CN107570111A - Height is adsorbed with the preparation method and application of engine dyeing material list wall carbon nano tube flexible membrane - Google Patents
Height is adsorbed with the preparation method and application of engine dyeing material list wall carbon nano tube flexible membrane Download PDFInfo
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Abstract
The present invention relates to carbon nano tube flexible film to adsorb dye field, specially a kind of high preparation method and application for being adsorbed with engine dyeing material list wall carbon nano tube flexible membrane.Single-walled carbon nanotube prepared by floating catalytic agent chemical vapour deposition technique is scattered in organic solvent, single wall carbon nano-tube film is can obtain through simply filtering, drying.Gained single-wall carbon nanotube membrane has excellent pliability, light, efficient absorption organic dyestuff and can be recycled.The present invention solves that current Carbon Materials are low to organic dyestuff adsorbance and secondary pollution problems are easily introduced using Carbon Materials powder as adsorbent, while also breaches current organic dyestuff adsorbed film in weight, flexibility, the limitation recycled etc..
Description
Technical field
The present invention relates to carbon nano tube flexible film to adsorb dye field, and specially a kind of height is adsorbed with engine dyeing material list wall carbon and received
The preparation method and application of mitron flexible membrane.
Background technology
The organic dyestuff such as methylene blue, rhodamine B, methyl orange, Congo red is as conventional dyestuff in weaving and food work
Industry is widely used；However, organic dyestuff has the shortcomings that toxic is big, carcinogenicity is high and biodegradation rate is slow.Cause
And the pressing issues that the organic dyestuff how removed in industrial wastewater is current weaving and development of food industry is faced.At present,
A variety of methods are developed, such as photocatalytic degradation, chemical degradation, Fenton-based oxidations, ozonisation etc..However, above-mentioned skill
The problems such as high poor selectivity, cost, not reproducible use (document 1.Ali, I.Chem.Rev., 2012,112 be present in art:5073.
Document 2.Li, L.X.；Li,B.C.；Wu,L.；Zhao,X.；Zhang,J.P.Chem.Commun.,2014,50:7831).Cause
This, develop reusable, efficient absorption organic dyestuff material or method be this area research emphasis and difficult point.
The Carbon Materials such as CNT (CNT), activated carbon, graphene have that specific surface area is high, stability is good, environment-friendly etc.
Feature is considered as to adsorb the ideal candidates material of heavy metal ion and organic pollution.However, most of carbon-based absorption at present
The problems such as agent is to exist in powder form, and this causes serious recontamination and powder sorbent to be difficult to recovery；Efficient absorption simultaneously
Research less (the document 1.Geim, A.K. of a variety of organic dyestuff；Novoselov,K.S.Nat.Mater.,2007,6:183.Text
Offer 2.Yang, Y.M.；Hu,G.W.；Chen,F.J.；Liu,J.；Liu,W.S.；Zhang,H.L.；Wang,
B.D.Chem.Commun.,2015,51:14405), although the flexible carbon-based material such as grapheme foam is reported available for sewage
Processing, but the adsorbance of general graphene sorbent treatment pollutant is small, constrains the development (text of grapheme foam adsorbent
Offer 1.Geng, Z.G.；Lin,Y.；Yu,X.X.；Shen,Q.H.；Ma,L.；Li,Z.Y.；Pan,N.；Wang,
X.P.J.Mater.Chem.,2012,22:3527.Document 2.Tiwari, J.N.；Mahesh,K.；Le,N.H.；Kemp,K.C.；
Timilsina,R.；Tiwari,R.N.；Kim,K.S.Carbon,2013,56:173).
Current subject matter is：How magnanimity prepares high-flexibility, high adsorption, reusable carbonaceous membrane,
Solve the secondary pollution of powdered Carbon Materials adsorbent at present and other adsorbent adsorbances are limited, the not reproducible technology such as use
Problem.
The content of the invention
It is an object of the invention to provide a kind of high preparation method for being adsorbed with engine dyeing material list wall carbon nano tube flexible membrane and
Using, pass through it is simply scattered, filter film technique, prepare the single-walled carbon nanotube of recyclable, reversible adsorption desorption organic dyestuff
Flexible membrane, solve nano-carbon material powder as adsorbent introducing secondary pollution and other sorbing materials it is not reproducible utilize ask
Topic, to obtain high absorption property, repeatable utilization, environment-friendly, stable performance single-walled carbon nanotube flexible membrane.
The technical scheme is that：
A kind of high preparation method for being adsorbed with engine dyeing material list wall carbon nano tube flexible membrane, is comprised the following steps that：Floating is urged
Agent chemical vapour deposition technique prepare single-walled carbon nanotube be scattered in organic solvent, through filtering, dry obtain single wall carbon receive
Mitron flexible membrane.
Described height is adsorbed with the preparation method of engine dyeing material list wall carbon nano tube flexible membrane, and single-walled carbon nanotube content is more than
95%, the length of single-walled carbon nanotube is 50~100 μm, specific surface area is 300~800m2g-1, pore-size distribution be 2~10nm.
Described height is adsorbed with the preparation method of engine dyeing material list wall carbon nano tube flexible membrane, and scattered organic solvent is second
Alcohol, acetone, ethylene glycol or isopropanol.
Described height is adsorbed with the preparation method of engine dyeing material list wall carbon nano tube flexible membrane, single-walled carbon nanotube flexible membrane
Thickness and size can be regulated and controled by content of carbon nanotubes and filter size.
Described height is adsorbed with the preparation method of engine dyeing material list wall carbon nano tube flexible membrane, single-walled carbon nanotube flexible membrane warp
The still integrality of holding structure, and strong stirring will not also destroy its structure in water or organic solvent after bending infinitely.
Described height is adsorbed with the application of engine dyeing material list wall carbon nano tube flexible membrane, and single-walled carbon nanotube flexible membrane is to organic
Dyestuff has high characterization of adsorption, applied to absorption dyestuff：Methylene blue, rhodamine B, methyl orange or Congo red, to methylene blue
Adsorbance reach 198mg g-1, 190mg g are reached to the adsorbance of rhodamine B-1, 130mg is reached to the adsorbance of methyl orange
g-1, 90mg g are reached to Congo red adsorbance-1。
Described height is adsorbed with the application of engine dyeing material list wall carbon nano tube flexible membrane, and single-walled carbon nanotube flexible membrane is to organic
The adsorption desorption of dyestuff is reversible, and single-walled carbon nanotube flexible membrane recycles.
The present invention design philosophy be：
Using the overlap joint effect of accurate one-dimensional single-walled carbon nanotube sample room and compared with strong interaction, other surfaces are not being introduced
Activating agent and strong physics chemical action, keep realizing high-flexibility single wall on the premise of the original intrinsic structure of single-walled carbon nanotube
The preparation of carbon nano-tube film, utilize the strong capillary action for the 2~10nm mesopore orbits constructed that lapped one another between CNT
And characterization of adsorption caused by the high activity specific surface area of exposure, realize efficient, the reversible suction to one or more of organic dyestuff
Desorption.
Advantages of the present invention and beneficial effect are：
1st, single-walled carbon nanotube prepared by floating catalytic agent chemical vapour deposition technique is scattered in organic solvent by the present invention,
Single wall carbon nano-tube film is can obtain through simply filtering, drying.The present invention utilizes single-walled carbon nanotube primary sample first
High-purity and big L/D ratio characteristic, high-flexibility single-wall carbon nanotube membrane is realized by simply scattered and filtering coating technology
The preparation of sorbing material, overcome the problem of current Carbon Materials introduce secondary pollution as powder adsorbent.
2nd, the present invention is lapped one another 2~10nm mesopore orbits for constructing using high-purity, the single-walled carbon nanotube of overlength
Characterization of adsorption caused by strong capillary action and the high activity specific surface area of exposure, is realized to methylene blue, rhodamine
B, one or more of efficient absorptions simultaneously in the organic dyestuff such as methyl orange, Congo red.Particularly, current Carbon Materials pair are solved
In low and be easily introduced two using Carbon Materials powder as adsorbent to the adsorbance such as methylene blue, rhodamine B, methyl orange, Congo red
The problems such as secondary pollution, while also breach limitation of the current organic dyestuff adsorbed film in weight, flexibility, recycling etc.
Property.
3rd, the reversible adsorption desorption of the invention realized by physisorption to organic dyestuff, solves current major part
Adsorb the not reproducible problem utilized of organic dye material.
What the 4th, the present invention developed prepare, and single-walled carbon nanotube flexibility membrane technology has that technique is simple, is easy to the spies such as scale
Point, so as to be expected to play a significant role in fields such as food, weavings.
5th, single-walled carbon nanotube of the present invention is without any purification and post processing, prepared single-walled carbon nanotube flexible membrane tool
Have the advantages that pliability is good, light, adsorbance is big, absorption kind of dyes is more, can prepare in batches.Organic solvent be ethanol, acetone,
The organic reagent such as ethylene glycol or isopropanol, without adding any surfactant, surfactant residual is avoided to single wall carbon
The influence of nanotube performance.
Brief description of the drawings
Fig. 1 is the optical photograph of various sizes of carbon nano-tube film.
Fig. 2 is the optical photograph of flexible carbon nano tube film.
Fig. 3 is the electron scanning micrograph of single-wall carbon nanotube membrane.
Fig. 4 is the single-walled carbon nanotube staple diagram counted under ESEM.
Fig. 5 is the differential thermal analysis curve figure of carbon nano-tube film.In figure, curve 1 is the relation of temperature and percent weight loss, bent
Line 2 is temperature and DSC (mW/mg, that is, flowing to the power of every milligram of sample) relation.
Fig. 6 is the absorption/desorption and graph of pore diameter distribution (illustration) of carbon nano-tube film.
Fig. 7 is the optical photograph before and after the flow chart and degradation of methylene blue for preparing carbon nano-tube film.
Fig. 8 is that carbon nano-tube film changes with time figure to organic dyestuff adsorbance.
Fig. 9 is that absorption/desorption optics of the carbon nano-tube film to organic dyestuff methylene blue (a-d) and rhodamine B (e-h) shines
Piece.
Figure 10 is the performance curve that carbon nano-tube film repeats absorption methylene blue (a) and rhodamine (b).
Embodiment
Below, the present invention is described in further detail by embodiment.
Embodiment 1
The preparation of single-walled carbon nanotube flexible membrane：20mg single wall carbon prepared by floating catalytic agent chemical vapour deposition technique is received
Mitron primary sample is added in 200mL ethanol solutions, ultrasonic disperse 30min.Then by scattered obtained carbon nano-tube solution
Film forming is filtered, according to filter caliber size used, various sizes of membranaceous sample (Fig. 1), and the membranaceous sample can be prepared
With excellent pliability (Fig. 2).Electron microscope, thermogravimetric analysis, low temperature are scanned to original single-walled carbon nanotube sample
The structural characterizations such as liquid nitrogen absorption.ESEM (Fig. 3) observation finds that sample is pure, and length of carbon nanotube is longer and straight, scanning
The length that CNT is counted under Electronic Speculum is 50~70 μm (Fig. 4).The differential thermal analysis curve (Fig. 5) of sample shows single
The concentration oxidizing temperature section of pipe is 700~850 DEG C, shows that sample has structural homogeneity and high crystalline；The impurity of sample
Content is only 7%, shows that sample has high-purity.The liquid nitrogen Adsorption and desorption isotherms and corresponding pore size distribution curve of sample are as schemed
Shown in 6, it is seen that the aperture integrated distribution of sample is 349m by the counted specific surface area of adsorption isotherm in 2~6nm2/g。
Flexibility, it can be recycled, the absorption property of high-performance adsorbed film：The single-walled carbon nanotube that above-mentioned steps are obtained
Membrane sample is placed in methylene blue solution and stirred, and carries out absorption property test, experiment flow such as Fig. 7.As shown in fig. 7, carbon nanometer
The preparation flow of periosteum is as follows：Single-walled carbon nanotube prepared by floating catalytic agent chemical vapour deposition technique is scattered in organic solvent
In, it can obtain single wall carbon nano-tube film through simply filtering, drying.
Fig. 8 is that carbon nano-tube film adsorbs the adsorption curve figure that methylene blue changes over time.As shown in Figure 8, the adsorbed film
198mg g are reached to the adsorbance of methylene blue-1, adsorption time 240min.
Flexibility, it can be recycled, the desorption performance of high-performance adsorbed film：The single-wall carbon nanotube membrane of methylene blue will be adsorbed
Sample is placed in ethanol solution and stirred, and carries out desorption performance test.As seen from Figure 9, desorption rate of the adsorbed film to methylene blue
For 194mg g-1, desorption time is 10 hours.After desorption, single-wall carbon nanotube membrane sample is dried, then to be placed in methylene blue molten
Stirred in liquid, carry out repeating absorption and desorption performance test.It is repeated 20 times, the structure of single-wall carbon nanotube membrane sample is not broken
Bad, significant change (Figure 10) does not occur for adsorbance.
Embodiment 2
The preparation of single-walled carbon nanotube flexible membrane：With embodiment 1, the dispersant used in the present embodiment is acetone, single wall carbon
Nanotube sample average length is 70~80 μm, and aperture integrated distribution is in 4~8nm, specific surface area 498m2/g。
Flexibility, it can be recycled, the absorption property of high-performance adsorbed film：With embodiment 1, the adsorbed dyestuff of the present embodiment
For rhodamine B, the adsorbed film reaches 190mg g to the adsorbance of rhodamine B-1, adsorption time is 240min (such as Fig. 8).
Flexibility, it can be recycled, the desorption performance of high-performance adsorbed film：With embodiment 1, the adsorbed film is to rhodamine B
Desorption rate is 174mg g-1, desorption time is 10 hours.
Embodiment 3
The preparation of single-walled carbon nanotube flexible membrane：With embodiment 1, the dispersant used in the present embodiment is ethylene glycol, single wall
Carbon nanotube-sample average length is 80~90 μm, and aperture integrated distribution is in 4~9nm, specific surface area 657m2/g。
Flexibility, it can be recycled, the absorption property of high-performance adsorbed film：With embodiment 1, the adsorbed dyestuff of the present embodiment
For methyl orange, the adsorbed film reaches 130mg g to the adsorbance of methyl orange-1, adsorption time is 240min (such as Fig. 8).
Flexibility, it can be recycled, the desorption performance of high-performance adsorbed film：With embodiment 1, the adsorbed film takes off to methyl orange
Attached amount is 121mg g-1, desorption time is 10 hours.
Embodiment 4
The preparation of single-walled carbon nanotube flexible membrane：With embodiment 1, the dispersant used in the present embodiment is isopropanol, single wall
Carbon nanotube-sample average length is 90~100 μm, and aperture integrated distribution is in 5~10nm, specific surface area 780m2/g。
Flexibility, it can be recycled, the absorption property of high-performance adsorbed film：With embodiment 1, the adsorbed dyestuff of the present embodiment
To be Congo red, the adsorbed film reaches 90mg g to Congo red adsorbance-1, adsorption time is 240min (such as Fig. 8).
Flexibility, it can be recycled, the desorption performance of high-performance adsorbed film：With embodiment 1, the adsorbed film takes off to Congo red
Attached amount is 82mg g-1, desorption time is 10 hours.
Embodiment result shows that the present invention designs and the single-walled carbon nanotube flexible membrane of preparation, wherein single-walled carbon nanotube
Quality is high, length length so that the carbon nano-tube film of preparation has excellent pliability, light, abundant pore structure, Gao Bibiao
Area and excellent reversible adsorption organic dyestuff characteristic, efficient absorption organic dyestuff and it can be recycled.For example, to rhodamine
B adsorbance reaches 190mg g-1, it is reported the optimal adsorptive value of Carbon Materials 1.3 times.The present invention is utilized and is simply filtered into
Embrane method realizes the preparation of high-flexibility, the high single wall carbon nano-tube film for adsorbing organic dyestuff characteristic, solves current carbon and receives
The crucial Science and Technology problems such as rice material adsorbed film low intensity, poor, the preparation process complexity of pliability.
Claims (7)
1. a kind of high preparation method for being adsorbed with engine dyeing material list wall carbon nano tube flexible membrane, it is characterised in that comprise the following steps that：
Single-walled carbon nanotube prepared by floating catalytic agent chemical vapour deposition technique is scattered in organic solvent, through filtering, dries acquisition
Single-walled carbon nanotube flexible membrane.
2. being adsorbed with the preparation method of engine dyeing material list wall carbon nano tube flexible membrane according to the height described in claim 1, its feature exists
Be more than 95% in, single-walled carbon nanotube content, the length of single-walled carbon nanotube is 50~100 μm, specific surface area be 300~
800m2g-1, pore-size distribution be 2~10nm.
3. being adsorbed with the preparation method of engine dyeing material list wall carbon nano tube flexible membrane according to the height described in claim 1, its feature exists
In scattered organic solvent is ethanol, acetone, ethylene glycol or isopropanol.
4. being adsorbed with the preparation method of engine dyeing material list wall carbon nano tube flexible membrane according to the height described in claim 1, its feature exists
In the thickness and size of single-walled carbon nanotube flexible membrane can be regulated and controled by content of carbon nanotubes and filter size.
5. being adsorbed with the preparation method of engine dyeing material list wall carbon nano tube flexible membrane according to the height described in claim 1, its feature exists
In single-walled carbon nanotube flexible membrane still integrality of holding structure, and the strength in water or organic solvent after bending infinitely
Stirring will not also destroy its structure.
6. the height described in a kind of claim 1 is adsorbed with the application of engine dyeing material list wall carbon nano tube flexible membrane, it is characterised in that single
Wall carbon nano tube flexible membrane has high characterization of adsorption to organic dyestuff, applied to absorption dyestuff：Methylene blue, rhodamine B, methyl
It is orange or Congo red, 198mg g are reached to the adsorbance of methylene blue-1, 190mg g are reached to the adsorbance of rhodamine B-1, to first
The adsorbance of base orange reaches 130mg g-1, 90mg g are reached to Congo red adsorbance-1。
7. the application of engine dyeing material list wall carbon nano tube flexible membrane is adsorbed with according to the height described in claim 6, it is characterised in that single
Wall carbon nano tube flexible membrane is reversible to the adsorption desorption of organic dyestuff, and single-walled carbon nanotube flexible membrane recycles.
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| WO2022121101A1 (en) * | 2020-12-09 | 2022-06-16 | 苏州大学 | Method for separating dye-containing wastewater based on porous polymer-modified metal carbon nanotube composite membrane |
| CN114797772A (en) * | 2022-04-02 | 2022-07-29 | 中国科学院理化技术研究所 | Adsorption film, preparation method thereof and electric heating adsorption bed for low-temperature system |
| US11999636B2 (en) * | 2020-12-09 | 2024-06-04 | Soochow University | Method for purifying dye-containing wastewater based on porous-polymer-modified metal carbon nanotube composite membrane |
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Application publication date: 20180112 |