CN103464122B - A kind of preparation method of graphene/chitosan adsorbent resin - Google Patents
A kind of preparation method of graphene/chitosan adsorbent resin Download PDFInfo
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- CN103464122B CN103464122B CN201310434322.2A CN201310434322A CN103464122B CN 103464122 B CN103464122 B CN 103464122B CN 201310434322 A CN201310434322 A CN 201310434322A CN 103464122 B CN103464122 B CN 103464122B
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 69
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 62
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000003463 adsorbent Substances 0.000 title claims abstract description 11
- 239000011347 resin Substances 0.000 title claims abstract description 11
- 229920005989 resin Polymers 0.000 title claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 78
- 239000000243 solution Substances 0.000 claims abstract description 49
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011259 mixed solution Substances 0.000 claims abstract description 24
- 239000000805 composite resin Substances 0.000 claims abstract description 21
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 16
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 10
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 239000002105 nanoparticle Substances 0.000 claims abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 36
- 239000010936 titanium Substances 0.000 claims description 36
- 229910052719 titanium Inorganic materials 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 abstract description 20
- 239000000975 dye Substances 0.000 abstract description 17
- 238000004043 dyeing Methods 0.000 abstract description 11
- 238000010521 absorption reaction Methods 0.000 abstract description 9
- 238000001179 sorption measurement Methods 0.000 abstract description 8
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005304 joining Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
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- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention provides the preparation method of a kind of graphene/chitosan adsorbent resin, is characterized in: joined by titanium dioxide nanoparticle in distilled water, disperses with high speed dispersor, obtains nano titanium oxide suspension;Take graphene oxide water solution, nano titanium oxide suspension is joined in graphene oxide solution, high-speed stirred mix homogeneously;Prepare chitosan solution with dilute acetic acid solution, titanium dioxide graphene oxide mixed solution is added in chitosan solution, after high-speed stirred, obtain titanium dioxide graphene oxide chitosan mixed solution;Preparation glutaraldehyde solution, it is added in titanium dioxide graphene oxide chitosan mixed solution, cross-link 14 hours under the conditions of 60 100 DEG C after mix homogeneously, dry at temperature is 90 DEG C, pulverized 200 mesh sieves and obtain titanium dioxide Graphene chitosan composite resin particle.Dyestuff in energy catalytic degradation and absorption dyeing waste water, and high adsorption capacity, absorption stability are good.
Description
Technical field
The invention belongs to photocatalytic degradation technical field of material, be specifically related to the preparation method of a kind of graphene/chitosan adsorbent resin, the degraded of dyestuff and absorption in organic dye waste water.
Background technology
Dyeing is always the main industries of China's industrial wastewater discharge, no matter for which type of dyeing waste water, mainly has following feature: (1) water yield is big;(2) concentration is high;(3) variation water quality is big;(4) based on Organic Pollution;(5) intractability is bigger;(6) effluent part contains noxious substance.In recent years, along with the fast development of chemical fibre so that the composition of the most intractable dyeing waste water becomes more complicated, intractability increases.Seek the efficient treatment of dyeing wastewater material treatment for reuse to the waste water that printing and dyeing industry is discharged, always make home and abroad environment engineering circles problem demanding prompt solution.
Because of TiO2Have that oxidability is strong, degraded completely and the advantage such as can reuse, and stable chemical nature, resistance to acids and bases are good, low cost, environmentally safe, and the aspect such as preparation in sewage disposal, cleaning material receives much concern always.But TiO2Band gap about 3.2eV, could can only show photochemical activity by the shorter ultraviolet excitation of wavelength in the wavelength ultra-violet (UV) band less than 378 nm, this utilization is only had 4% the sunlight of ultraviolet light content totally unfavorable.It addition, its light induced electron and hole-recombination rate are higher, photo-quantum efficiency is low, reduces its photocatalysis efficiency.Therefore, TiO is improved2Photocatalytic activity is the study hotspot studying its photocatalysis technology field.
Graphene is a kind of New Type of Carbon nanometer light material, has the monoatomic layer two dimensional crystal structure of uniqueness, has bigger specific surface area and stronger electronic transmission performance, absorption, heat-transfer matcrial preparation in terms of be widely studied.By Graphene and TiO2The employing sol-gel processes such as carrying out compound catalysis material of preparing also is the focus that recent people study, as newborn in Geng Jingyi, Zhu of University Of Suzhou are prepared for TiO2-Graphene photo-catalyst, result shows, the introducing of Graphene improves TiO2Photocatalytic activity.Deng Lingjuan etc. are with graphite oxide and TiO2For predecessor, being prepared for titanium dioxide-graphene complex, methylene blue solution simulated wastewater carries out degraded absorption research, result shows: the photocatalysis performance of this complex is than pure TiO2Improve a lot.
Chitosan has good absorption and chelation to many dye molecules and heavy metal ion, is widely used in terms of water process, chemical industry and environmental protection.
How to design a kind of reasonably composite resin, the advantage of collection titanium dioxide, chitosan and Graphene and one, utilize the effective synergism between three, can have and effectively degrade the Organic substance that dyeing waste water and other compositions are complex and adsorb, this is technical task the most urgently to be resolved hurrily.
Summary of the invention
The present invention solves the problem that prior art exists, it is provided that the preparation method of a kind of graphene/chitosan adsorbent resin, dyestuff in energy catalytic degradation and absorption dyeing waste water, and high adsorption capacity, absorption stability are good, recycling rate of waterused is high.
It is an object of the invention to be achieved through the following technical solutions: the preparation method of a kind of graphene/chitosan adsorbent resin, it is characterised in that: preparation method comprises the following steps:
(1) a certain amount of nanometer anatase titania granule is joined in a certain amount of distilled water, carry out high speed dispersion with high speed dispersor, obtain finely dispersed nano titanium oxide suspension;
(2) take a certain amount of graphene oxide water solution, while stirring scattered nano titanium oxide suspension is joined in graphene oxide solution, high-speed stirred mix homogeneously;
(3) prepare certain density chitosan solution with dilute acetic acid solution, titanium dioxide-graphene oxide mixed solution is slowly added drop-wise in chitosan solution, after high-speed stirred, obtains titanium dioxide-graphene oxide-chitosan mixed solution;Wherein the content of graphene oxide is 1%-30%, and the content of titanium dioxide is 2%-5%;
(4) compound concentration is the glutaraldehyde solution of 3.5%, it is added drop-wise to while stirring in titanium dioxide-graphene oxide-chitosan mixed solution, cross-link 1-4 hour under the conditions of 60-100 DEG C after mix homogeneously, dry at temperature is 90 DEG C, pulverized 200 mesh sieves and obtain titanium dioxide-Graphene-chitosan composite resin particle.
Improvement to technique scheme: in described step (1), rotating speed when utilizing high speed dispersor dispersion titanium dioxide nanoparticle is 6000rpm.
Further improvement to technique scheme: in described step (2), the concentration of graphene oxide used is 2%-5%.
Further improvement to technique scheme: in described step (3), the concentration of acetic acid used during preparation chitosan solution is 2%, and the chitosan concentration of preparation is 2%.
The present invention compared with prior art has many advantages and a good effect:
1, titanium dioxide-Graphene-chitosan composite resin prepared by the present invention, the advantage of collection titanium dioxide, chitosan and Graphene and one, utilize the effective synergism between three, good to degradation efficiency height, the absorption property of dyestuff, stability is strong, and the advantages such as recycling rate of waterused is high are inhaled in desorbing again.
2, preparation technology of the present invention is simple, reaction condition is gentle, is suitable for large-scale production.
Detailed description of the invention
Below in conjunction with concrete embodiment, the present invention is described further.
The detailed description of the invention of the preparation method of a kind of graphene/chitosan adsorbent resin of the present invention, comprises the following steps:
(1) a certain amount of nanometer anatase titania granule is joined in a certain amount of distilled water, carry out high speed dispersion with high speed dispersor, obtain finely dispersed nano titanium oxide suspension;
(2) take a certain amount of graphene oxide water solution, while stirring scattered nano titanium oxide suspension is joined in graphene oxide solution, high-speed stirred mix homogeneously;
(3) prepare certain density chitosan solution with dilute acetic acid solution, titanium dioxide graphene oxide mixed solution is slowly added drop-wise in chitosan solution, after high-speed stirred, obtains titanium dioxide-graphene oxide-chitosan mixed solution;Wherein the content of graphene oxide is 1%-30%, and the content of titanium dioxide is 2%-5%;
(4) compound concentration is the glutaraldehyde solution of 3.5%, it is added drop-wise to while stirring in titanium dioxide-graphene oxide-chitosan mixed solution, cross-link 1-4 hour under the conditions of 60-100 DEG C after mix homogeneously, dry at temperature is 90 DEG C, pulverized 200 mesh sieves and obtain titanium dioxide-Graphene-chitosan composite resin particle.
The specific embodiment of the present invention is as follows:
Embodiment 1: the preparation method of a kind of graphene/chitosan adsorbent resin
1, the preparation of titanium dioxide-Graphene-chitosan mixed solution
Joining in a certain amount of distilled water by a certain amount of nanometer anatase titania granule (particle diameter is about 80nm), carry out high speed dispersion with high speed dispersor, rotating speed is 6000rpm, obtains finely dispersed nano titanium oxide suspension.Taking a certain amount of mass concentration is 2% graphene oxide water solution, joins in graphene oxide solution by scattered nano titanium oxide suspension while stirring, high-speed stirred mix homogeneously.It is the chitosan solution of 2% by the dilute acetic acid solution preparation mass concentration that mass concentration is 2%, titanium dioxide graphene oxide mixed solution is slowly added drop-wise in chitosan solution, titanium dioxide-graphene oxide-chitosan mixed solution is obtained after high-speed stirred, wherein the content of graphene oxide is 8%, and the content of titanium dioxide is 5%.
2, the preparation of titanium dioxide-Graphene-chitosan composite resin
Compound concentration is the glutaraldehyde solution of 3.5%, it is added drop-wise to while stirring in titanium dioxide-graphene oxide-chitosan mixed solution, cross-link 4 hours under the conditions of 60 DEG C after mix homogeneously, dry at temperature is 90 DEG C, pulverized 200 mesh sieves and obtain titanium dioxide-Graphene-chitosan composite resin particle.
The degraded to stimulated dye wastewater of the titanium dioxide-Graphene-chitosan composite resin of embodiment 1 and adsorption effect:
Under room temperature, take 0.03g titanium dioxide-Graphene-chitosan composite resin, add in the active red CL-5B stimulated dye wastewater that 25 milliliters of concentration is 80mg/L, while be irradiated with magnetic agitation limit ultraviolet light, irradiation condition is: light source distance 15cm, and light intensity is 20mW/cm2, wavelength is 365nm, timing when light source starts to irradiate, after 30min, takes the supernatant and utilizes the change of spectrophotometer detection Wastewater Dyes concentration.
Result shows, the titanium dioxide-Graphene-chitosan composite resin of the present embodiment 1 preparation reaches more than 93% to the degraded adsorption rate of dyestuff in the dyeing waste water of 80mg/L.
Embodiment 2: the preparation method of a kind of graphene/chitosan adsorbent resin
1, the preparation of titanium dioxide-Graphene-chitosan mixed solution
Joining in a certain amount of distilled water by a certain amount of nanometer anatase titania granule (particle diameter is about 80nm), carry out high speed dispersion with high speed dispersor, rotating speed is 6000rpm, obtains finely dispersed nano titanium oxide suspension.Taking a certain amount of mass concentration is 2% graphene oxide water solution, joins in graphene oxide solution by scattered nano titanium oxide suspension while stirring, high-speed stirred mix homogeneously.It is the chitosan solution of 2% by the dilute acetic acid solution preparation mass concentration that mass concentration is 2%, titanium dioxide graphene oxide mixed solution is slowly added drop-wise in chitosan solution, titanium dioxide-graphene oxide-chitosan mixed solution is obtained after high-speed stirred, wherein the content of graphene oxide is 19%, and the content of titanium dioxide is 3.5%.
2, the preparation of titanium dioxide-Graphene-chitosan composite resin
Compound concentration is the glutaraldehyde solution of 3.5%, it is added drop-wise to while stirring in titanium dioxide-graphene oxide-chitosan mixed solution, cross-link 2 hours under the conditions of 80 DEG C after mix homogeneously, dry at temperature is 90 DEG C, pulverized 200 mesh sieves and obtain titanium dioxide-Graphene-chitosan composite resin particle.
The degraded to stimulated dye wastewater of the titanium dioxide-Graphene-chitosan composite resin of embodiment 2 and adsorption effect:
Under room temperature, take 0.03g titanium dioxide-Graphene-chitosan composite resin, add in the active red CL-5B stimulated dye wastewater that 25 milliliters of concentration is 80mg/L, while be irradiated with magnetic agitation limit ultraviolet light, irradiation condition is: light source distance 15cm, and light intensity is 20mW/cm2, wavelength is 365nm, timing when light source starts to irradiate, after 30min, takes the supernatant and utilizes the change of spectrophotometer detection Wastewater Dyes concentration.
Result shows, the titanium dioxide-Graphene-chitosan composite resin of the present embodiment 2 preparation reaches more than 96% to the degraded adsorption rate of dyestuff in the dyeing waste water of 80mg/L.
Embodiment 3: the preparation method of a kind of graphene/chitosan adsorbent resin
1, the preparation of titanium dioxide-Graphene-chitosan mixed solution
Joining in a certain amount of distilled water by a certain amount of nanometer anatase titania granule (particle diameter is about 80nm), carry out high speed dispersion with high speed dispersor, rotating speed is 6000rpm, obtains finely dispersed nano titanium oxide suspension.Taking a certain amount of mass concentration is 2% graphene oxide water solution, joins in graphene oxide solution by scattered nano titanium oxide suspension while stirring, high-speed stirred mix homogeneously.It is the chitosan solution of 2% by the dilute acetic acid solution preparation mass concentration that mass concentration is 2%, titanium dioxide graphene oxide mixed solution is slowly added drop-wise in chitosan solution, titanium dioxide-graphene oxide-chitosan mixed solution is obtained after high-speed stirred, wherein the content of graphene oxide is 30%, and the content of titanium dioxide is 2%..
2, the preparation of titanium dioxide-Graphene-chitosan composite resin
Compound concentration is the glutaraldehyde solution of 3.5%, it is added drop-wise to while stirring in titanium dioxide based on chitosan/graphene oxide mixed solution, cross-link 1 hour under the conditions of 100 DEG C after mix homogeneously, dry at temperature is 90 DEG C, pulverized 200 mesh sieves and obtain titanium dioxide-Graphene-chitosan composite resin particle.
The degraded to stimulated dye wastewater of the titanium dioxide-Graphene-chitosan composite resin of embodiment 3 and adsorption effect:
Under room temperature, take 0.03g titanium dioxide-Graphene-chitosan composite resin, add in the active red CL-5B stimulated dye wastewater that 25 milliliters of concentration is 80mg/L, while be irradiated with magnetic agitation limit ultraviolet light, irradiation condition is: light source distance 15cm, and light intensity is 20mW/cm2, wavelength is 365nm, timing when light source starts to irradiate, after 30min, takes the supernatant and utilizes the change of spectrophotometer detection Wastewater Dyes concentration.
Result shows, titanium dioxide-Graphene-chitosan composite resin prepared by this programme reaches more than 98% to the degraded adsorption rate of dyestuff in the dyeing waste water of 80mg/L.
Above example is only in order to illustrate technical scheme, rather than is limited;Although the present invention being described in detail with reference to previous embodiment, for the person of ordinary skill of the art, still the technical scheme described in previous embodiment can be modified, or wherein portion of techniques feature is carried out equivalent;And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of claimed technical solution of the invention.
Claims (1)
1. the preparation method of a graphene/chitosan adsorbent resin, it is characterised in that: preparation method comprises the following steps:
(1) a certain amount of nanometer anatase titania granule is joined in a certain amount of distilled water, carry out high speed dispersion with high speed dispersor, obtain finely dispersed nano titanium oxide suspension;
(2) take a certain amount of graphene oxide water solution, while stirring scattered nano titanium oxide suspension is joined in graphene oxide solution, high-speed stirred mix homogeneously;
(3) prepare certain density chitosan solution with dilute acetic acid solution, titanium dioxide-graphene oxide mixed solution is slowly added drop-wise in chitosan solution, after high-speed stirred, obtains titanium dioxide-graphene oxide-chitosan mixed solution;Wherein the content of graphene oxide is 1%-30%, and the content of titanium dioxide is 2%-5%;
(4) compound concentration is the glutaraldehyde solution of 3.5%, it is added drop-wise to while stirring in titanium dioxide-graphene oxide-chitosan mixed solution, cross-link 1-4 hour under the conditions of 60-100 DEG C after mix homogeneously, dry at temperature is 90 DEG C, pulverized 200 mesh sieves and obtain titanium dioxide-Graphene-chitosan composite resin particle;
In described step (1), rotating speed when utilizing high speed dispersor dispersion titanium dioxide nanoparticle is 6000rpm;In described step (2), the mass concentration of graphene oxide used is 2%-5%;In described step (3), the mass concentration of acetic acid used during preparation chitosan solution is 2%, and the chitosan mass concentration of preparation is 2%.
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CN110862557B (en) * | 2019-11-25 | 2021-11-23 | 华南理工大学 | Cellulose/graphene oxide/titanium dioxide hydrogel applied to fields of photocatalysis and physical adsorption and preparation method thereof |
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CN102266787A (en) * | 2010-06-07 | 2011-12-07 | 付文甫 | Preparation method of novel noble-metal-free catalyst for photolysis of water to produce hydrogen |
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CN102553559A (en) * | 2010-12-08 | 2012-07-11 | 财团法人纺织产业综合研究所 | Graphene/nanometer titanium dioxide compound and preparation method thereof |
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CN102872848A (en) * | 2012-10-17 | 2013-01-16 | 东南大学 | Preparation method for adsorption enhanced graphene titanium dioxide nano-composite photocatalyst |
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