is 1/500 ~ 1/100 of waste water weight, adsorb 30 ~ 90min at normal temperatures, after absorption, adsorbent is separated with waste water from dyestuff.
Another object of the present invention, after being separated by the adsorbent after absorbing dye, soaking 1 ~ 120min with bronsted lowry acids and bases bronsted lowry solution successively or soaks 1 ~ 120min with alkali and acid solution successively, realizing the desorption of dyestuff and the regeneration of adsorbent.
The present invention further improves and is, alkali used is one or more in NaOH, potassium hydroxide, calcium hydroxide, lithium hydroxide, barium hydroxide or ammoniacal liquor; Acid used is one or more in nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid, formic acid, acetic acid, hydrofluoric acid or benzoic acid.
The present invention further improves and is, paper mill wastewater used is 0.01 ~ 15molL
-1, the concentration of acid used is 0.01 ~ 15molL
-1.
Relative to prior art, the invention has the advantages that:
1, the present invention adopts organic or inorganic titanium source to be raw material, and by the modification of polyaniline, prepare new composite adsorbent, its raw material is easy to get, and technique is simple, with low cost;
2, in the adsorbent use procedure prepared of the present invention, consumption is few, and time of equilibrium adsorption is short, and adsorption is high, dye wastewater treatment with low cost;
3, the adsorbent reactivation prepared of the present invention is very good, and regenerative process is very little on the impact of its absorption property, and the adsorbent after repeatedly regeneration still shows good absorption property, and is applicable to large-scale industrial production and use.
[detailed description of the invention]
Below in conjunction with specific embodiment, the present invention is described in further details.
One, the preparation of adsorbent
Pulp furnish: Organic Alcohol: titanium source: acid solution=(0.4 ~ 10): 1: (0.1 ~ 60) (with volume basis), aniline monomer: acid solution: oxidant=1: 0.02 ~ 20: 0.1 ~ 3(is with molar ratio computing)
The concrete technology prescription of TiO 2 sol is as shown in the table:
The concrete pulp furnish of compound adsorbent is as shown in the table:
Processing step:
1) be (0.04 ~ 10) according to the volume ratio of titanium source and alcohol: 1, titanium source and alcohol are mixed with the alcoholic solution of titaniferous, under agitation, the alcoholic solution of titaniferous is added drop-wise to pH value is 0.5 ~ 6.0, temperature is be hydrolyzed in the salpeter solution of 0 ~ 100 DEG C, the volume ratio keeping water in titanium source and salpeter solution is 1:(0.1 ~ 60), and stir 3 ~ 24h at normal temperatures, obtain transparent or translucent TiO 2 sol;
2) be 1:(0.05 ~ 50 by the TiO 2 sol of gained and aniline monomer with mol ratio) be mixed to get mixture, then be 1:(0.1 ~ 3 by the mol ratio of oxidant and aniline monomer) in mixture, add oxidant, 2 ~ 48h is reacted at-20 ~ 80 DEG C, finally to product after filtration, dry, obtain polyaniline composite nano titanium dioxide adsorbent.
Two, adsorbent is tested the adsorption capacity of dyestuff
In adsorption test, the adsorbent prepared is placed in certain density dye solution by us, and the adsorption rate measuring its absorbing dye is to weigh the adsorption capacity of this adsorbent to anionic dye and the dye of positive ion.
Adsorbent: polyaniline/titanium dioxide compound adsorbent (processing with acid or alkali in advance).
Anionic dye: Acid Red G; The dye of positive ion: methylene blue.
Adsorption conditions: dye strength is 500mgL
-1, adsorption temp is room temperature; Ratio (adsorbent and dye liquor mass ratio) is 1:1000; Absorption 30 ~ 90min.
Test and operation: accurately take various dyestuff 0.500g, put into small beaker, adding distil water dissolves, and then move in 1000mL volumetric flask, it is stand-by that adding distil water is diluted to scale.
Install adsorbent equipment, two kinds of dyestuffs are each a set of.Accurately taking each 30mL of above-mentioned joined dye liquor with pipette joins in adsorbent equipment, adds the pretreated adsorbent of 30mg, take out adsorbent after 45min in anionic dye solution, retains raffinate; In dye of positive ion solution, add the pretreated adsorbent of 30mg, centrifugal recovery adsorbent after 90min, the centrifugal supernatant obtained measures absorbance.
Centrifugal clear liquid obtained above and blank dye solution (not adding the dye solution of adsorbent) are used its absorbance A of spectrophotometric determination (blank dye liquor is too dense, can suitably dilute) respectively
Wherein A
1the absorbance of solution after various dyestuff adsorbent, A
0it is the absorbance of the dye solution not adding adsorbent.
Three, adsorbent reactivation
1) will be adsorbed with the adsorbent of anionic dye, be 0.01 ~ 15molL by concentration
-1aqueous slkali soaking 1 ~ 120 minute, can get off anionic dye from desorption adsorbent; Use 0.01 ~ 15molL again
-1acid solution soaks 1 ~ 120min, can realize the regeneration of adsorbent.
2) will be adsorbed with the adsorbent of the dye of positive ion, be 0.01 ~ 15molL by concentration
-1acid solution soaks 1 ~ 120min, the dye of positive ion can be got off from desorption adsorbent; Use 0.01 ~ 15molL again
-1aqueous slkali soaking 1 ~ 120min, can realize the regeneration of adsorbent.
Adsorbent after regeneration, then be used for adsorbing different dyestuffs, and measure its adsorption efficiency, then adopt soda acid process to realize the regeneration of adsorbent; Adsorbent after regeneration is used for adsorbing different dyestuffs again, realizes recycling.
Embodiment 1:
1) 20mL normal propyl alcohol and 20mL tetrabutyl titanate is got, be mixed with the alcoholic solution of tetrabutyl titanate, with vigorous stirring, the alcoholic solution of tetrabutyl titanate be slowly added drop-wise to pH is 1, temperature is be hydrolyzed in the salpeter solution of the 400mL of 100 DEG C, and stir 4h, can transparent titania sol be obtained;
2) at-10 DEG C, add the aniline monomer of 0.15mL in the colloidal sol of gained, mix and blend 0.5h, dropwise adds 20mL, 1molL
-1ammonium persulfate solution realize oxidation polymerization as oxidant, drip after-5 DEG C leave standstill reaction more than 20h, after filtration dry after can obtain cyan product, be polyaniline composite nano titanium dioxide sorbing material;
3) remove the anionic dye Acid Red G in solution with the adsorbent prepared, in the brown bottle of lucifuge process, add initial concentration is 500mgL
-1acid Red G solution 30mL, adsorbent dosage acid-treated is in advance 60mg, magnetic agitation 45min, after stirring, centrifugal and measure the concentration of Acid Red G in supernatant, obtains adsorbent and can reach more than 90% to the eliminating rate of absorption of the Acid Red G under this concentration;
4) adsorb the adsorbent of Acid Red G, first use 5molL
-1soaking with sodium hydroxide 10min, then use 1molL
-1hydrochloric acid solution soak 10min, namely realize the regeneration of adsorbent; Adsorbent after regeneration is again in order to remove the Acid Red G in solution, and in the brown bottle of lucifuge process, add initial concentration is 500mgL
-1acid Red G solution 30mL, add the adsorbent after regeneration (30mg), magnetic agitation 45min, after stirring, the concentration of Acid Red G in centrifugal mensuration filtrate, obtain the adsorbent after regenerating and can reach more than 90% to the eliminating rate of absorption of the Acid Red G under this concentration, after ten absorption regenerations, adsorbent still can reach more than 90% to the adsorption rate of the Acid Red G under this concentration.
Embodiment 2:
1) 20mL methyl alcohol and 20mL titanium tetrachloride is got, be mixed with the alcoholic solution of titanium tetrachloride, with vigorous stirring, the alcoholic solution of titanium tetrachloride be slowly added drop-wise to pH is 0.5, temperature is be hydrolyzed in the salpeter solution of the 400mL of 100 DEG C, and stir 4h, can transparent titania sol be obtained;
2) at-10 DEG C, add the aniline monomer of 0.15mL in the TiO 2 sol of gained, mix and blend 0.5h, dropwise adds 20mL, 1molL
-1potassium persulfate solution realize oxidation polymerization as oxidant, after dripping, at-5 DEG C leave standstill reaction more than 20h, after filtration dry after can obtain cyan product, be polyaniline composite nano titanium dioxide sorbing material;
3) remove the anionic dye Acid Red G in solution with the adsorbent prepared, in the brown bottle of lucifuge process, add initial concentration is 500mgL
-1acid Red G solution 30mL, adsorbent dosage acid-treated is in advance 60mg, magnetic agitation 45min, after stirring, centrifugal and measure the concentration of Acid Red G in supernatant, obtains adsorbent and can reach more than 90% to the eliminating rate of absorption of the Acid Red G under this concentration;
4) adsorb the adsorbent of Acid Red G, first use 5molL
-1soaking with sodium hydroxide 10min, then use 1molL
-1hydrochloric acid solution soak 10min, namely realize the regeneration of adsorbent; Adsorbent after regeneration is again in order to remove the Acid Red G in solution, and in the brown bottle of lucifuge process, add initial concentration is 500mgL
-1acid Red G solution 30mL, add the adsorbent after regeneration (30mg), magnetic agitation 45min, after stirring, the concentration of Acid Red G in centrifugal mensuration filtrate, obtain the adsorbent after regenerating and can reach more than 90% to the eliminating rate of absorption of the Acid Red G under this concentration, after ten absorption regenerations, adsorbent still can reach more than 90% to the adsorption rate of the Acid Red G under this concentration.
Embodiment 3:
1) 10mL metatitanic acid methyl esters and 20mL absolute ethyl alcohol is got, be mixed with the alcoholic solution of metatitanic acid methyl esters, with vigorous stirring, the alcoholic solution of metatitanic acid methyl esters be slowly added drop-wise to pH is 3, temperature is be hydrolyzed in the salpeter solution of the 100mL of 25 DEG C, and stir 5h, can transparent titania sol be obtained;
2) at 50 DEG C, in the colloidal sol of gained, add the aniline monomer of 30mL, mix and blend 0.5h, dropwise adds 150mL, 1molL
-1ammonium persulfate solution realize oxidation polymerization as oxidant, at 50 DEG C of standing more than sustained response 20h after dripping, the product of black after drying, can be obtained after filtration, be polyaniline composite nano titanium dioxide sorbing material;
3) by the adsorbent prepared in order to remove the methylene blue in solution, in the brown bottle of lucifuge process, add initial concentration is 500mgL
-1methylene blue solution 30mL, the dosage of adsorbent alkali-treated is in advance 50mg, magnetic agitation 90min, after stirring, the concentration of centrifugal mensuration supernatant Methylene Blue, obtains adsorbent and can reach more than 90% to the eliminating rate of absorption of the methylene blue under this concentration;
4) adsorb the adsorbent of methylene blue, first use 1molL
-1nitric acid dousing 10min, then use 1molL
-1sodium hydroxide solution soak 10min, namely realize the regeneration of adsorbent; Adsorbent after regeneration is again in order to remove the methylene blue in solution, and in the brown bottle of lucifuge process, add initial concentration is 500mgL
-1acid Red G solution 30mL, add the adsorbent after regeneration (50mg), magnetic agitation 90min, after stirring, the concentration of centrifugal mensuration filtrate Methylene Blue, obtain adsorbent and can reach more than 90% to the eliminating rate of absorption of the methylene blue under this concentration, after seven absorption regenerations, adsorbent still can reach more than 90% to the adsorption rate of the methylene blue under this concentration.
Embodiment 4:
1) 10mL titanium tetrachloride and the 20mL tert-butyl alcohol is got, be mixed with the alcoholic solution of titanium tetrachloride, with vigorous stirring, the alcoholic solution of titanium tetrachloride be slowly added drop-wise to pH is 3, temperature is be hydrolyzed in the salpeter solution of the 100mL of 25 DEG C, and stir 5h, can transparent titania sol be obtained;
2) at 50 DEG C, in the colloidal sol of gained, add the aniline monomer of 30mL, mix and blend 0.5h, dropwise adds 150mL, 1molL
-1ammonium persulfate solution realize oxidation polymerization as oxidant, at 50 DEG C of standing more than sustained response 20h after dripping, the product of black after drying, can be obtained after filtration, be polyaniline composite nano titanium dioxide sorbing material;
3) by the adsorbent prepared in order to remove the methylene blue in solution.In the brown bottle of lucifuge process, add initial concentration is 500mgL
-1methylene blue solution 30mL, the dosage of adsorbent alkali-treated is in advance 50mg, magnetic agitation 90min, after stirring, the concentration of centrifugal mensuration supernatant Methylene Blue, obtains adsorbent and can reach more than 90% to the eliminating rate of absorption of the methylene blue under this concentration;
4) adsorb the adsorbent of methylene blue, first use 1molL
-1nitric acid dousing 10min, then use 1molL
-1sodium hydroxide solution soak 10min, namely realize the regeneration of adsorbent; Adsorbent after regeneration is again in order to remove the methylene blue in solution, and in the brown bottle of lucifuge process, add initial concentration is 500mgL
-1acid Red G solution 30mL, add the adsorbent after regeneration (50mg), magnetic agitation 90min, after stirring, the concentration of centrifugal mensuration filtrate Methylene Blue, obtain adsorbent and can reach more than 90% to the eliminating rate of absorption of the methylene blue under this concentration, after seven absorption regenerations, adsorbent still can reach more than 90% to the adsorption rate of the methylene blue under this concentration.
The regenerability of adsorbent is as shown in the table:
In sum, the present invention replaces its photocatalysis performance by the adsorption capacity of research polyaniline/titanium dioxide composite, makes suction-operated become the predominant intermolecular forces removing dyes.The absorption property of this adsorbent is suitable with the absorption property commonly using activated carbon of sorbent at present, even better.Polyaniline composite titanium dioxide performance of the adsorbent prepared by the present invention is stable, nontoxic, easy to use, adding less, elapsed time is short, effectively can adsorb the various dyestuffs in the waste water from dyestuff of high concentration, easy regeneration and can repeatedly recycling, adsorbent after regeneration still has very strong absorption property, obviously can reduce the cost of dye wastewater treatment.Sorbent material wide material sources prepared by the present invention, cost of material is low, and preparation technology is simple, prepares under atmospheric low-temperature, safe and reliable, has higher economic results in society.
Claims (6)
1. the renovation process of polyaniline composite titanium dioxide adsorbent, it is characterized in that, after adsorbent after absorbing dye is separated, soaks 1 ~ 120min with bronsted lowry acids and bases bronsted lowry solution successively or soak 1 ~ 120min with alkali and acid solution successively, realizing the desorption of dyestuff and the regeneration of adsorbent; Wherein, the preparation method of this polyaniline composite titanium dioxide adsorbent comprises the steps:
1) be (0.04 ~ 10) according to the volume ratio of titanium source and alcohol: 1, titanium source and alcohol are mixed with the alcoholic solution of titaniferous, under agitation, the alcoholic solution of titaniferous is added drop-wise to pH value is 0.5 ~ 6.0, temperature is be hydrolyzed in the salpeter solution of 0 ~ 100 DEG C, the volume ratio keeping water in titanium source and salpeter solution is 1:(0.1 ~ 60), and stir 3 ~ 24h at normal temperatures, obtain transparent or translucent TiO 2 sol;
2) be 1:(0.05 ~ 50 by the TiO 2 sol of gained and aniline monomer with mol ratio) be mixed to get mixture, then be 1:(0.1 ~ 3 by the mol ratio of oxidant and aniline monomer) in mixture, add oxidant, 2 ~ 48h is reacted at-20 ~ 80 DEG C, finally to product after filtration, dry, obtain polyaniline composite nano titanium dioxide adsorbent.
2. the renovation process of polyaniline composite titanium dioxide adsorbent according to claim 1, is characterized in that, alkali used is one or more in NaOH, potassium hydroxide, calcium hydroxide, lithium hydroxide, barium hydroxide or ammoniacal liquor; Acid used is one or more in nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid, formic acid, acetic acid, hydrofluoric acid or benzoic acid.
3. the renovation process of polyaniline composite titanium dioxide adsorbent according to claim 1, is characterized in that, the concentration of aqueous slkali used is 0.01 ~ 15molL
-1, the concentration of acid solution used is 0.01 ~ 15molL
-1.
4. the renovation process of polyaniline composite titanium dioxide adsorbent according to claim 1, is characterized in that, step 1) in, described titanium source is one or more in titanium tetrachloride, tetrabutyl titanate, isopropyl titanate or metatitanic acid methyl esters.
5. the renovation process of polyaniline composite titanium dioxide adsorbent according to claim 1, is characterized in that, step 1) in, described alcohol is one or more in normal propyl alcohol, isopropyl alcohol, absolute ethyl alcohol, methyl alcohol, butanols or the tert-butyl alcohol.
6. the renovation process of polyaniline composite titanium dioxide adsorbent according to claim 1, is characterized in that, step 2) in, oxidant is one or more in iron chloride, ammonium persulfate, potassium peroxydisulfate or potassium permanganate.
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| CN104383966A (en) * | 2014-12-03 | 2015-03-04 | 中国石油大学(华东) | Preparation method of 3D ordered macroporous polyaniline (OM PANI)/TiO2 composite photocatalytic material and application thereof |
| CN107335495A (en) * | 2017-06-08 | 2017-11-10 | 全椒县崇明米业有限公司 | A kind of big rice processing method for reducing content of cracking rice |
| CN107417050A (en) * | 2017-09-12 | 2017-12-01 | 西安交通大学 | A kind of low concentration advanced treatment method for printing and dyeing wastewater |
| CN110433778A (en) * | 2019-07-05 | 2019-11-12 | 南华大学 | Polyaniline/graphite oxide phase carbon nitride composite material preparation method and application |
| CN110605101A (en) * | 2019-10-08 | 2019-12-24 | 西安交通大学 | Adsorbent for adsorbing lead ions, and membrane protective agent and water treatment agent containing same |
| CN110605102A (en) * | 2019-10-08 | 2019-12-24 | 西安交通大学 | Composite adsorbent, membrane protective agent and water treatment agent |
| CN110975846A (en) * | 2019-12-23 | 2020-04-10 | 武汉工程大学 | Clay mineral/conductive polymer composite adsorbent and preparation method and application thereof |
| CN111908672A (en) * | 2020-06-29 | 2020-11-10 | 西安交通大学 | Method and system for adsorbing, removing and recycling chloride ions in chlorine-containing wastewater |
| CN112387257A (en) * | 2020-11-05 | 2021-02-23 | 西安工程大学 | Preparation method of high-molecular polyaniline porous filler water treatment adsorbent |
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