CN102350317B - Polypyrrole/titanium dioxide composite adsorbent, its preparation, application and regeneration methods - Google Patents
Polypyrrole/titanium dioxide composite adsorbent, its preparation, application and regeneration methods Download PDFInfo
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Abstract
The invention relates to an adsorbent for adsorbing dye in water, and its preparation, application and regeneration methods. The adsorbent provided by the invention is prepared by in situ composition of polypyrrole and titanium dioxide. The mass ratio of titanium dioxide to polypyrrole in the composite adsorbent is 1: 0.05-50. The preparation method comprises the following steps of: using an organic or inorganic titanium source as a raw material, and adopting a sol-gel method at the temperature of 0-100 DEG C to prepare a titanium dioxide sol; Mixing the obtained titanium dioxide sol with a pyrrole monomer at the temperature of minus 20-80 DEG C, realizing in situ composite by the chemical oxidation process, filtering and drying to obtain the polypyrrole nanometer titanium dioxide composite adsorbent. By the adoption of the adsorbent, dye in high-density dye wastewater can be effectively adsorbed. The preparation method is simple, and has short process and mild reaction condition; the addition quantity of the prepared adsorbent during the dye wastewater treatment process is little; the adsorption balance time is short; the adsorbent can be repeatedly regenerated and used for a long time; and the regenerated adsorbent still has high adsorption performance.
Description
Technical field
The present invention relates to utilize a kind of adsorbent and preparation method thereof, particularly polypyrrole/titanium dioxide compound adsorbent and preparation method thereof, this invention also relates to described adsorbent and utilizes the application of absorption principle dye wastewater treatment using and the renovation process of this adsorbent.
Background technology
All having a large amount of waste water from dyestuff from fields such as printing and dyeing, papermaking, plastics, leather, food and mineral processing industry to be discharged into every year goes in the water body, features such as high concentration, color are dark because such waste water has, complicated component, not only cause visual pollution, also can disturb the bioprocess in the water body, so can cause the problem of serious water pollution.Therefore, from water body, remove dyestuff and have great environment and technical significance.
Dye waste water treatment method commonly used at present has absorption method, flocculent precipitation, electrolysis, oxidizing process and biological degradation method etc.Shortcomings such as but the some of them method has the cost height, and timeliness is short.And absorption method is effective ways of removing this pollutant owing to have simple to operate, advantages such as energy consumption is low, cost is low, non-secondary pollution.In numerous adsorbents, the specific area of active carbon and adsorbance are all bigger, are desirable sorbing materials.But the active carbon price comparison is expensive, and the absorption property that is difficult for after regeneration or the regeneration reduces greatly, has limited it and has used widely.Therefore develop cheap, preparation is simple, clearance adsorbent high, easy regeneration becomes the focus of research.Titanium dioxide becomes the focus of people's research as a kind of nontoxic, stable, semi-conducting material cheaply.Composite titania material after the high molecular polymer modification has excellent more performance, but as dye sorbent bibliographical information is not arranged as yet through conducting polymer modified composite titania material.
Summary of the invention
The present invention seeks to: sorbent material of dyestuff in a kind of novel efficiently adsorbed water and preparation method thereof is provided, with and use and renovation process.
Technical scheme of the present invention is:
Polypyrrole/titanium dioxide compound adsorbent is polymerized by TiO 2 sol and oxidizable pyrrole, and the sorbent molecule formula is:
, the mol ratio of TiO 2 sol and pyrrole monomer is n:m=0.05 ~ 50:1 in the adsorbent.
The preparation method of polypyrrole/titanium dioxide compound adsorbent, its processing step is as follows:
(1) preparation TiO 2 sol: the volume ratio in titanium source and alcohol is 0.1 ~ 25 ratio, titanium source and alcohol is mixed with the alcoholic solution of titaniferous.Under vigorous stirring, with this alcoholic solution that obtains be added drop-wise to slowly that pH is 0.5 ~ 6.0, temperature is hydrolysis in 0 ~ 100 ℃ the salpeter solution, keeping the volume ratio of water in titanium source and the aqueous acid is 1: 0.1 ~ 60, and stir 3 ~ 24h at normal temperatures, can obtain transparent or translucent TiO 2 sol.
(2) under-20 ~ 80 ℃, the ratio that the TiO 2 sol and the pyrrole monomer of gained with the mol ratio is 1:0.05 ~ 50 is mixed mutually, adopt chemical oxidization method to realize oxidation polymerization, and the mol ratio of oxidant and pyrrole monomer is 1:0.1 ~ 3, and more than-20 ~ 80 ℃ of following sustained response 20h, filtration drying get final product polypyrrole composite nano titanium dioxide adsorbent.
Titanium source in the described step (1) is one or more the mixture in titanium tetrachloride, tetrabutyl titanate, isopropyl titanate, the metatitanic acid methyl esters.
Alcohol in the described step (1) is one or more mixtures in normal propyl alcohol, isopropyl alcohol, absolute ethyl alcohol, methyl alcohol, butanols, the tert-butyl alcohol.
Oxidant in the described step (2) is one or more mixtures in iron chloride, ammonium persulfate, potassium peroxydisulfate, the potassium permanganate.
The use renovation process of polypyrrole/titanium dioxide compound adsorbent, its processing step is as follows:
Handle anionic dye:
(1) absorption: with adsorbent with 0.01 ~ 15 mol L
-1Acid solution soaked 1 ~ 120 minute, put into the sewage that contains anionic dye then, its concentration is 500 mg L
-1, the quantity of sorbent of adding is 1/100 ~ 1/500 of a sewage weight, and adsorption temp is under the normal temperature, and adsorption time is 30 ~ 90 minutes, and adsorbent reactivation is taken out in the absorption back;
(2) regeneration: the adsorbent that will be adsorbed with anionic dye is with 0.01 ~ 15 mol L
-1Aqueous slkali soaking 1 ~ 120 minute, inhale that to take off than (volume ratio of alkali lye and sewage) be 10 ~ 100:1, anionic dye desorb from the adsorbent can be got off.With the adsorbent after the desorb with 0.01 ~ 15 mol L
-1Acid solution soaked 1 ~ 120 minute, acid solution can use repeatedly to solution and be neutral, can make its absorption property regeneration, the adsorbent after the regeneration can be recycled and repeatedly still has very high adsorption capacity.
Handle the dye of positive ion:
(3) absorption: with adsorbent with 0.01 ~ 15 mol L
-1Aqueous slkali soaking 1 ~ 120 minute, put into the sewage that contains the dye of positive ion then, its concentration is 500 mg L
-1, the quantity of sorbent of adding is 1/100 ~ 1/500 of a sewage weight, and adsorption temp is under the normal temperature, and adsorption time is 30 ~ 90 minutes, and adsorbent reactivation is taken out in the absorption back;
(4) regeneration: the adsorbent that will be adsorbed with the dye of positive ion is with 0.01 ~ 15 mol L
-1Acid solution soaked 1 ~ 120 minute, inhale that to take off than (volume ratio of acid solution and sewage) be 10 ~ 100:1, dye of positive ion desorb from the adsorbent can be got off.With the adsorbent after the desorb with 0.01 ~ 15 mol L
-1Aqueous slkali soaking 1 ~ 120 minute, aqueous slkali can use repeatedly to solution and be neutral, can make its absorption property regeneration, the adsorbent after the regeneration can be recycled and repeatedly still has very high adsorption capacity.
Described step (1), (2) and (4) used acid are one or more the mixture in nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid, formic acid, acetate, hydrofluoric acid, the benzoic acid.
Described step (2), (3) and (4) used alkali are one or more mixtures in NaOH, potassium hydroxide, calcium hydroxide, lithium hydroxide, barium hydroxide, the ammoniacal liquor.
The desorption of described dyestuff and the regenerative process of adsorbent can realize in position, also can realize in dystopy.
The present invention replaces its photocatalysis performance by the adsorption capacity of discovering polypyrrole/composite titania material, becomes the main active force of removing dyestuff in the water body.The absorption property of this adsorbent is suitable with the absorption property of activated carbon of sorbent at present commonly used, at home and abroad there is no special in the report of polymer modification titanium dioxide to the absorption of dyestuff in the water body at present.Product of the present invention is stable, nontoxic, easy to use, adding less, elapsed time is short, can effectively adsorb the various dyestuffs in the waste water from dyestuff of high concentration, easily regeneration and can repeatedly recycling, adsorbent after the regeneration still has very strong absorption property, can obviously reduce the cost of dye wastewater treatment using.The sorbent material wide material sources of the present invention's preparation, cost of material is low, and preparation technology is simple, and atmospheric low-temperature preparation down is safe and reliable, has higher economic results in society.
Advantage of the present invention is:
1. to adopt organic or inorganic titanium source be raw material in the present invention, by the modification of polypyrrole, and preparation NEW TYPE OF COMPOSITE adsorbent, raw material is easy to get, and technology is simple, and is with low cost.
2. consumption is few in the adsorbent use, and the adsorption equilibrium time is short, absorption usefulness height, dye wastewater treatment using with low cost.
3. product of the present invention is easy to regeneration, and reproducibility is good, and the adsorbent after the regeneration still shows excellent absorption property.Still show good adsorption property through the adsorbent after repeatedly regenerating.
4. be fit to large-scale industrial production and use.
Description of drawings
Below in conjunction with drawings and Examples the present invention is further described:
Fig. 1 is the X-ray diffractogram of adsorbent of the present invention;
Fig. 1 explanation: the diffraction maximum that appears at 25.3 °, 37.8 ° and 48.1 ° in the X-ray diffractogram is (101), (004) and (200) face of corresponding anatase titania respectively; The diffraction maximum that appears at 27.5 °, 36.1 ° and 41.2 ° is (110), (101) and (111) face of corresponding rutile titanium dioxide respectively, illustrates that titanium dioxide is the mixed crystal of anatase and rutile.The diffraction maximum that does not occur polypyrrole in the X-ray diffractogram illustrates that polypyrrole is amorphous.
Fig. 2 is the infrared-visible light spectrogram of adsorbent of the present invention.
Fig. 2 explanation: in infrared spectrogram, appear at 400-700 cm
-1The Ti O beam mode of the corresponding titanium dioxide of broad peak; Appear at 3425cm
-1The corresponding titanium dioxide in peak-the OH group or the stretching vibration of the NH group of polypyrrole; 1640 cm
-1The in-plane bending vibration of the NH group of corresponding polypyrrole; 1451 cm
-1The C N stretching vibration of corresponding polypyrrole.Prove that this adsorbent is the compound of polypyrrole and titanium dioxide.
The specific embodiment
At first, preparation adsorbent; Secondly, the adsorbent for preparing is placed certain density dye solution, measure the adsorption rate of its absorbing dye and weigh the adsorption capacity of this adsorbent dyestuff; At last, through suitable renovation process, measure the recyclability that this adsorbent is evaluated to the adsorption rate and the absorption regeneration number of times of dyestuff in its regeneration back.
The method of testing of eliminating rate of absorption is as follows:
Install and inhale the look device, and accurately take by weighing certain volume and certain density dye liquor joins in the dyeing apparatus, add a certain amount of pretreated adsorbent again, take out adsorbent after absorption a period of time, keep raffinate with pipette.Above-mentioned raffinate and blank dye liquor (dye liquor that does not add adsorbent) are used its absorbance A of UV-vis spectrophotometric determination (blank dye liquor is too dense, can suitably dilute) respectively.
A wherein
1Be various dyestuffs with adsorbents adsorb after the absorbance of raffinate, A
0It is the absorbance of blank dye liquor.
Specific embodiment 1:
Preparation:
(1) get 20 mL butyl titanates, 20 mL normal propyl alcohols are mixed with the alcoholic solution of butyl titanate; Under vigorous stirring, with the alcoholic solution of butyl titanate be added drop-wise to slowly that pH is 1, temperature is hydrolysis in 100 ℃ the salpeter solution of 400 mL, and stirs 5h, can obtain transparent titanium dioxide colloidal sol.
℃ (2)-20 ~ 10 under, in the colloidal sol of gained, add the pyrrole monomer of 0.10 mL, mix and stir 0.5 h, dropwise add 20 mL, 1 mol L
-1Ferric chloride solution realize oxidation polymerization as oxidant, drip the back leaving standstill under this temperature more than reaction 20 h, can get the product of black after filtration after the oven dry, be polypyrrole composite nano titanium dioxide sorbing material.
Use:
(3) adsorbent for preparing is used for removing the anionic dye Acid Red G of solution.Adding initial concentration in the brown bottle that lucifuge is handled is 500 mg L
-1Acid Red G solution 30 mL, the dosage of the adsorbent of acid treatment in advance is 60 mg, magnetic agitation 45 min, after the stirring, the concentration of Acid Red G in the centrifugal mensuration filtrate obtains adsorbent and can reach more than 90% the eliminating rate of absorption of the Acid Red G under this concentration.
Renovation process and regenerability:
(4) adsorbed the adsorbent of Acid Red G, earlier with 5 mol L
-1Soaking with sodium hydroxide 10 min, use 1 mol L again
-1Salpeter solution soak 10 min, promptly realize the regeneration of adsorbent.Adsorbent after the regeneration is again in order to remove the Acid Red G in the solution.Adding initial concentration in the brown bottle that lucifuge is handled is 500 mg L
-1Acid Red G solution 30 mL, add the adsorbent (60mg) after the regeneration, magnetic agitation 45 min, after the stirring, the concentration of Acid Red G in the centrifugal mensuration filtrate, the adsorbent after obtaining regenerating can reach more than 90% the eliminating rate of absorption of the Acid Red G under this concentration.Through behind ten absorption regenerations, adsorbent still can reach more than 90% the adsorption rate of the Acid Red G under this concentration.
Specific embodiment 2:
Preparation:
(1) get 10 mL butyl titanates, 10 mL isopropyl alcohols are mixed with the alcoholic solution of butyl titanate; Under vigorous stirring, with the alcoholic solution of butyl titanate be added drop-wise to slowly that pH is 2, temperature is hydrolysis in 80 ℃ the salpeter solution of 100 mL, and stirs 5h, can obtain transparent titanium dioxide colloidal sol.
Under (2) 10 ~ 25 ℃, in the colloidal sol of gained, add the pyrrole monomer of 5.0 mL, mix and stir 0.5 h, dropwise add 10 mL, 1 mol L
-1Ferric chloride solution realize oxidation polymerization as oxidant, drip the back leaving standstill under this temperature more than reaction 20 h, can get the product of black after filtration after the oven dry, be polypyrrole composite nano titanium dioxide sorbing material.
Use:
(3) adsorbent for preparing is used for removing the Acid Red G of solution.Adding initial concentration in the brown bottle that lucifuge is handled is 500 mg L
-1Acid Red G solution 30 mL, the dosage of the adsorbent of acid treatment in advance is 80 mg, magnetic agitation 45 min, after the stirring, the concentration of Acid Red G in the centrifugal mensuration filtrate obtains adsorbent and can reach more than 90% the eliminating rate of absorption of the Acid Red G under this concentration.
Regeneration and regenerability:
(4) adsorbed the adsorbent of Acid Red G, earlier with 3 mol L
-1Soaking with sodium hydroxide 10 min, use 1 mol L again
-1Hydrochloric acid solution soak 10 min, promptly realize the regeneration of adsorbent.Adsorbent after the regeneration is again in order to remove the Acid Red G in the solution.Adding initial concentration in the brown bottle that lucifuge is handled is 500 mg L
-1Acid Red G solution 30 mL, add the adsorbent (80 mg) after the regeneration, magnetic agitation 45 min, after the stirring, the concentration of Acid Red G in the centrifugal mensuration filtrate obtains adsorbent and can reach more than 90% the eliminating rate of absorption of the Acid Red G under this concentration.Through behind ten absorption regenerations, adsorbent still can reach more than 90% the adsorption rate of the Acid Red G under this concentration.
Specific embodiment 3:
Preparation:
(1) get 10 mL butyl titanates, 20 mL absolute ethyl alcohols are mixed with the alcoholic solution of butyl titanate; Under vigorous stirring, with the alcoholic solution of butyl titanate be added drop-wise to slowly that pH is 2, temperature is hydrolysis in 25 ℃ the salpeter solution of 100 mL, and stirs 5h, can obtain transparent titanium dioxide colloidal sol.
Under (2) 50 ~ 75 ℃, in the colloidal sol of gained, add the pyrrole monomer of 30 mL, mix and stir 0.5 h, dropwise add 150 mL, 1 mol L
-1Ammonium persulfate solution realize oxidation polymerization as oxidant, drip the back leaving standstill under this temperature more than sustained response 20 h, can get the product of black after filtration after the drying, be polypyrrole composite nano titanium dioxide sorbing material.
Use:
(3) with the adsorbent for preparing in order to remove the methylene blue in the solution.Adding initial concentration in the brown bottle that lucifuge is handled is 500 mg L
-1Methylene blue solution 30 mL, the dosage of the adsorbent of alkali treatment in advance is 60 mg, and magnetic agitation 90 min are after the stirring, the concentration of methylene blue in the centrifugal mensuration filtrate obtains adsorbent and can reach more than 90% the eliminating rate of absorption of the methylene blue under this concentration.
Regeneration and regenerability:
(4) adsorbed the adsorbent of methylene blue, earlier with 1 mol L
-1Nitric acid dousing 10 min, use 1 mol L again
-1Sodium hydroxide solution soak 10 min, promptly realize the regeneration of adsorbent.Adsorbent after the regeneration is again in order to remove the methylene blue in the solution.Adding initial concentration in the brown bottle that lucifuge is handled is 500 mg L
-1Acid Red G solution 30 mL, add the adsorbent (60 mg) after the regeneration, magnetic agitation 90 min, after the stirring, the concentration of methylene blue in the centrifugal mensuration filtrate obtains adsorbent and can reach more than 90% the eliminating rate of absorption of the methylene blue under this concentration.Through behind seven absorption regenerations, adsorbent still can reach more than 90% the adsorption rate of the methylene blue under this concentration.
Claims (9)
1. polypyrrole/titanium dioxide compound adsorbent is characterized in that the sorbent molecule formula that is polymerized by TiO 2 sol and oxidizable pyrrole is:
It utilizes the absorption principle dye wastewater treatment using, and adsorbable dyestuff comprises one or more the mixture in acid dyes, the basic-dyeable fibre; Its preparation method may further comprise the steps:
(1) volume ratio in titanium source and alcohol is 0.1～25 ratio, titanium source and alcohol is mixed with the alcoholic solution of titaniferous; Under vigorous stirring, with the described alcoholic solution that obtains be added drop-wise to slowly that pH is 0.5～6.0, temperature is hydrolysis in 0～100 ℃ the salpeter solution, keeping the volume ratio of water in titanium source and the aqueous acid is 1: 0.1～60, and stir 3～24h at normal temperatures, can obtain transparent or semitransparent TiO 2 sol;
(2) under-20～80 ℃, the ratio that the TiO 2 sol and the pyrrole monomer of gained with the mol ratio is 1:0.05～50 is mixed mutually, adopt chemical oxidization method to realize oxidation polymerization, and the mol ratio of oxidant and pyrrole monomer is 1:0.1～3, and more than-20～80 ℃ of following sustained response 20h, filtration drying get final product polypyrrole composite titanium dioxide adsorbent.
2. polypyrrole according to claim 1/titanium dioxide compound adsorbent is characterized in that described titanium source is one or more the mixture in titanium tetrachloride, tetrabutyl titanate, isopropyl titanate, the metatitanic acid methyl esters.
3. polypyrrole according to claim 1/titanium dioxide compound adsorbent is characterized in that described alcohol is one or more mixtures in normal propyl alcohol, isopropyl alcohol, absolute ethyl alcohol, methyl alcohol, butanols, the tert-butyl alcohol.
4. polypyrrole according to claim 1/titanium dioxide compound adsorbent is characterized in that the used oxidant of oxidation polymerization is one or more mixtures in iron chloride, ammonium persulfate, potassium peroxydisulfate, the potassium permanganate.
5. polypyrrole according to claim 1/titanium dioxide compound adsorbent, it is characterized in that concrete technique for applying step is: described polypyrrole/titanium dioxide adsorbent was soaked 1～120 minute with acid or alkali, add then and contain in the sewage of dyestuff, the quantity of sorbent that adds is 1/100～1/500 of a sewage weight, adsorption temp is a normal temperature, adsorption time is 30～90 minutes, after the absorption adsorbent is separated the back with waste water from dyestuff and regenerates.
6. the renovation process of polypyrrole according to claim 1/titanium dioxide compound adsorbent is characterized in that, can use alkali, acid or both and usefulness to soak the desorption of 1～120 minute realization dyestuff and the regeneration of adsorbent behind the described adsorbents adsorb dyestuff.
7. renovation process according to claim 6 is characterized in that, the desorption of dyestuff and the regenerative process of adsorbent can realize in position, also can realize in dystopy.
8. according to the described renovation process of claim 6, it is characterized in that the used alkali of regenerating is one or more mixtures in NaOH, potassium hydroxide, calcium hydroxide, lithium hydroxide, barium hydroxide, the ammoniacal liquor; Used acid is one or more the mixture in nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid, formic acid, acetate, hydrofluoric acid, the benzoic acid.
9. renovation process according to claim 6 is characterized in that, the concentration range of the alkali that regeneration is used is 0.01～15mol L
-1, the concentration range of acid is 0.01～15mol L
-1
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