CN104874367B - Reproduction method of chitosan-TiO2 absorbent for treating acid dyes - Google Patents
Reproduction method of chitosan-TiO2 absorbent for treating acid dyes Download PDFInfo
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- CN104874367B CN104874367B CN201510333960.4A CN201510333960A CN104874367B CN 104874367 B CN104874367 B CN 104874367B CN 201510333960 A CN201510333960 A CN 201510333960A CN 104874367 B CN104874367 B CN 104874367B
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Abstract
The invention belongs to the technical field of reproduction of functional materials, and relates to a reproduction method of a chitosan-TiO2 absorbent for treating acid dyes. The method comprises the steps of adding ultra-pure water to a reaction container; regulating pH to be 1 to 5 through hydrochloric acid; adding hydrogen peroxide to obtain a reproduction treatment solution; feeding the chitosan-TiO2 absorbent absorbed with the acid dyes to the reproduction treatment solution; illuminating with visible light for 1.5 to 8 hours; separating out the illuminated chitosan-TiO2 absorbent; drying to obtain the reproduced chitosan-TiO2 absorbent. According to the method, the acid reproduction treatment solution is treated by illuminating with the visible light; the complete degrading of the absorbed acid dyes and the reproduction of the chitosan-TiO2 absorbent can be synchronously achieved under the acid condition; the utilization efficiency of light energy can be increased; the stability of a chemical structure of chitosan can be ensured; the use times of the chitosan-TiO2 absorbent can be increased; the treatment cost of acid dyes wastewater can be reduced.
Description
Technical field
The invention belongs to functional material technical field of regeneration, specifically, is related to a kind of shell for acid dyes process
Glycan-TiO2The renovation process of adsorbent.
Background technology
Dyestuff is widely used in the industrial circles such as weaving, light industry, chemical industry.According to statistics, the dyestuff that the whole world is used every year is big
700,000 ton is there are about, and therein 10%～15% is lost in processing and manufacturing and operation are processed, and is arranged in the form of industrial wastewater
Put into into environment.Can not only directly affect in aquatic ecological, and dye molecule more containing groups such as phenyl ring, azo, amidos, be in
Potential carcinogenicity, jeopardizes human health.That what is generally acknowledged at present administers the effective way of waste water from dyestuff is：First pass through physico-chemical process
Pretreatment decolouring is carried out, the dye molecule that bio-toxicity is big, colourity is high is removed, the biodegradability of waste water is improved；Then after passing through
Continuous biochemical treatment, the comprehensive regulation.Wherein, it is very crucial that the physical chemistry as waste water from dyestuff pretreatment is processed.Absorption, from
The physico-chemical processes such as sub- exchange, condensation-flocculation, advanced oxidation, UF membrane, electrochemistry be applied to it is dye decolored in.Compare
Under, the process flow of absorption method is big, effluent quality is preferable, investment cost is relatively low, simple to operate, in waste water from dyestuff actual treatment
In occupy larger specific gravity.
The selection of adsorbent is the key that dyestuff is removed.Shitosan (Chitosan) have absorption property height, aboundresources,
The features such as biocompatibility, biological degradability, obtain paying much attention to and widely studied in dye wastewater treatment field.Shitosan
Can be in forms such as powder, sheet, pearl, threadinesss as adsorbent application.Wherein, pearl shitosan is with its higher absorption
Capacity, it is easy to separate and recover, it is adaptable to the advantages of filling dress post batch processing is used, becomes chitosan-based adsorbent practical application
In preferred form.However, the essence of absorption is a kind of physics phase transition behavior, it means that adsorbed dye substance is not
Thoroughly decomposed, remained in the waste that adsorbent surface not only causes adsorbent, and easily secondary pollution is caused to environment.Cause
This, thoroughly removes adsorbed Dyes on Environment protection and reduction absorption cost is very important using effective method.
Shitosan is a kind of alkaline polysaccharide, and on its linear molecule chain a large amount of free amine groups are dispersed with, be Dye Adsorption most
Chief active group.At present to dyestuff, (particularly the anionic such as acid dyes, reactive dye contaminates well accepted shitosan
Material) adsorption mechanism be：In acid condition, the amino (- NH in chitosan molecule2) protonate：
Meanwhile, dye molecule dissolving, its sulfonic group dissociation makes dye molecule be in elecrtonegativity：
Finally, dye molecule is adsorbed on shitosan in the presence of electrostatic attraction：
From this mechanism as can be seen that solution in proton presence or acid solution to acid dyes on shitosan
Absorption is very important.Contrary, in alkaline solution, the amino on shitosan can occur deprotonation, shitosan and dye
Electrostatic attraction effect between material dies down, and the dye molecule for ultimately resulting in absorption is desorbed from shitosan：
-NH3 +-O3S-dye+OH-→-NH2+Dye-SO3Na
The principle that adsorbed dyestuff general at present is removed, i.e., under conditions of contrary with adsorption reaction, such as NaOH
Or the strong alkali solution such as sodium acid carbonate, adsorbed dyestuff desorption is made, realize the regeneration of chitosan absorbent.Although this method energy
Enough dyestuffs for removing absorption on shitosan surface, but the dyestuff of desorption is not still thoroughly decomposed, and still has potential two
Secondary pollution.
Nano titanium oxide (TiO2) used as a kind of emerging conductor photocatalysis material, its catalytic oxidation activity is higher,
And the degradable of organic matter is capable of achieving, there is fabulous application prospect in terms of the purified treatment of waste water from dyestuff.By nanometer
TiO2It is carried on shitosan sorbing material, it is possible to use TiO2Photocatalytic activity, realize the in-situ regeneration and adsorbed dye of carrier
The thorough degraded of material.Such as magazine RSC Advances, 2014, volume 4,5518-5523 page of " Self-regenerative
adsorbent based on the crosslinking chitosan for adsorbing and mineralizing
Azo dye " one are literary, it is disclosed can self-regeneration chitosan-based sorbing material, be exactly by nano-TiO2With Cross-linked shitosan
Combine the flake nano hybrid material being prepared from.After absorption, irradiate 30 minutes under ultraviolet light, you can realize adsorbent
Regeneration.But while there is also some shortcomings part：
(1) light source for using is ultraviolet light.Due to TiO2The greater band gap (being 3.2eV) of itself, general will be ultraviolet
Light is excited and lower could show catalysis activity.Ultraviolet light only accounts for 4% up to the solar energy on ground, using ultraviolet light to solar energy
Utilization ratio it is low, and artificial ultraviolet source has the shortcomings that power consumption big, apparatus expensive, stability are poor.Moreover, it is ultraviolet
Light can also destroy the chemical constitution of shitosan by photooxidation, make glycosidic bond break to form carbonyl, be unfavorable for acid dyes
Absorption.
(2) processed adsorbent is in flake.Due to sheet adsorbent system separate it is more difficult, it is difficult to reclaim repeat
Use, be not also suitable for packed column or batch adsorption treatment is used, thus it is in actual treatment and rarely needed.Moreover,
Laminar adsorbent, in its preparation process, although also have many nano-TiOs2In being wrapped in glycan substrate, to it
Photocatalytic activity causes certain negatively influencing, but most nano-TiO2Still it is exposed to glycan substrate surface, this point
Can be confirmed from SEM characterization result, therefore, with nano-TiO2Photocatalytic activity realize shitosan
The regeneration of adsorbent not difficult matter.But for beaded adsorbents commonly used in actual treatment, in its preparation process
In, most nano-TiO2In being wrapped in glycan substrate, photocatalytic activity becomes very faint.In this case,
Realize that the regeneration of chitosan absorbent is relatively difficult to achieve in illumination form merely.These limit to a certain extent it actually useless
Application in water process.Therefore, the regeneration that suitable method realizes pearl chitosan absorbent is developed, is to be badly in need of solving at present
Problem.
The content of the invention
It is an object of the invention to overcome prior art, seek a kind of adsorbed acid dye of realization in acid condition of design
Material is degradable, the shitosan-TiO for acid dyes process of adsorbent reactivation2The renovation process of adsorbent.
To achieve these goals, the technical solution used in the present invention is：It is a kind of for acid dyes process shitosan-
TiO2The renovation process of adsorbent, comprises the following steps：
Step 1：Prepare regeneration treatment fluid
In reaction vessel, ultra-pure water is added, and with salt acid for adjusting pH to 1～5, then ultra-pure water in mass ratio：Peroxidating
Hydrogen=100：(0.00005～0.0002) hydrogen peroxide is added, obtains regenerating treatment fluid；
Step 2：Photo-irradiation treatment
Shitosan-the TiO of acid dyes will be adsorbed with2Adsorbent is put in the regeneration treatment fluid that step 1 is obtained, it is seen that light
Illumination 1.5～8 hours；
Step 3：Separate drying
By the shitosan-TiO after photo-irradiation treatment in step 22Adsorbent is separated, and is put in baking oven and is dried, and is obtained again
Raw shitosan-TiO2Adsorbent.
Preferably, the shitosan-TiO2Adsorbent is (0.1-0.3) with the mass ratio of regeneration treatment fluid：100.
Preferably, the wave-length coverage of the visible ray is 420nm-760nm.
Preferably, drying temperature is 55-65 DEG C in the step 3.
Preferably, the shitosan-TiO2Adsorbent is pearl.
Pearl shitosan-TiO2The preparation method of adsorbent is comprised the following steps：
Step 1：Chitosan powder, acetum and shitosan are added in the acetum that mass concentration is 1%-3%
The mass ratio of powder is acetum：Chitosan powder=100：(1-5), while stirring, is completely dissolved to Chitosan powder, obtain
To uniform shitosan colloidal solution；
Step 2：Chitosan powder in mass ratio：TiO2Nano particle=(1-5)：(0.2-1), to shitosan colloidal solution
Middle addition TiO2Nano particle, after 30～60 minutes, stirred overnight is well mixed ultrasonic disperse, obtains shitosan-TiO2Mixing is molten
Liquid；
Step 3：Chitosan powder in mass ratio：Epoxychloropropane=(1-5)：(2.366～11.83), to shitosan-
TiO2Epoxychloropropane, the lower cross-linking reaction of stirring 10～60 minutes is added to obtain the shitosan-TiO being crosslinked in mixed solution2It is mixed
Close solution；
Step 4：Under stirring, to mass concentration for dropwise implantation step 3 is obtained in the sodium hydroxide solution of 0.4%-1%
Shitosan-the TiO of crosslinking2Mixed solution, obtains shitosan-TiO2Gelled pill；
Step 5：Collect shitosan-TiO2Gelled pill, bead surface is rinsed to neutrality with ultra-pure water repeatedly, is put into baking oven
Middle drying, obtains pearl shitosan-TiO2Adsorbent.
Preferably, drying temperature is 55-65 DEG C in the step 5.
Beneficial effects of the present invention are：
(1) with present adsorbed dyestuff desorption is made by strong alkali solution, realizes the regeneration of chitosan absorbent, desorption
Dyestuff is not thoroughly decomposed, and still be there is secondary pollution and is compared, and the method for the present invention passes through acid reclaim treatment fluid, using visible
Light photo-irradiation treatment, in acid condition, while realizing thorough degraded and the shitosan-TiO of adsorbed acid dyes2Adsorbent
Regeneration；
(2) photo-irradiation treatment is carried out using visible ray, improves the utilization ratio to solar energy, it is ensured that shitosan chemistry
The stability of structure, increased shitosan-TiO2The Reusability number of times of adsorbent；
(3) shitosan-TiO is realized2The regeneration of adsorbent, reduces the processing cost of Acid Dye Wastewater.
Description of the drawings
Fig. 1 is shitosan-TiO2Adsorbent is adsorbed with acid dyes, regeneration shitosan-TiO2Adsorbent, original preparation
Shitosan-TiO2The FTIR collection of illustrative plates comparison diagrams of adsorbent；
As shown in Figure 1：A () is adsorbed with the pearl shitosan-TiO of acid dyes2Adsorbent, the pearl shell of (b) regeneration gather
Sugar-TiO2Pearl shitosan-the TiO of adsorbent, (c) unadsorbed dyestuff2Adsorbent；
Fig. 2 is the UV-vis absorption spectrum comparison diagrams that acid dyes solution and regeneration process aftertreatment fluid；
As shown in Figure 2：Spectrum a is the UV-vis absorption spectrums of acid dyes；Spectrum b is that treatment fluid is regenerated after illumination
UV-vis absorption spectrums.
Specific embodiment
Below by specific embodiment, the invention will be further described：
Embodiment 1
Shitosan-the TiO for acid dyes process of the present embodiment2The renovation process of adsorbent, comprises the following steps：
Step 1：Prepare regeneration treatment fluid
In reaction vessel, ultra-pure water is added, and with salt acid for adjusting pH to 1, then ultra-pure water in mass ratio：Hydrogen peroxide=
100：0.00005 adds hydrogen peroxide, obtains regenerating treatment fluid；
Step 2：Photo-irradiation treatment
Shitosan-the TiO of acid dyes will be adsorbed with2Adsorbent is put in the regeneration treatment fluid that step 1 is obtained, it is seen that light
Illumination 1.5 hours；Shitosan-TiO2Adsorbent is (0.1-0.3) with the mass ratio of regeneration treatment fluid：100；The wavelength of visible ray
Scope is 420nm-760nm；
Step 3：Separate drying
By the shitosan-TiO after photo-irradiation treatment in step 22Adsorbent is separated, and is put in baking oven and is dried, and is obtained again
Raw shitosan-TiO2Adsorbent；Drying temperature is 55-65 DEG C.
Embodiment 2
Shitosan-the TiO for acid dyes process of the present embodiment2The renovation process of adsorbent, comprises the following steps：
Step 1：Prepare regeneration treatment fluid
In reaction vessel, ultra-pure water is added, and with salt acid for adjusting pH to 5, then ultra-pure water in mass ratio：Hydrogen peroxide=
100：0.0002 adds hydrogen peroxide, obtains regenerating treatment fluid；
Step 2：Photo-irradiation treatment
Shitosan-the TiO of acid dyes will be adsorbed with2Adsorbent is put in the regeneration treatment fluid that step 1 is obtained, it is seen that light
Illumination 8 hours；Shitosan-TiO2Adsorbent is (0.1-0.3) with the mass ratio of regeneration treatment fluid：100；The wavelength model of visible ray
Enclose for 420nm-760nm；
Step 3：Separate drying
By the shitosan-TiO after photo-irradiation treatment in step 22Adsorbent is separated, and is put in baking oven and is dried, and is obtained again
Raw shitosan-TiO2Adsorbent；Drying temperature is 55-65 DEG C.
Embodiment 3
Shitosan-the TiO for acid dyes process of the present embodiment2The renovation process of adsorbent, comprises the following steps：
Step 1：Prepare regeneration treatment fluid
In reaction vessel, ultra-pure water is added, and with salt acid for adjusting pH to 3, then ultra-pure water in mass ratio：Hydrogen peroxide=
100：0.0001 adds hydrogen peroxide, obtains regenerating treatment fluid；
Step 2：Photo-irradiation treatment
Pearl shitosan-the TiO of acid dyes will be adsorbed with2Adsorbent is put in the regeneration treatment fluid that step 1 is obtained, can
See light illumination 5 hours；Shitosan-TiO2Adsorbent is (0.1-0.3) with the mass ratio of regeneration treatment fluid：100；
Step 3：Separate drying
By the shitosan-TiO after photo-irradiation treatment in step 22Adsorbent is separated, and is put in baking oven and is dried, and is obtained again
Raw shitosan-TiO2Adsorbent；Drying temperature is 60 DEG C.
Pearl shitosan-TiO2The preparation method of adsorbent is comprised the following steps：
Step 1：Chitosan powder, acetum and shitosan are added in the acetum that mass concentration is 1%-3%
The mass ratio of powder is acetum：Chitosan powder=100：(1-5), while stirring, is completely dissolved to Chitosan powder, obtain
To uniform shitosan colloidal solution；
Step 2：Chitosan powder in mass ratio：TiO2Nano particle=(1-5)：(0.2-1), to shitosan colloidal solution
Middle addition TiO2Nano particle, after 30～60 minutes, stirred overnight is well mixed ultrasonic disperse, obtains shitosan-TiO2Mixing is molten
Liquid；
Step 3：Chitosan powder in mass ratio：Epoxychloropropane=(1-5)：(2.366～11.83), to shitosan-
TiO2Epoxychloropropane, the lower cross-linking reaction of stirring 10～60 minutes is added to obtain the shitosan-TiO being crosslinked in mixed solution2It is mixed
Close solution；
Step 4：Under stirring, to mass concentration for dropwise implantation step 3 is obtained in the sodium hydroxide solution of 0.4%-1%
Shitosan-the TiO of crosslinking2Mixed solution, obtains shitosan-TiO2Gelled pill；
Step 5：Collect shitosan-TiO2Gelled pill, bead surface is rinsed to neutrality with ultra-pure water repeatedly, is put into baking oven
Middle drying, obtains pearl shitosan-TiO2Adsorbent；Drying temperature is 55-65 DEG C.
It is to investigate pearl shitosan-TiO after regeneration is processed2Adsorbent surface and inside whether there is dyestuff, using in Fu
Leaf transformation infrared spectrometer (FTIR) is to pearl shitosan-TiO2The functional group of adsorbent surface and inside is characterized；
As shown in figure 1, (a) is adsorbed with the pearl shitosan-TiO of acid dyes2Adsorbent, the pearl shell of (b) regeneration gather
Sugar-TiO2Pearl shitosan-the TiO of adsorbent, (c) unadsorbed dyestuff2Adsorbent
Pearl shitosan-TiO2Before absorbing dye, spectrum c shows adsorbent, and the stretching vibration peak of its amino is in
3380cm-1Place；Because amino is Main Function site of the chitosan-based adsorbent to acid dyes, after absorption acid dyes,
Spectrum a shows that its amino stretching vibration peak is blue shifted to 3286cm-1Place；And after regeneration is processed, spectrum b shows its amino stretching vibration
Peak returns to 3380cm-1Place.This explanation, after regeneration is processed, the amino of adsorbent is no longer acted on dyestuff.Moreover, on spectrum a
3286cm-1Place's vibration peak is also related to dyestuff azo group, and this peak disappears on spectrum b and c.Analysis result shows,
After regeneration is processed, pearl shitosan-TiO2Adsorbent surface and internal no acidic dyestuff.
It is to prove in regeneration treatment fluid with the presence or absence of dyestuff, using UV-vis spectroscopy spectrometer (UV- after regeneration is processed
Vis) characterize to regenerating treatment fluid after illumination, as shown in Figure 2：Spectrum a is shown that the UV-vis of acid dyes absorbs light
Spectrum, it can be seen that dyestuff has a characteristic absorption peak at 509nm.And in spectrum b, this absworption peak disappears, illumination is illustrated
Afterwards, regenerate in treatment fluid without dyestuff residual.
Claims (7)
1. it is a kind of for acid dyes process shitosan-TiO2The renovation process of adsorbent, it is characterised in that：Including following step
Suddenly：
Step 1：Prepare regeneration treatment fluid
In reaction vessel, ultra-pure water is added, and with salt acid for adjusting pH to 1～5, then ultra-pure water in mass ratio：Hydrogen peroxide=
100：(0.00005～0.0002) hydrogen peroxide is added, obtains regenerating treatment fluid；
Step 2：Photo-irradiation treatment
Shitosan-the TiO of acid dyes will be adsorbed with2Adsorbent is put in the regeneration treatment fluid that step 1 is obtained, it is seen that light illumination
1.5～8 hours；
Step 3：Separate drying
By the shitosan-TiO after photo-irradiation treatment in step 22Adsorbent is separated, and is put in baking oven and is dried, and obtains the shell for regenerating
Glycan-TiO2Adsorbent.
2. it is according to claim 1 for acid dyes process shitosan-TiO2The renovation process of adsorbent, its feature
It is：Shitosan-the TiO2Adsorbent is (0.1-0.3) with the mass ratio of regeneration treatment fluid：100.
3. it is according to claim 1 for acid dyes process shitosan-TiO2The renovation process of adsorbent, its feature
It is：The wave-length coverage of the visible ray is 420nm-760nm.
4. it is according to claim 1 for acid dyes process shitosan-TiO2The renovation process of adsorbent, its feature
It is：Drying temperature is 55-65 DEG C in the step 3.
5. according to any one of claim 1-4 for acid dyes process shitosan-TiO2The regeneration side of adsorbent
Method, it is characterised in that：Shitosan-the TiO2Adsorbent is pearl.
6. it is according to claim 5 for acid dyes process shitosan-TiO2The renovation process of adsorbent, its feature
It is：Pearl shitosan-the TiO2The preparation method of adsorbent is comprised the following steps：
Step 1：Chitosan powder, acetum and Chitosan powder are added in the acetum that mass concentration is 1%-3%
Mass ratio be acetum：Chitosan powder=100：(1-5), while stirring, is completely dissolved to Chitosan powder, obtain
Even shitosan colloidal solution；
Step 2：Chitosan powder in mass ratio：TiO2Nano particle=(1-5)：(0.2-1), add in shitosan colloidal solution
Enter TiO2Nano particle, after 30～60 minutes, stirred overnight is well mixed ultrasonic disperse, obtains shitosan-TiO2Mixed solution；
Step 3：Chitosan powder in mass ratio：Epoxychloropropane=(1-5)：(2.366～11.83), to shitosan-TiO2It is mixed
Close and epoxychloropropane is added in solution, the lower cross-linking reaction of stirring 10～60 minutes obtains the shitosan-TiO being crosslinked2Mixing is molten
Liquid；
Step 4：Under stirring, the crosslinking that dropwise implantation step 3 is obtained in the sodium hydroxide solution that mass concentration is 0.4%-1%
Shitosan-TiO2Mixed solution, obtains shitosan-TiO2Gelled pill；
Step 5：Collect shitosan-TiO2Gelled pill, bead surface is rinsed to neutrality with ultra-pure water repeatedly, is put in baking oven and is dried
It is dry, obtain pearl shitosan-TiO2Adsorbent.
7. it is according to claim 6 for acid dyes process shitosan-TiO2The renovation process of adsorbent, its feature
It is：Drying temperature is 55-65 DEG C in the step 5.
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