CN108384049A - A kind of titanium dioxide-graphene composite sponge and its preparation method and application - Google Patents
A kind of titanium dioxide-graphene composite sponge and its preparation method and application Download PDFInfo
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- CN108384049A CN108384049A CN201810214454.7A CN201810214454A CN108384049A CN 108384049 A CN108384049 A CN 108384049A CN 201810214454 A CN201810214454 A CN 201810214454A CN 108384049 A CN108384049 A CN 108384049A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08J2361/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The present invention provides a kind of preparation methods of titanium dioxide graphene composite sponge, and water, graphene oxide and titanium dioxide are mixed, mixed liquor is obtained；The mixed liquor is mixed with reducing agent, obtains reaction solution；In the reaction solution by sponge impregnating, reduction reaction is carried out under air-proof condition, obtains titanium dioxide graphene composite sponge.Titanium dioxide graphene composite sponge provided by the invention avoids secondary pollution, and titanium dioxide and graphene will not fall off from sponge during use convenient for recycling, reusable.Embodiment the experimental results showed that, titanium dioxide graphene composite sponge photocatalysis efficiency provided by the invention is high, photocatalysis stability is good.
Description
Technical field
The present invention relates to photocatalysis technology fields, and in particular to a kind of titanium dioxide-graphene composite sponge and its preparation
Methods and applications.
Background technology
With the rapid development of industrial production with the aggravation of mankind's destructive activity, water pollution problems becomes to be on the rise,
Significant impact is generated to human health, novel water pollution processing method is researched and developed and is of great significance.Titanium dioxide (TiO2) light
Catalysis technique is a kind of emerging water technology, has the advantages such as low energy consumption, easy to operate, reaction condition is mild.Meanwhile
TiO2Have many advantages, such as conductor photocatalysis material, such as chemical stability is good, at low cost, nontoxic, in environmental protection
It has a wide range of applications with energy field.But TiO2Energy gap is big (about 3.2eV), make its in use without
Method makes full use of solar energy, catalytic efficiency low；Meanwhile TiO2Granular size is nanoscale, is difficult to recycle after use, the day of one's doom
Its practical application in production and life is made.
Currently, solving the problems, such as this main method mainly by TiO2Directly and other materials, such as activated carbon, graphene
Etc. compound.TiO is loaded in activated carbon surface2Although catalytic efficiency can be made to increase, in use TiO2With activity
Charcoal combines insecure, is easy to fall off from activated carbon surface, and activated carbon contains certain impurity, and secondary dirt can be caused to water quality
Dye.Graphene has many advantages, such as that large specific surface area, electron-transport be fast, high mechanical strength, by TiO2It is compound with graphene so that
TiO2The absorption of visible light is greatly enhanced, while improving pollutant to a certain extent in TiO2The bioaccumulation efficiency on surface, into
And photocatalysis efficiency is improved, but recycle still highly difficult.
Invention content
The purpose of the present invention is to provide a kind of titanium dioxide-graphene composite sponges and its preparation method and application, originally
Titanium dioxide-graphene composite sponge that invention provides is convenient for recycling, and titanium dioxide and graphene will not be from during use
It falls off on sponge, it is reusable.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The present invention provides a kind of preparation methods of titanium dioxide-graphene composite sponge, include the following steps：
Water, graphene oxide and titanium dioxide are mixed, mixed liquor is obtained；
The mixed liquor is mixed with reducing agent, obtains reaction solution；
In the reaction solution by sponge impregnating, reduction reaction is carried out under air-proof condition, obtains titanium dioxide-graphene
Composite sponge.
Preferably, the concentration of graphene oxide and titanium dioxide stands alone as 0.1~10mg/mL in the mixed liquor.
Preferably, the reducing agent is hydrazine hydrate, ascorbic acid or ammonium hydroxide.
Preferably, a concentration of 0.4~0.65mg/mL of the hydrazine hydrate；Hydrazine and graphene oxide in the hydrazine hydrate
Mass ratio is (2~5)：11.
Preferably, the mass ratio of the ascorbic acid and graphene oxide is (1~3)：1.
Preferably, the ammon amount of the ammonium hydroxide is 25~28%；The volume ratio of the ammonium hydroxide and mixed liquor is 1：(10~
100)。
Preferably, the sponge is melamine sponge or polyurethane sponge.
Preferably, the temperature of the reduction reaction is 80~100 DEG C, and the time of reduction reaction is 0.5~10h.
The titanium dioxide being prepared the present invention provides preparation method described in above-mentioned technical proposal-graphene compounding sea
Silk floss, including sponge and the titanium dioxide and graphene that are supported on the sponge.
The present invention provides titanium dioxide described in above-mentioned technical proposal-graphene composite sponge answering in water pollution processing
With.
The present invention provides a kind of preparation methods of titanium dioxide-graphene composite sponge, by water, graphene oxide and two
Titanium oxide mixes, and obtains mixed liquor；The mixed liquor is mixed with reducing agent, obtains reaction solution；By sponge impregnating described anti-
It answers in liquid, reduction reaction is carried out under air-proof condition, obtain titanium dioxide-graphene composite sponge.Dioxy provided by the invention
Change titanium-graphene composite sponge convenient for recycling, avoids secondary pollution, and titanium dioxide and graphene will not be from seas during use
It falls off on silk floss, it is reusable.Embodiment the experimental results showed that, titanium dioxide provided by the invention-graphene composite sponge
Photocatalysis efficiency is high, photocatalysis stability is good.
In addition, the preparation method simple process and low cost of titanium dioxide provided by the invention-graphene composite sponge is honest and clean,
It can be applied in industrialized production.
Description of the drawings
Fig. 1 is the color contrast figure of sunlight pre-irradiation methylene blue solution；
Fig. 2 is the color contrast figure of methylene blue solution after sunlight irradiation；
Fig. 3 is SEM figure of the titanium dioxide-graphene composite sponge of the preparation of embodiment 1 before use；
Fig. 4 is the SEM figures of titanium dioxide-graphene composite sponge of the preparation of embodiment 1 after use.
Specific implementation mode
The present invention provides a kind of preparation methods of titanium dioxide-graphene composite sponge, include the following steps：
Water, graphene oxide and titanium dioxide are mixed, mixed liquor is obtained；
The mixed liquor is mixed with reducing agent, obtains reaction solution；
In the reaction solution by sponge impregnating, reduction reaction is carried out under air-proof condition, obtains titanium dioxide-graphene
Composite sponge.
The present invention mixes water, graphene oxide and titanium dioxide, obtains mixed liquor.In the present invention, the mixed liquor
The concentration of middle graphene oxide and titanium dioxide preferably stands alone as 0.1~10mg/mL, more preferably 0.5~6mg/mL, most preferably
For 1~3mg/mL.
The present invention does not have the source of the graphene oxide special restriction, use well known to those skilled in the art
The product that commercial goods or preparation method are prepared.
In the present invention, the granularity of the titanium dioxide is preferably 10~100nm, more preferably 30~70nm.In this hair
In bright, the titanium dioxide is preferably hydrophilic titanium oxide；Hydrophilic titanium oxide can be very good to be dispersed in water, and be easy to
Stable colloid is formed in water, and the uniformity of titanium dichloride load is may insure in sequential reduction reaction process.The present invention couple
There is no special restriction in the source of the titanium dioxide, using commercial goods well known to those skilled in the art.
In the present invention, the mixing of the water, graphene oxide and titanium dioxide is preferably first by water and graphene oxide
Mixing, obtains graphene oxide dispersion, then mixes the graphene oxide dispersion with titanium dioxide.In the present invention
In, the mixing of the graphene oxide dispersion and titanium dioxide preferably carries out under ultrasound condition, to ensure that material mixing is equal
It is even.In the present invention, the time of the ultrasound is preferably 10~120min, more preferably 30~90min, most preferably 50~
70min；The present invention does not have special restriction for the power of the ultrasound, using ultrasonic power well known to those skilled in the art
.
After obtaining mixed liquor, the present invention mixes the mixed liquor with reducing agent, obtains reaction solution.In the present invention, institute
It is preferably hydrazine hydrate, ascorbic acid or ammonium hydroxide to state reducing agent.In the present invention, the concentration of the hydrazine hydrate be preferably 0.4~
0.65mg/mL, more preferably 0.45~0.6mg/mL；In the hydrazine hydrate mass ratio of hydrazine and graphene oxide be preferably (2~
5)：11, more preferably (3~4)：11.In the present invention, the mass ratio of the ascorbic acid and graphene oxide be preferably (1~
3)：1, more preferably (1.5~2.5)：1.In the present invention, the ammon amount of the ammonium hydroxide is preferably 25~28%；The ammonium hydroxide
Volume ratio with mixed liquor is preferably 1：(10~100), more preferably 1：(30~70), most preferably 1：(40~50).
In the present invention, preferably reducing agent is added into the mixed liquor in the mixing of the mixed liquor and reducing agent.
In the present invention, when the reducing agent is hydrazine hydrate or ammonium hydroxide, the feed postition of the hydrazine hydrate or ammonium hydroxide is preferably added dropwise；Institute
The rate for stating dropwise addition is preferably 1 drop/sec；When the reducing agent is ascorbic acid, the ascorbic acid is preferably directly with powder
Form is added in the mixed liquor.In the present invention, the mixing of the mixed liquor and reducing agent preferably under agitation into
Row；The rate of the stirring is preferably 400~600rpm.
After obtaining reaction solution, sponge impregnating in the reaction solution, is carried out reduction reaction by the present invention under air-proof condition,
Obtain titanium dioxide-graphene composite sponge.In the present invention, the sponge is preferably melamine sponge or polyurethane sponge.This
Invention does not have the source of the sponge special restriction, using commercial goods well known to those skilled in the art.
In the present invention, the volume ratio of the sponge and reaction solution is preferably 1：(0.8~1.2), more preferably 1：1.
In the present invention, the sponge is preferably washed and is dried successively before.In the present invention, the washing
Used washing reagent is preferably followed successively by ethyl alcohol, acetone and deionized water；In the present invention, the washing is preferably in ultrasonic item
It is carried out under part；The ultrasonic time needed for washing is preferably 10~20min every time, more preferably 15min.In the present invention, described
Dry temperature is preferably 90~110 DEG C, more preferably 100 DEG C；The time of the drying is preferably 10~14h, more preferably
12h。
In the present invention, the temperature of the reduction reaction is preferably 80~100 DEG C, more preferably 85~95 DEG C, most preferably
It is 90 DEG C；The time of the reduction reaction is preferably 0.5~10h, more preferably 2~8h, most preferably 4~6h.In the present invention
In, the reduction reaction carries out under air-proof condition, and the loss such as volatilization of reducing agent can be avoided multiple to titanium dioxide-graphene
The performance for closing sponge impacts.The present invention removes hydroxyl, carboxyl, carbonyl contained by graphene oxide by the reduction reaction
Equal oxygen-containing functional groups, graphene is reduced by graphene oxide；Meanwhile in the process, graphene surface formed electronics with
Titanium dioxide surface electronically forms Ti-O-C keys, is conducive to improve photocatalysis efficiency.
After completing the reduction reaction, preferably gained wet sponge after reduction reaction is dried by the present invention, obtains dioxy
Change titanium-graphene composite sponge.In the present invention, the temperature of the drying is preferably 90~110 DEG C, more preferably 100 DEG C；Institute
It is preferably 10~14h to state the dry time, more preferably 12h.
The titanium dioxide being prepared the present invention provides preparation method described in above-mentioned technical proposal-graphene compounding sea
Silk floss, including sponge and the titanium dioxide and graphene that are supported on the sponge.In the present invention, the titanium dioxide and graphite
Alkene is uniformly supported on sponge, while there is also Ti-O-C keys between titanium dioxide and graphene, titanium dioxide and graphene,
Sponge is firmly combined with, and stability is good.
The present invention provides titanium dioxide described in above-mentioned technical proposal-graphene composite sponge answering in water pollution processing
With.In the present invention, the application is specifically using being polluted in the titanium dioxide-graphene composite sponge photocatalytic degradation water
Object.In the present invention, the pollutant preferably includes dyestuff, surfactant or organophosphorus insecticide.In the implementation of the present invention
In example, the photocatalysis of titanium dioxide provided by the invention-graphene composite sponge is specifically evaluated using methylene blue as pollutant
Degradation effect.
Below in conjunction with the embodiment in the present invention, the technical solution in the present invention is clearly and completely described.It is aobvious
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1
Graphene oxide is mixed with water, obtains the graphene oxide dispersion of a concentration of 0.1mg/mL of 100mL；To described
10mg hydrophilies TiO is added in graphene oxide dispersion2, ultrasonic 10min obtains mixed liquor；
Under 500rpm stir speed (S.S.)s, with 1 drop/sec of drop rate, hydrazine hydrate is added dropwise into the mixed liquor, and (hydrazine contains
Amount is 1.8mg), obtain reaction solution；
In the reaction solution by melamine sponge impregnating, under air-proof condition, reduction reaction 0.5h is carried out in 80 DEG C, by institute
Dry 12h at 100 DEG C of wet sponge is obtained, titanium dioxide-graphene composite sponge is obtained；Wherein, the melamine sponge is before use
It is cleaned by ultrasonic 15min respectively with ethyl alcohol, acetone and deionized water successively, then dry 12h at 100 DEG C.
Titanium dioxide-graphene composite sponge prepared by embodiment 1 is tested for the property, it is specific as follows：
The titanium dioxide-graphene composite sponge is added in the methylene blue solution of a concentration of 2mg/mL, is carried out
1h sunlights irradiate.
Control experiment, color contrast figure such as Fig. 1 and Fig. 2 institutes of the front and back methylene blue solution of sunlight irradiation are set simultaneously
Show, wherein be not load TiO in No. 2 beakers without any product in No. 1 beaker2Graphene sponge, be in No. 3 beakers
Titanium dioxide-graphene composite sponge prepared by embodiment 1.Fig. 1 and Fig. 2 are shown, are irradiated by the sunlight of 1h, No. 1 beaker
The variation of methylene indigo plant solution colour is little, and for No. 2 beakers due to the suction-operated of graphene, methylene blue solution color becomes light
Blue, No. 3 beaker methylene indigo plant Solutions Solutions have turned into colourless.It is possible thereby to illustrate titanium dioxide-stone prepared by embodiment 1
Black alkene composite sponge, while playing suction-operated and the TiO of graphene2Photocatalysis, and photocatalysis efficiency is high.
Titanium dioxide-graphene the composite sponge prepared to embodiment 1 characterizes before and after use, wherein Fig. 3 and figure
4 be that titanium dioxide-graphene composite sponge prepared by embodiment 1 is schemed using front and back SEM, can from Fig. 3 and Fig. 4
Go out, before and after use, TiO in titanium dioxide-graphene composite sponge2There are a large amount of loads, shows TiO2With graphene, sponge
It is firmly combined with, can be used with repetitive cycling.It is possible thereby to illustrate that titanium dioxide-graphene composite sponge prepared by embodiment 1 is steady
It is qualitative good.
Embodiment 2
Preparation method substantially with embodiment 1, the difference is that：A concentration of 10mg/mL of graphene oxide dispersion, adds
Enter TiO2Quality be 1g, ultrasonic time 120min, be added hydrazine hydrate in hydrazine content be 454.5mg, reduction reaction temperature
It it is 100 DEG C, the reduction reaction time is 10h.
According to the method for embodiment 1, to the titanium dioxide-that is prepared, graphene composite sponge is tested for the property and table
Sign, it is as a result almost the same with embodiment 1.
Embodiment 3
Preparation method substantially with embodiment 1, the difference is that：Sponge used is polyurethane sponge, graphene oxide
TiO is added in a concentration of 5mg/mL of dispersion liquid2Quality be 0.5g, ultrasonic time 60min, hydrazine in hydrazine hydrate is added and contains
Amount is 145.5mg, and reduction reaction temperature is 90 DEG C, and the reduction reaction time is 5h.
According to the method for embodiment 1, to the titanium dioxide-that is prepared, graphene composite sponge is tested for the property and table
Sign, it is as a result almost the same with embodiment 1.
Embodiment 4
Preparation method substantially with embodiment 3, the difference is that：The reducing agent of addition is ascorbic acid, and Vitamin C is added
The quality of acid is 0.5g, and reduction reaction temperature is 80 DEG C, and the reduction reaction time is 8h.
According to the method for embodiment 1, to the titanium dioxide-that is prepared, graphene composite sponge is tested for the property and table
Sign, it is as a result almost the same with embodiment 1.
Embodiment 5
Preparation method substantially with embodiment 4, the difference is that：The reducing agent of addition is ammonium hydroxide (ammon amount 26%),
The volume of the ammonium hydroxide of addition is 5mL, and the reduction reaction time is 10h.
According to the method for embodiment 1, to the titanium dioxide-that is prepared, graphene composite sponge is tested for the property and table
Sign, it is as a result almost the same with embodiment 1.
As seen from the above embodiment, titanium dioxide provided by the invention-graphene composite sponge avoids secondary convenient for recycling
Pollution, and titanium dioxide and graphene will not fall off from sponge during use, it is reusable.The experimental result of embodiment
Show that titanium dioxide provided by the invention-graphene composite sponge photocatalysis efficiency is high, photocatalysis stability is good.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of titanium dioxide-graphene composite sponge, includes the following steps：
Water, graphene oxide and titanium dioxide are mixed, mixed liquor is obtained；
The mixed liquor is mixed with reducing agent, obtains reaction solution；
In the reaction solution by sponge impregnating, reduction reaction is carried out under air-proof condition, and it is compound to obtain titanium dioxide-graphene
Sponge.
2. preparation method according to claim 1, which is characterized in that graphene oxide and titanium dioxide in the mixed liquor
Concentration stand alone as 0.1~10mg/mL.
3. preparation method according to claim 1, which is characterized in that the reducing agent is hydrazine hydrate, ascorbic acid or ammonia
Water.
4. preparation method according to claim 3, which is characterized in that a concentration of 0.4~0.65mg/ of the hydrazine hydrate
mL；The mass ratio of hydrazine and graphene oxide is (2~5) in the hydrazine hydrate：11.
5. preparation method according to claim 3, which is characterized in that the mass ratio of the ascorbic acid and graphene oxide
For (1~3)：1.
6. preparation method according to claim 3, which is characterized in that the ammon amount of the ammonium hydroxide is 25~28%；It is described
The volume ratio of ammonium hydroxide and mixed liquor is 1：(10~100).
7. preparation method according to claim 1, which is characterized in that the sponge is melamine sponge or polyurethane sponge.
8. preparation method according to claim 1, which is characterized in that the temperature of the reduction reaction is 80~100 DEG C, also
The time of original reaction is 0.5~10h.
9. titanium dioxide-graphene composite sponge that any one of claim 1~8 preparation method is prepared, including sea
The tender titanium dioxide and graphene being supported on the sponge.
10. application of titanium dioxide described in the claim 9-graphene composite sponge in water pollution processing.
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| CN110240731B (en) * | 2019-05-23 | 2021-06-25 | 东南大学 | Preparation method of graphene-metal oxide composite sponge with high specific surface area |
| CN110182887A (en) * | 2019-06-27 | 2019-08-30 | 中素新科技有限公司 | The processing method of organic dyestuff in wastewater |
| CN110180513A (en) * | 2019-06-27 | 2019-08-30 | 中素新科技有限公司 | Titanium dioxide-graphene oxide composite sponge and its preparation method and application |
| WO2020258931A1 (en) * | 2019-06-27 | 2020-12-30 | 童裳慧 | Method for treating organic dye in waste water |
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