CN107099271B - A kind of strong UV, visible light powder body material and preparation method thereof compound based on Carbon fibe and ferrocene - Google Patents
A kind of strong UV, visible light powder body material and preparation method thereof compound based on Carbon fibe and ferrocene Download PDFInfo
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- CN107099271B CN107099271B CN201710225403.XA CN201710225403A CN107099271B CN 107099271 B CN107099271 B CN 107099271B CN 201710225403 A CN201710225403 A CN 201710225403A CN 107099271 B CN107099271 B CN 107099271B
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Abstract
The invention discloses a kind of preparation methods of strong UV, visible light powder body material compound based on carbon fiber and ferrocene.Fire and carbon fiber and activate first with sugarcane skin, then using solid phase reaction will the carbon fiber of activation and ferrocene mix after grind uniformly, be uniformly mixed it and sufficiently compound, composite powder material be made.The present invention has good absorption to light in the region of the wider ultraviolet-visible wavelength of 200~800nm using composite material prepared by sugarcane skin and ferrocene, is expected to do ideal light absorbent in solar cells, and realize the purpose to turn waste into wealth.
Description
Technical field
The invention belongs to composite functional material technical fields.It is multiple based on Carbon fibe and ferrocene more particularly, to one kind
The strong UV, visible light powder body material and preparation method thereof closed.
Background technique
Ferrocene derivatives are made ferrocene and its are spread out as non-benzene aromatic compound due to the presence of iron atom in molecule
The physicochemical property of biology shows uncommon diversity.Therefore, various countries to the synthesis of Ferrocene and its derivative, property and divide
The research of minor structure is very active, flourishing long time for decades.Just because of ferrocene derivatives qualitative diversity and stability,
Make its wide range of applications.Such as in combustibility regulator, asymmetric catalysis agent, magnetic material, liquid crystal material
And all various aspects such as biochemical medicine have significant application value.
Activated carbon fibre (activatedcarbonfiber, ACF) is early 1970s on the basis of Carbon fibe
A kind of novel adsorption functional material to grow up is the third generation active carbon adsorption material after powdery, granular active carbon.It is living
The filament diameter of property Carbon fibe is thin, microcellular structure is flourishing, specific surface area and adsorption capacity are big, a large amount of pore openings are in fiber filament
Surface, thus inhale, desorption rate it is fast；Have the characteristics that pore-size distribution is concentrated, is particularly excellent to low concentration adsorbate adsorption capacity,
It has been widely used in gas separation and wastewater treatment etc..The surface chemical structure and pore structure of activated carbon fibre are to influence
An important factor for its adsorption capacity, can change its surface chemical structure and hole knot by means such as physical modification and chemical modifications
Structure, to further increase its absorption property.Therefore, the surface of Study On The Activated Carbon fiber is modified and its pore structure has important meaning
Justice.
It is rich in organic matter abundant and a considerable amount of wood fibre in sugarcane skin, there is very big application value.But
Because itself is not by certain concern, most of sugarcane skin is all directly to be thrown away, and causes great waste.
Summary of the invention
The purpose of the present invention is have bigger pi-electron conjugated system and stronger inside based on ferrocene derivatives
Molecular electronic transfer characteristic has good photoelectric functional property；And Carbon fibe and organo-metallic compound have good interface
Interaction, Carbon fibe have special optical property in UV light region；By Carbon fibe and ferrocene under certain condition with not
Same molar ratio carries out a kind of compound, obtained novel organic/inorganic composite material.The composite material 200~800nm compared with
There is good absorption in the region of wide ultraviolet-visible wavelength to light, is expected to become the ideal light absorbent of solar battery etc., and
Achieve the purpose that turn waste into wealth.
The object of the present invention is to provide a kind of strong UV, visible light powder body material compound based on Carbon fibe and ferrocene and its
Preparation method.
Another object of the present invention is to provide application of the strong UV, visible light powder body material in terms of light absorbent.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of the strong UV, visible light powder body material compound based on Carbon fibe and ferrocene, including walk as follows
It is rapid:
S1. Carbon fibe is fired using sugarcane skin；
S2. activated carbon fibre is prepared；
S3. Carbon fibe and ferrocene composite material are prepared using solid phase reaction: after active carbon fibre peacekeeping ferrocene is mixed
Grinding uniformly, keeps it uniformly mixed and sufficiently compound, composite powder material is made.
Preferably, the mass ratio of active carbon fibre peacekeeping ferrocene is 3~5:5~7 in step S3.
Preferably, the time of grinding described in step S3 is 1.0~2.0 hours.
Preferably, the method that step S1 fires Carbon fibe using sugarcane skin are as follows: successively will be new with H3PO4 solution and distilled water
After fresh sugarcane skin cleaning (3 times) is clean, 102~110 DEG C drying to constant weight, is crushed (such as being shredded with scissors), 500~700 DEG C
1.5~2.5h of calcining makes its carbonization, is then ground to powdered.
Wherein preferably, the volume ratio of H3PO4 and distilled water is 1:15~25mol in the H3PO4 solution.
Preferably, the method that step S2 prepares activated carbon fibre are as follows: the method for step S2 preparation activated carbon fibre are as follows: will walk
The Carbon fibe that rapid S1 is obtained is added in phosphoric acid solution, 50~70 DEG C of 80~100min of activation (preferably 60 DEG C activation 90min)；Then
Solution is filtered, then with distilled water flushing filter residue to neutral or close neutrality；Filter paper and filter residue are placed on 100 together again~
Inside 120 DEG C (preferably 110 DEG C) of baking oven, drying to constant weight to get activated carbon fibre is arrived, and stores in wide-mouth bottle.
Preferably, the volume ratio of phosphoric acid and water is 1:5~15 in the phosphoric acid solution.
It is highly preferred that the volume ratio of phosphoric acid and water is 1:10 in the phosphoric acid solution.
Preferably, the quality volume of the Carbon fibe and phosphoric acid solution are as follows: 1.5~2.0g:3.0~5.0mL.
The present invention is prepared for Carbon fibe using sugarcane skin, contains a considerable amount of wood fibre in sugarcane skin, through overdrying
Dry to remove moisture removal, Muffle furnace high-temperature calcination makes it be carbonized and increases specific surface area, reduces partial size finally with can be with after phosphoric acid activation
It is transformed into performance to stablize, the minimum activated carbon fibre of partial size.After Carbon fibe is activated, with ferrocene under certain condition with not
Same molar ratio carries out compound, obtained organic/inorganic combination product through solid grinding method.And combination product is subjected to structure point
Analysis, inquires into its photoelectric properties, provides theoretical and experimental basis for exploitation novel ferrocene functional composite material.
The invention has the following advantages:
The composite material that the present invention is prepared using sugarcane skin and ferrocene is in the wider ultraviolet-visible wavelength of 200~800nm
Region have good absorption to light, be expected to do ideal light absorbent in solar cells, and realize the mesh turned waste into wealth
's.
Detailed description of the invention
Fig. 1 is the electron microscopic picture of 400 DEG C of firing Carbon fibes.
Fig. 2 is the electron microscopic picture of 500 DEG C of firing Carbon fibes.
Fig. 3 is the electron microscopic picture of 600 DEG C of firing Carbon fibes.
Fig. 4 is the electron microscopic picture of 700 DEG C of firing Carbon fibes.
Fig. 5 is the XRD diagram piece of Carbon fibe and ferrocene composite material.
Fig. 6 is the solid ultraviolet image of Carbon fibe and ferrocene composite material.
Specific embodiment
The present invention is further illustrated below in conjunction with Figure of description and specific embodiment, but embodiment is not to the present invention
It limits in any form.Unless stated otherwise, the present invention uses reagent, method and apparatus routinely try for the art
Agent, method and apparatus.
Unless stated otherwise, following embodiment agents useful for same and material are commercially available.
The preparation of embodiment the last 1 UV, visible light powder body material
1, the carbonization of sugarcane skin --- fire Carbon fibe
(1) first with H3PO4 solution (volume ratio of H3PO4 and distilled water is 1:15~25 in H3PO4 solution) and distilled water
Fresh sugarcane skin is cleaned 3 times afterwards, cleans to be placed in 102~110 DEG C of baking ovens and dries to constant weight, by sugarcane skin with cutting after taking-up
Knife shreds, and is placed in spare in wide-mouth bottle.It weighs 4.5~5.5g and shreds the sugarcane skin sample handled well and be placed in porcelain crucible, cover
After be placed on Muffle furnace high temperature calcining make its carbonization, calcination temperature is respectively that 400,500,600,700 DEG C of high-temperature calcinations make it
Carbonization, calcination time are 1.5~2.5h.Calcined sugarcane skin is taken out, is ground into powder down in grinding ware with grinding pestle
Enter beaker, the activation for next step.
(2) the scanning electron microscope detection of Carbon fibe is fired
Micro 400 DEG C, 500 DEG C, 600 DEG C, the 700 DEG C Carbon fibes progress Electronic Speculum detections fired after activation are taken respectively.It is logical
The difference for crossing electron microscopic picture is compared the firing degree under different temperatures, and most suitable and relative energy-saving firing temperature is discussed out
Degree.
What the carbon fired it can be seen from the image (Fig. 1~4) of Electronic Speculum was shown is a kind of layer of fibrous structure.But
When 400 DEG C, this layer threadiness is not obvious, only small part layered fibre, is existed in the form of block-like mostly.
With the raising of firing temperature, bulk is separated at 500 DEG C, forms fraction of threadiness, and at 600~700 DEG C, layer fibrosis is bright
Aobvious, the carbon of fritter also starts presentation layer threadiness.
The result shows that Carbon fibe is fired more thorough, and crystal is smaller, laminated fiber structure when temperature is higher
It is apparent.The completeness for comprehensively considering energy conservation and firing, the present invention carry out the conjunction of next step using the Carbon fibe of 600 DEG C of firings
At experiment.
2, the activation of Carbon fibe
(1) it is ground into powder in the beaker of Carbon fibe equipped with 1.5~2.0g one step up and 3.0~5.0mL phosphoric acid is added
Solution (volume ratio of phosphoric acid and water is 1:5~15 in phosphoric acid solution), is placed in 60 DEG C of baking oven and activates 90min.
(2) it is taken out after activating, solution is filtered, then with distilled water flushing filter residue to neutral or close neutrality.It again will filter
Paper and filter residue are placed on together inside 110 DEG C of baking oven, and drying to constant weight to get activated carbon fibre is arrived, and are stored up in wide-mouth bottle
It deposits.
3, the preparation of Carbon fibe and ferrocene composite material
Using solid phase reaction: active carbon fibre 0.5~0.7g of the peacekeeping ferrocene for taking 0.3~0.5g to prepare is in grinding ware
In, with grinding pestle abrasive flour 1.0~2.0 hours, grinding uniformly, kept it uniformly mixed and sufficiently compound, composite granule is made
Material (solid powder).
It is found in inventor team research process, in material preparation method of the invention, solid phase reaction saves solvent and anti-
It is environmentally protective between seasonable；And material ultravioletvisible absorption effect is very strong.But solid phase reaction has to grinding uniformly, to guarantee
Grinding uniformly, can be segmented during the grinding process and take a certain amount of a little sample, weigh after washing away ferrocene with dehydrated alcohol, if twice
Quality relative error of weighing then shows that grinding is uniform 0.1~0.2%.
The detection of embodiment 2 Carbon fibe and ferrocene composite material
1, XRD is detected
The solid powder (i.e. Carbon fibe and ferrocene composite material) that ground ware is ground is taken into the appropriate detection for carrying out XRD.
As a result as shown in figure 5, there are peak values 47.63, the feature which is iron is compared according to PDF standard card
Peak, it was demonstrated that the presence of iron illustrates polished solid powder, carbon with ferrocene compound success.
2, solid ultraviolet detection
The solid powder (i.e. Carbon fibe and ferrocene composite material) that ground ware is ground is taken into appropriate carry out outside solid violet
Detection.
As a result as shown in fig. 6, can be clearly seen that complex solid dusty material maximum absorption wavelength is located at
240nm, 433nm, there is very strong ultravioletvisible absorption effect in 200~550nm wave-length coverage, have portion in 550~800nm
Divide visible absorbance effect.
Experiment shows the composite material ultravioletvisible absorption wider range, is expected to do full ultravioletvisible absorption material and application
In fields such as photovoltaic material, electronic devices.
The optimization of embodiment 3 Carbon fibe and ferrocene complex method
1, the preparation and activation of Carbon fibe be with embodiment 1, and difference is the complex method of Carbon fibe and ferrocene using molten
Agent method, specifically: the ferrocene for the active carbon fibre peacekeeping 0.9301g for taking 0.6032g to prepare is added in a round bottom flask
30mL, nitrile make solvent, stirrer, above flask plus spherical condensating tube, water flowing, and heating stirring 2h under conditions of 65 degrees Celsius,
Keep its compound.It will be stirred at reflux condensation, obtain orange black microcrystalline powder after being precipitated within 1~3 day.
2, the results show that this method not only expends solvent and time, it is often more important that obtained material ultravioletvisible absorption effect
The material of the method for the present invention preparation should be significantly smaller than.
Claims (6)
1. a kind of preparation method of the strong UV, visible light powder body material compound based on Carbon fibe and ferrocene, which is characterized in that packet
Include following steps:
S1. Carbon fibe is fired using sugarcane skin: using H3PO4After solution and distilled water successively clean up fresh sugarcane skin,
102~110 DEG C drying to constant weight, is crushed, 500~700 DEG C of 1.5~2.5 h of calcining make its carbonization, are then ground to powdered；
S2. prepare activated carbon fibre: the Carbon fibe that step S1 is obtained is added in phosphoric acid solution, 50~70 DEG C of activation 80~100
min；Then solution is filtered, then with distilled water flushing filter residue to neutrality；Again by filter paper and filter residue together at 100~120 DEG C
Drying to constant weight to get activated carbon fibre is arrived；
S3. Carbon fibe and ferrocene composite material are prepared using solid phase reaction: is ground after active carbon fibre peacekeeping ferrocene is mixed
Uniformly, it is uniformly mixed it and sufficiently compound, obtained composite powder material.
2. preparation method according to claim 1, which is characterized in that the quality of active carbon fibre peacekeeping ferrocene in step S3
Than for 3~5:5~7.
3. preparation method according to claim 1, which is characterized in that the time of grinding described in step S3 is 1.0~2.0
Hour.
4. preparation method according to claim 1, which is characterized in that the H3PO4H in solution3PO4With the volume of distilled water
Than for 1:15~25.
5. preparation method according to claim 1, which is characterized in that the volume ratio of phosphoric acid and water is in the phosphoric acid solution
1:5~15.
6. preparation method according to claim 1, which is characterized in that the mass volume ratio of the Carbon fibe and phosphoric acid solution
For the mL of 1.5~2.0 g:3.0~5.0.
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| CN201710225403.XA CN107099271B (en) | 2017-04-07 | 2017-04-07 | A kind of strong UV, visible light powder body material and preparation method thereof compound based on Carbon fibe and ferrocene |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1090300A (en) * | 1993-12-27 | 1994-08-03 | 中国科学院上海有机化学研究所 | A kind of controllably graded polyolefine plastics, manufacturing and application that contains aminoalkyl ferrocene derivative |
| CN102504460A (en) * | 2011-11-11 | 2012-06-20 | 苏州大学 | Sweetcane bark fiber composite and preparation method thereof |
| CN103495402A (en) * | 2013-08-30 | 2014-01-08 | 蚌埠凤凰滤清器有限责任公司 | Modified activated carbon absorb based desulfurizer for absorbing ultraviolet ray and its preparation method |
| CN106118595A (en) * | 2016-07-06 | 2016-11-16 | 安徽科技学院 | A kind of method that quartz sand mine tailing prepares uv absorption powder body material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1090300A (en) * | 1993-12-27 | 1994-08-03 | 中国科学院上海有机化学研究所 | A kind of controllably graded polyolefine plastics, manufacturing and application that contains aminoalkyl ferrocene derivative |
| CN102504460A (en) * | 2011-11-11 | 2012-06-20 | 苏州大学 | Sweetcane bark fiber composite and preparation method thereof |
| CN103495402A (en) * | 2013-08-30 | 2014-01-08 | 蚌埠凤凰滤清器有限责任公司 | Modified activated carbon absorb based desulfurizer for absorbing ultraviolet ray and its preparation method |
| CN106118595A (en) * | 2016-07-06 | 2016-11-16 | 安徽科技学院 | A kind of method that quartz sand mine tailing prepares uv absorption powder body material |
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