CN104772120A - Visible photocatalysis renewable graphene-based hydrogel adsorbent, and preparation method and application thereof - Google Patents
Visible photocatalysis renewable graphene-based hydrogel adsorbent, and preparation method and application thereof Download PDFInfo
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- CN104772120A CN104772120A CN201510134734.3A CN201510134734A CN104772120A CN 104772120 A CN104772120 A CN 104772120A CN 201510134734 A CN201510134734 A CN 201510134734A CN 104772120 A CN104772120 A CN 104772120A
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Abstract
The invention discloses a silver phosphate supported graphene-based hydrogel adsorbent, and a preparation method and an application thereof. The method comprises the following steps: carrying out ultrasonic peeling on an aqueous graphene oxide solution, adding glutathione, maintaining the above obtained glutathione-containing graphene solution under sealing conditions at 80DEG C for 12h to obtain a glutathione-containing graphene-based hydrogel, immersing the glutathione-containing graphene-based hydrogel in distilled water to remove residual glutathione, adding an aqueous AgNO3 solution into the glutathione-containing graphene-based hydrogel, and reacting to obtain an Ag ion supported hydrogel; and adding an aqueous NaH2PO4 solution, and reacting to obtain the silver phosphate supported graphene-based hydrogel adsorbent which can be used for treatment of methyl orange-containing dye wastewater. The adsorbent has greatly larger methyl orange adsorption ability than graphene, and can be recycled through photocatalysis regeneration after use. The methyl orange adsorption ability of the adsorbent used three times still reaches 405.316-514.553mg/g.
Description
Technical field
The present invention relates to nano material and technical field of environmental science, graphene-based hydrogel adsorbent particularly relating to a kind of load silver orthophosphate and its preparation method and application.
Background technology
The waste water that dyestuff produces in its preparation and use procedure contains the bio-toxicity of multiple difficult degradation.Along with chemical industry, papermaking, the developing rapidly of printing and dyeing industry, the pollution of waste water from dyestuff is day by day serious.Wherein azo dyes is more common one, azo dyes is that after diazotising, activated methylene compound, phenols, aromatic amine coupling form aromatic amine with tool mostly, its stable chemical nature, biological degradability is low, easily accumulates in the environment and then works the mischief to human body and the whole ecosystem.Azo dye wastewater biodegradability is poor, colourity is high, complicated, and the azo dyes being easily decomposed into carcinogenicity aromatic amine is under the reducing conditions disabled in developed country.There is no cost-effective method for treating water both at home and abroad at present, this also result in the high residue of azo dyes in process waste water, causes strong interest and the worry of people.How effectively to process it, receive the concern of researcher always, its research has important social benefit.And methyl orange is as typical azo dyes, and structure is simple, thus is often used to dye wastewater.
Graphene graphite flake is peeled off into the single-layered carbon nanotube material only having a carbon atom thickness (about 0.335 nm), has bi-dimensional cellular shape lattice structure.Since report in 2004, Graphene is widely used at numerous areas with the physics of its excellence, chemical property, thus becomes the focus that scientific research personnel competitively studies.Graphene has the particular advantages such as high-specific surface area, high conductivity, good thermal conductivity and structure-controllable, and it can be used to remove the pollutant in environment water as potential effective sorbing material.It also has gel characteristic, can form graphene-based hydrogel under certain condition.Hydrogel is decentralized medium primarily of water, the inner water-soluble three-dimensional network structuring polymer gel containing hydrophilic radical.
Graphene hydrogel can be absorption and provides more avtive spot, and overcomes that nano-powder adsorbent is easily reunited, not segregative difficult problem, is a kind of desirable sorbing material.
Summary of the invention
An object of the present invention is the Graphene hydrogel adsorbent in order to provide a kind of adsorption capacity to be better than a kind of load silver orthophosphate of Graphene hydrogel.The Graphene hydrogel adsorbent of this load silver orthophosphate has given full play to the physicochemical characteristics of Graphene hydrogel, and owing to containing AgPO in the Graphene hydrogel adsorbent of the load silver orthophosphate of gained
4, it has better absorption property to methyl orange.And owing to containing AgPO in the Graphene hydrogel adsorbent of load silver orthophosphate
4, there is good adsorption photochemical catalysis characteristic, thus can repetitive cycling recycling.
Two of object of the present invention is to provide the preparation method of the Graphene hydrogel adsorbent of above-mentioned a kind of load silver orthophosphate.
Three of object of the present invention the graphene-based hydrogel adsorbent of above-mentioned load silver orthophosphate is used for the process to the waste water from dyestuff containing methyl orange.
Technical scheme of the present invention
A graphene-based hydrogel adsorbent for load silver orthophosphate, is prepared by a method comprising the following steps and forms:
(1), graphite oxide is joined in deionized water, obtain the graphite oxide aqueous solution that concentration is 2mg/mL, control ultrasonic temperature under sealed environment to be no more than 25 DEG C and to carry out ultrasonic 2h, then glutathione is added, and use glass bar stirring and dissolving, control ultrasonic temperature to be more in a sealed meter environment no more than 25 DEG C and to carry out ultrasonic 15min, obtain glutathione graphene solution;
The addition of glutathione, calculates in mass ratio, graphite oxide: glutathione is 2:1;
(2), by the glutathione graphene solution that obtains under sealed conditions, temperature controlled water baths is 80 DEG C and keeps 12h, forms hydrogel, then takes out hydrogel with tweezers and uses distilled water immersion 1d instead, repeatedly change water, till bubbling out wherein residual glutathione;
(3), in the hydrogel, in step (2) obtained, add by each hydrogel the AgNO that 3ml concentration is 0.6M
3the aqueous solution, adds the AgNO of 0.6M in hydrogel
3take out after shaking 12h after the aqueous solution, use distilled water immersion 30min, obtain the hydrogel of loaded Ag ion;
Then, then by each hydrogel add the NaH that 3ml concentration is 0.2M
2pO
4the aqueous solution, adds the NaH of 0.2M in the hydrogel of loaded Ag ion obtained above
2pO
4take out after aqueous solution concussion 12h, dewater with after distilled water immersion 30min, obtain the hydrogel adsorbent of load silver orthophosphate.
The Graphene hydrogel adsorbent of above-mentioned load silver orthophosphate, because the π-π between Graphene and organic dyestuff interacts, therefore it may be used for the absorption to methyl orange, and its adsorption capacity increases substantially compared with the Graphene hydrogel of non-load silver orthophosphate, refers to Application Example 1.
After the Graphene hydrogel adsorbent use of above-mentioned load silver orthophosphate, regeneration cycle can use after white light or ultra violet lamp, concrete steps are as follows:
30min is soaked with the Graphene hydrogel adsorbent of deionized water to the load silver orthophosphate after absorption methyl orange, then distilled water is put into after taking out the Graphene hydrogel adsorbent of the load silver orthophosphate after absorption methyl orange, after the white light of 500W or ultra violet lamp 90min, namely complete the regeneration process of the Graphene hydrogel adsorbent of the load silver orthophosphate after absorption methyl orange, can be recycled after process.After recycling 3 times, it still can reach the graphene-based hydrogel adsorbent of 405.316-514.553mg methyl orange/g load silver orthophosphate to the adsorption capacity of methyl orange.
Beneficial effect of the present invention
The graphene-based hydrogel adsorbent of a kind of load silver orthophosphate of the present invention, its specific area is large, and the active adsorption sites on surface is many, when the waste water from dyestuff therefore used it for containing methyl orange carries out adsorption treatment, can substantially increase its absorption property to methyl orange.
The preparation method of the Graphene hydrogel adsorbent of load silver orthophosphate of the present invention, owing to adopting Graphene three-dimensional macro body system-hydrogel in preparation process, be applied to the efficient removal of pollutant in waste water from dyestuff, solve nano adsorber easily to reunite, not segregative difficult problem, and make full use of the high chemically active peculiar property of Graphene high-ratio surface sum.
Further, the preparation method of the Graphene hydrogel adsorbent of load silver orthophosphate of the present invention, preparation process is simple, can large-scale mass production, and this sorbing material can recycle through Photocatalytic Regeneration.
Detailed description of the invention
Be further illustrate of the present invention below by embodiment, instead of limit the scope of the invention.
embodiment 1
A preparation method for the Graphene hydrogel adsorbent of load silver orthophosphate, specifically comprises the steps:
(1), 1000mg graphite oxide is joined in 500ml volumetric flask, obtain the graphite oxide aqueous solution that concentration is 2mg/mL, control ultrasonic temperature under sealed environment to be no more than 25 DEG C and to carry out ultrasonic 2h, then 500mg glutathione is added, and use glass bar stirring and dissolving, control ultrasonic temperature to be more in a sealed meter environment no more than 25 DEG C and to carry out ultrasonic 15min, obtain glutathione graphene solution;
The addition of glutathione, calculates in mass ratio, graphite oxide: glutathione is 2:1;
(2), by the glutathione graphene solution of step (1) gained under sealed conditions, temperature controlled water baths is after 80 DEG C of maintenance 12h, then take out with tweezers the hydrogel formed and use distilled water immersion 1d instead, repeatedly change water, bubble out wherein residual glutathione;
(3), first, by 3ml concentration be the AgNO of 0.6M
3the aqueous solution joins in each hydrogel that step (3) obtains, and takes out, use distilled water immersion 30min after putting into shaking table concussion 12h;
Then in each hydrogel, add 3ml concentration be 0.2MNaH then,
2pO
4the aqueous solution, takes out after putting into shaking table concussion 12h, dewaters, obtain the hydrogel adsorbent of load silver orthophosphate with after distilled water immersion 30min.
comparative examples 1
The preparation method of the Graphene hydrogel adsorbent of non-load silver orthophosphate, specifically comprises the steps:
(1), 1000mg graphite oxide is joined in 500ml volumetric flask, obtain the graphite oxide solution that concentration is 2mg/mL, control ultrasonic temperature under sealed environment to be no more than 25 DEG C and to carry out ultrasonic 2h, then 500mg glutathione is added, and use glass bar stirring and dissolving, control ultrasonic temperature to be more in a sealed meter environment no more than 25 DEG C and to carry out ultrasonic 15min, obtain graphene solution;
The addition of glutathione, calculates in mass ratio, graphite oxide: glutathione is 2:1;
(2), by the graphene solution of step (1) gained under sealed conditions, temperature controlled water baths is after 80 DEG C of maintenance 12h, then take out hydrogel with tweezers and use distilled water immersion 1d instead, repeatedly change water, bubble out wherein residual glutathione, obtain the Graphene hydrogel adsorbent of non-load silver orthophosphate.
application Example 1
Every part of 240mg, be that the methyl orange aqueous solution of 10mg/L, 20mg/L, 30mg/L, 40mg/L, 50mg/L, 60mg/L, 70mg/L, 80mg/L, 90mg/L, 100mg/L is mixed in conical flask respectively with 20ml concentration by the Graphene hydrogel adsorbent of 10 parts of embodiment 1 gained load silver orthophosphates, be placed in 25 DEG C of shaking tables at the uniform velocity to shake, every rapid disposable syringe at regular intervals extracts 10ml liquid, and fall impurity with filtering with microporous membrane, filtrate adopts spectrophotometer to measure its absorbance at its maximum absorption wavelength 465nm place.
Experimental result shows, the Graphene hydrogel adsorbent of the load silver orthophosphate of gained of the present invention is to the adsorption capacity of methyl orange, and namely the Graphene hydrogel adsorbent of every gram of load silver orthophosphate is 664.598mg to the adsorption capacity of methyl orange;
And the Graphene hydrogel of the non-load silver orthophosphate of gained in comparative examples 1, under similarity condition, namely the adsorption capacity of Graphene hydrogel absorbent particles to methyl orange of every gram of non-load silver orthophosphate is only 153.324mg.
The above results shows that the Graphene hydrogel adsorbent of load silver orthophosphate is compared with the Graphene hydrogel of non-load silver orthophosphate, and the Graphene hydrogel adsorbent of load silver orthophosphate, due to the load of silver orthophosphate, it adds about 5 times to the adsorption capacity of methyl orange.
embodiment 2
A preparation method for the graphene-based hydrogel adsorbent of load silver orthophosphate, specifically comprises the steps:
(1), 500mg graphite oxide is joined in 250ml volumetric flask, obtain the graphite oxide aqueous solution that concentration is 2mg/mL, control ultrasonic temperature under sealed environment to be no more than 25 DEG C and to carry out ultrasonic 2h, then 250mg glutathione is added, and use glass bar stirring and dissolving, control ultrasonic temperature to be more in a sealed meter environment no more than 25 DEG C and to carry out ultrasonic 15min, obtain glutathione graphene solution;
The addition of glutathione, calculates in mass ratio, graphite oxide: glutathione is 2:1;
(2), by the glutathione graphene solution of step (1) gained under sealed conditions, temperature controlled water baths is after 80 DEG C of maintenance 12h, then take out with tweezers the hydrogel prepared and use distilled water immersion 1d instead, repeatedly change water, bubble out wherein residual glutathione;
(3), first, by 3ml concentration be the AgNO of 0.6M
3the aqueous solution joins in each hydrogel that step (3) obtains, and takes out, use distilled water immersion 30min after putting into shaking table concussion 12h;
Then in each hydrogel, add 3ml concentration be 0.2MNaH then,
2pO
4the aqueous solution, takes out after putting into shaking table concussion 12h, dewaters, obtain the Graphene hydrogel adsorbent of load silver orthophosphate with after distilled water immersion 30min.
application Example 2
The application of graphene-based hydrogel adsorbent in absorption methyl orange of the load silver orthophosphate of embodiment 2 gained, step is as follows:
(1), every part of 240mg, get the Graphene hydrogel absorbent particles of the load silver orthophosphate of 6 parts of embodiment 2 gained, adding 20ml concentration in every part is respectively in the methyl orange aqueous solution of 100mg/L, number consecutively 1-6, put into 25 DEG C of constant-temperature tables, take out after at the uniform velocity shaking 24h, 10ml liquid is extracted with disposable syringe, and with filtering with microporous membrane, filtrate adopts spectrophotometer to measure its absorbance at its maximum absorption wavelength 465nm place, calculate adsorption capacity, namely the Graphene hydrogel absorbent particles absorption methyl orange of every gram of load silver orthophosphate is respectively 658.219 mg, 662.574 mg, 660.125 mg, 662.417mg, 663.521mg, 660.528mg,
(2), by the graphene-based hydrogel adsorbent of 6 parts of absorption methyl orange back loading silver orthophosphates in step (1) regenerate, concrete steps are as follows:
Respectively 30min is soaked to the Graphene hydrogel absorbent particles of 6 parts of absorption methyl orange back loading silver orthophosphates by deionized water, then clean ampoule is put into after taking out the Graphene hydrogel absorbent particles of 6 parts of absorption methyl orange back loading silver orthophosphates respectively, every part adds 10ml distilled water, corresponding original serial number 1-6;
The white light of 1-3 sample 500W is irradiated 90min, by the irradiation 90min of 4-6 sample with 500W uviol lamp, namely completes the regeneration of the Graphene hydrogel absorbent particles of absorption methyl orange back loading silver orthophosphate;
(3), the Graphene hydrogel absorbent particles of 6 parts of load silver orthophosphates after regeneration process in step (2), use distilled water flushing respectively, then clean ampoule is put into successively, the methyl orange solution that 20ml concentration is 100mg/L is added respectively in the Graphene hydrogel absorbent particles of every part of load silver orthophosphate after regeneration process, put into 25 DEG C of constant-temperature tables, take out after at the uniform velocity shaking 24h, 10ml liquid is extracted with disposable syringe, and with filtering with microporous membrane, filtrate adopts spectrophotometer to measure its absorbance at its maximum absorption wavelength 465nm place respectively,
Result shows, experiment draws the expendable adsorption capacity of Graphene hydrogel sorbent circulation of No. 1-6 load silver orthophosphate regenerated, namely every gram of Graphene hydrogel absorbent particles absorption methyl orange recycling load silver orthophosphate is once respectively 642.514mg, 644.115mg, 635.521 mg; 608.342mg, 610.453mg, 605.617mg;
(4), step (1)-(3) 1 time is repeated;
Result shows, experiment show that the Graphene hydrogel sorbent circulation of No. 1-6 load silver orthophosphate regenerated uses the adsorption capacity of twice, namely every gram of Graphene hydrogel absorbent particles absorption methyl orange recycling the load silver orthophosphate of secondary is respectively 630.417mg, 638.104 mg, 633.215 mg, 528.733mg, 532.816mg, 526.424mg;
(4), step (1)-(3) 2 times are repeated;
Result shows, experiment show that the Graphene hydrogel sorbent circulation of No. 1-6 load silver orthophosphate regenerated uses the adsorption capacity of three times, namely every gram of Graphene hydrogel absorbent particles absorption methyl orange recycling the load silver orthophosphate of three times is respectively 509.246mg, 514.553 mg, 501.695 mg, 412.450mg, 413.112mg, 405.316mg.
The above results shows: along with the number of times recycled increases, the adsorption capacity of the graphene-based hydrogel adsorbent of load silver orthophosphate reduces to some extent, but changes not very big.Under same case, the effect of the Graphene hydrogel adsorbent of the load silver orthophosphate regenerated after the catalytic regeneration effect of the Graphene hydrogel of the load silver orthophosphate regenerated after white light is slightly better than UV-irradiation.
In sum, the Graphene hydrogel adsorbent of load silver orthophosphate of the present invention is through experiment test, the adsorption capacity of methyl orange is increased substantially relative to the Graphene hydrogel adsorbent of non-load silver orthophosphate, and through visible ray or UV-irradiation is renewable reuses after using.It is simple that its preparation method has preparation process, and condition is controlled, is suitable for large-scale mass production.
The above is only the citing of embodiments of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (4)
1. a preparation method for the graphene-based hydrogel adsorbent of load silver orthophosphate of visible light catalytic regeneration, is characterized in that specifically comprising the steps:
(1), graphite oxide is joined in deionized water, obtain the graphite oxide aqueous solution that concentration is 2mg/mL, under sealed environment, control temperature is no more than 25 DEG C and carries out ultrasonic 2h, then glutathione is added, stirring and dissolving, under sealed environment, control temperature 25 DEG C carries out ultrasonic 15min, obtains the graphene solution containing glutathione;
The addition of glutathione, calculates in mass ratio, graphite oxide: glutathione is 2:1;
(2) the glutathione graphene solution, step (1) obtained under sealed conditions, temperature controlled water baths is 80 DEG C and keeps 12h, obtain the hydrogel based hydrogel solution containing glutathione, then the hydrogel based hydrogel containing glutathione is taken out with tweezers, by the hydrogel based hydrogel distilled water immersion 1d containing glutathione taken out, repeatedly change water, the glutathione wherein remained is removed;
(3) what, in step (2) obtain contains in the hydrogel based hydrogel of glutathione, adds the AgNO that concentration is 0.6M
3the aqueous solution, concussion reaction 12h, obtains the hydrogel solution of loaded Ag ion, then takes out the hydrogel of loaded Ag ion, use distilled water immersion 30min;
Concentration is the AgNO of 0.6M
3the addition of the aqueous solution, the concentration added by each hydrogel based hydrogel containing glutathione is the AgNO of 0.6M
3the aqueous solution is that the ratio of 3ml calculates;
Then, then by the hydrogel of each loaded Ag ion add the NaH that 3ml concentration is 0.2M
2pO
4the amount of the aqueous solution, adds the NaH of 0.2M in the hydrogel of loaded Ag ion obtained above
2pO
4aqueous solution concussion reaction 12h, obtains the graphene-based hydrogel solution of load silver orthophosphate, takes out the graphene-based hydrogel of load silver orthophosphate, dewater, obtain the graphene-based hydrogel adsorbent of load silver orthophosphate with after distilled water immersion 30min.
2. the graphene-based hydrogel adsorbent of a kind of load silver orthophosphate of preparation method's gained as claimed in claim 1.
3. the graphene-based hydrogel adsorbent of a kind of load silver orthophosphate as claimed in claim 2 is used for processing the waste water from dyestuff containing methyl orange.
4. the graphene-based hydrogel adsorbent of a kind of load silver orthophosphate as claimed in claim 3 is used for the regeneration treating method after processing the waste water from dyestuff containing methyl orange, it is characterized in that step is as follows:
30min is soaked with the Graphene hydrogel adsorbent of deionized water to the load silver orthophosphate after absorption methyl orange, then distilled water is put into after taking out the Graphene hydrogel adsorbent of the load silver orthophosphate after absorption methyl orange, after the white light of 500W or ultra violet lamp 90min, namely complete the regeneration process of the Graphene hydrogel adsorbent of load silver orthophosphate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152158A (en) * | 2015-09-23 | 2015-12-16 | 同济大学 | Preparation method for three-dimensional graphene hydrogel electrode material and application thereof to capacitive deionization |
| CN112090398A (en) * | 2020-09-18 | 2020-12-18 | 纳琦绿能工程有限公司 | Photocatalytic adsorbent, preparation method thereof and application thereof in sewage treatment |
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| CN102350335A (en) * | 2011-08-10 | 2012-02-15 | 东华大学 | Method for preparing nanometer titanium dioxide/graphene composite hydrogel at room temperature |
| US20130230496A1 (en) * | 2012-02-23 | 2013-09-05 | Subhra Mohapatra | Graphene hydrogel and method for using the same |
| CN103537307A (en) * | 2012-07-16 | 2014-01-29 | 中国科学院理化技术研究所 | Graphene-silver phosphate composite photocatalyst and preparation method and application thereof |
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- 2015-03-25 CN CN201510134734.3A patent/CN104772120A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350335A (en) * | 2011-08-10 | 2012-02-15 | 东华大学 | Method for preparing nanometer titanium dioxide/graphene composite hydrogel at room temperature |
| US20130230496A1 (en) * | 2012-02-23 | 2013-09-05 | Subhra Mohapatra | Graphene hydrogel and method for using the same |
| CN103537307A (en) * | 2012-07-16 | 2014-01-29 | 中国科学院理化技术研究所 | Graphene-silver phosphate composite photocatalyst and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152158A (en) * | 2015-09-23 | 2015-12-16 | 同济大学 | Preparation method for three-dimensional graphene hydrogel electrode material and application thereof to capacitive deionization |
| CN112090398A (en) * | 2020-09-18 | 2020-12-18 | 纳琦绿能工程有限公司 | Photocatalytic adsorbent, preparation method thereof and application thereof in sewage treatment |
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