CN106031860A - Nano-porous material pore channel inner surface plasma modification treatment method and application - Google Patents
Nano-porous material pore channel inner surface plasma modification treatment method and application Download PDFInfo
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Abstract
The invention provides a nano-porous material pore channel inner surface plasma modification treatment method. The method comprises the step that a nano-porous material is treated in different atmospheres in a normal-temperature and atmospheric-pressure dielectric barrier discharge mode, wherein the output power is controlled to range from 80 w to 110 w, the treatment time ranges from 20 min to 40 min, the alternating current power supply amplitude ranges from 30 KV to 50 KV, and the frequency can be adjusted between 5 KHz and 20 KHz. The nano-porous material treated with plasma is subjected to organic functional modification in pore channels, and the modified nano-porous material can serve as an efficient adsorption material; when the nano-porous material treated with plasma is subjected to metal loading, the metal-loaded nano-porous material can serve as an efficient catalyst.
Description
Technical field
The present invention relates to the modification treatment technology of nano-porous materials inner surfaces of pores, especially a kind of etc.
Gas ions modification processing method.
Background technology
Nano-porous materials is due to its abundant pore passage structure, and specific surface area is big, can realize functionalized modification
Etc. excellent specific property, in fields such as adsorbing separation, catalysis, medicine bioengineerings, it is with a wide range of applications.
In the modification of common nano-porous materials, the site energy of duct port is high, and functional group repaiies
Decorations easily occur in aperture, cause duct to block, and the load capacity of functionalization material is low.Therefore, hole is strengthened
Road inner surface activity, increase surface active groups quantity, develop a kind of more excellent method of modifying, make
Obtain functionalization material and be uniformly distributed significant in duct.
Plasma technique passes through electrion, produces a large amount of high-energy electron, ion, free radical etc.
Active particle, is a kind of material surface treatment method quick, uniform, efficient.Such as Li Shou in 2010
" the utilizing the plasma discharge method to elongated insulation tube modifying inner surface under normal pressure " of wise man's application
(CN101876065A) propose under macro-scale internal surface of elongated tube Plasma modification method；
" surface of nanometer zinc oxide atmospheric pressure, the normal-temperature plasma modification process of the application such as Zhang Yingchen in 2009
Method " (CN 101428844A), it is proposed that the method modified to nano granular of zinc oxide outer surface, change
Having become the surface nature of material, structure and form, these results show that Cement Composite Treated by Plasma can be successful
Outer surface for material processes.It is well known that, the internal specific surface area in the duct of porous material
Being far longer than the external area of material, the hugest duct inner ratio surface area imparts porous material merit
The probability of energyization, the activity therefore improving inner surfaces of pores is key technology.
In the mode that multiple plasma produces, dielectric barrier discharge (DBD) is that one is the most non-flat
Weighing apparatus gas discharge, can be carried out under normal pressure, low temperature.DBD discharge process is by numerous micro-electric current
Carrying out micro discharge composition, these micro discharges, in time, spatially random distribution, are formed the most uniform
, large-area plasma.The present invention by DBD plasma application in nano-porous materials duct
The process of inner surface, improves inner surfaces of pores activity, and the functionalization that nano-porous materials is greatly improved is repaiied
Decorations efficiency, makes material have absorption and the catalysis of excellence.
Summary of the invention
It is an object of the invention to provide at the plasma modification of a kind of nano-porous materials inner surfaces of pores
Reason method, solves low, high the asking of process duration, cost few, active of inner surfaces of pores radical amount
Topic.The nano material obtained after treatment is modified and metal load through organic functional, can be as height
The adsorbent of effect and catalyst.
The present invention adopts the following technical scheme that and uses the mode of dielectric barrier discharge under normal temperature and pressure,
Under different atmosphere processing nano-porous materials, its output power, at 80-110 watt, processes
Time is 20-40 minute, obtains the nano-porous materials after Cement Composite Treated by Plasma.
Alternating current power supply amplitude is 25-40 kilovolt, and frequency is adjustable in 5-15 KHz.
It is block media discharge reactor cavity with quartz glass, is placed between two stainless steel electrodes,
It it is highly 8-10 millimeter.
Plasma atmosphere can be oxygen, steam, fluoroform, tetrafluoromethane or noble gas
Deng.
The duct of nano-porous materials can be one-dimensional, two-dimentional, three dimensional structure.
Nano-porous materials after plasma processes carries out organic functional modification in duct, permissible
As efficient absorption material.
Nano-porous materials after plasma processes carries out metal load, can be as efficient catalytic
Agent.
The present invention inner duct surface modification method to nano-porous materials, largely adds and receives
The quantity of rice inner surfaces of pores active group and activity, shorten the time of functional modification, improves function
Change the efficiency modified.
Accompanying drawing explanation
Fig. 1 is surface treating nano porous material plasma medium discharge-blocking device schematic diagram
Fig. 2 is the ultraviolet spectrogram of SBA-15 before and after oxygen plasma processes
Fig. 3 is the infrared spectrogram of SBA-15 before and after fluoro plasma processes
Fig. 4 is the infrared spectrogram of GO before and after oxygen plasma processes
Fig. 5 is the oxygen element x-ray photoelectron spectroscopy of MCF before and after oxygen plasma processes
Fig. 6 is the thermogravimetric analysis figure of SBA-15-NH2 before and after Cement Composite Treated by Plasma
Fig. 7 is the CO2 adsorption desorption curve of amino functional before and after SBA-15 Cement Composite Treated by Plasma
Fig. 8 is the transmission electron microscope picture of MCF-Ag after Cement Composite Treated by Plasma
Fig. 9 is the ultraviolet-visible spectrogram of MCF-Ag catalysis 4-nitrophenol reduction reaction
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Embodiment one
Cement Composite Treated by Plasma nano-porous materials method in the present invention, for different materials and difference
Functional modification, its processing method is similar with principle, and those of ordinary skill in the art only need according to material
The fracture of material component chemical bond and atmosphere generate the complexity of plasma, and regulation processes
Time, voltage, the treatment conditions such as atmosphere.Therefore, this specification mainly provides a typical wiener
Meter You Xu duct silicon dioxide SBA-15, two-dimensional nano porous oxidation Graphene GO, and three-dimensional intercommunication receives
Metre hole road silicon dioxide MCF is as typical case's nano pore model, but is not limited only to above-mentioned material.Deng from
Before and after daughter process, the change of inner surfaces of pores activity uses infrared spectrum, ultraviolet spectra, X-ray light
The methods such as electron spectrum characterize.Nano-porous materials after plasma process is organic in carrying out duct
Functional modification, can be as efficient absorption material.Nano-porous materials after plasma process
Carry out metal load, can be as effective catalyst.Use organo-functional group amido modified and metal is born
Carrying and modify approach respectively as representative functionsization, range of application is not limited only to adsorbent and catalyst
Application.Describe the present invention below in conjunction with detailed description of the invention and accompanying drawing.
The plasma process to SBA-15 under embodiment 1, oxygen atmosphere
In plasma processing apparatus as shown in Figure 1, dielectric impedance under room temperature, normal pressure, is used to put
The mode of electricity, produces voltage, the high frequency of 10 KHz of 40 kilovolts with high tension generator, anti-at quartz
Answer electric discharge in device cavity.Quartz reactor cavity is placed between two stainless steel electrodes, and distance is 8
Millimeter.1 gram of SBA-15 uniformly spreads over the bottom straticulation of reactor, to guarantee that all powder is subject to
The Cement Composite Treated by Plasma that environment is similar.It is passed through oxygen, under conditions of output is 110 watts,
Dielectric barrier discharge produces plasma, processes SBA-15 material 30 minutes, the material note after process
For SBA-15-O.
Before and after Cement Composite Treated by Plasma, the ultraviolet spectrogram of SBA-15 is as in figure 2 it is shown, analysis result shows,
After process, the silicone hydroxyl in SBA-15-O is activated.
The plasma process to SBA-15 under embodiment 2, fluoroform atmosphere
In plasma processing apparatus as shown in Figure 1, dielectric impedance under room temperature, normal pressure, is used to put
The mode of electricity, produces voltage, the high frequency of 15 KHz of 25 kilovolts with high tension generator, anti-at quartz
Answer electric discharge in device cavity.Quartz reactor cavity is placed between two stainless steel electrodes, and distance is 10
Millimeter.1 gram of SBA-15 uniformly spreads over the bottom straticulation of reactor, to guarantee that all powder is subject to
The Cement Composite Treated by Plasma that environment is similar.It is passed through fluoroform gas, is 80 watts at output
Under the conditions of, dielectric barrier discharge produces plasma, processes SBA-15 material 40 minutes, after process
Material be designated as SBA-15-F.
Before and after Cement Composite Treated by Plasma, the infrared spectrogram of SBA-15 is as it is shown on figure 3, analysis result shows,
Containing fluorine in SBA-15-F after process, hydrophobic performance improves.
The plasma process to GO under embodiment 3, oxygen atmosphere
In plasma processing apparatus as shown in Figure 1, dielectric impedance under room temperature, normal pressure, is used to put
The mode of electricity, produces voltage, the high frequency of 5 KHz of 30 kilovolts with high tension generator, anti-at quartz
Answer electric discharge in device cavity.Quartz reactor cavity is placed between two stainless steel electrodes, and distance is 8
Millimeter.1 gram of GO uniformly spreads over the bottom straticulation of reactor, to guarantee that all powder is by environment
The Cement Composite Treated by Plasma that atmosphere is similar.It is passed through oxygen, under conditions of output is 90 watts, medium
Barrier discharge produces plasma, processes GO material 20 minutes, and the material after process is designated as GO-O.
Before and after Cement Composite Treated by Plasma, as shown in Figure 4, analysis result shows the infrared spectrum of GO, after process
Containing more carbon hydroxyl in GO-O.
The plasma process to MCF under embodiment 4, oxygen atmosphere
In plasma processing apparatus as shown in Figure 1, dielectric impedance under room temperature, normal pressure, is used to put
The mode of electricity, produces voltage, the high frequency of 10 KHz of 30 kilovolts with high tension generator, anti-at quartz
Answer electric discharge in device cavity.Quartz reactor cavity is placed between two stainless steel electrodes, and distance is 8
Millimeter.1 gram of MCF uniformly spreads over the bottom straticulation of reactor, to guarantee that all powder is by environment
The Cement Composite Treated by Plasma that atmosphere is similar.It is passed through oxygen, under conditions of output is 100 watts, is situated between
Matter barrier discharge produces plasma, processes MCF material 30 minutes, and the material after process is designated as MCF
-O。
Before and after Cement Composite Treated by Plasma, the oxygen element x-ray photoelectron spectroscopy of MCF is as it is shown in figure 5, analyze
Result shows, containing more silicone hydroxyl in MCF-O after process.
Embodiment 5, the Cement Composite Treated by Plasma effect to SBA-15 amino functional
Take 1 gram of undressed SBA-15, be dispersed in 30 milliliters except in the toluene after water, room temperature
Lower stirring 20 minutes, is slowly added dropwise 3-aminopropyl triethoxysilane, and temperature rising reflux is cold after 18 hours
But, filter, washing, respectively wash three times with toluene and isopropanol, washed rear cold drying overnight,
Obtain the material of amino functional, be designated as SBA-15-NH2.Same condition and step, take 1 gram of oxygen
SBA-15-O after Cement Composite Treated by Plasma, is dispersed in toluene solution, is slowly added dropwise 3-aminopropyl three second
TMOS, heats up, and return time shortens to 2 hours, and same post processing i.e. obtains SBA-15-O
-NH2。
Before and after Cement Composite Treated by Plasma, the thermogravimetric analysis figure of SBA-15-NH2 is as shown in Figure 6, at plasma
Before reason, the SBA-15-NH2 amido modified amount after backflow is 1.56 mMs/gram, at plasma
After reason, the amido modified amount of SBA-15-O-NH2 is 2.43 mMs/gram, modification amount increase by 56%, and
And the response time was shortened to 2 hours by 18 hours.After Cement Composite Treated by Plasma, nano-porous materials is organic
Functional modification effect significantly improves.
Embodiment 6, the CO2 absorption property of amido modified SBA-15
Weigh 0.1 gram of SBA-15-NH2 and SBA-15-O-NH2 obtained by embodiment 5 respectively, put into
In quartz ampoule, measured the absorption of the CO2 of 25 degree of lower two kinds of amino functional samples by gas absorption instrument
Performance, carries out pretreatment, is warmed up to 120 degree, deaerates 6 hours under nitrogen protection sample before measuring,
Then evacuation, is slowly introducing CO2 gas.
The adsorption desorption curve of the CO2 of two kinds of amino functional samples as it is shown in fig. 7, at 25 degree, one
Under atmospheric pressure, SBA-15-O-NH2 is 1.26 mMs/gram to the adsorbance of CO2, and for not etc.
Gas ions processes SBA-15 sample, and after amino functional, CO2 absorbability is only 0.95 mM/gram.
It can be seen that the adsorbance to CO2 significantly increases after material amino functional after Cement Composite Treated by Plasma,
It it is excellent CO2 adsorbent.
Embodiment 7, the Cement Composite Treated by Plasma effect to MCF loading nano silvery
Take the MCF-O after 1 gram of oxygen plasma processes, be dispersed in toluene solution, be slowly added dropwise 3-
Aminopropyl triethoxysilane, heat up, reflux 2 hours, separated after drying, the MCF-O-obtained
NH2 is dispersed in the silver nitrate aqueous solution of 40 milliliters, stirring 10 hours under 40 degree, then filter,
Being dried, under nitrogen protection, calcine 4 hours for 450 degree, powder is become blackish green by original white,
It is designated as MCF-Ag.
Use the structure of transmission electron microscope observation MCF-Ag.As shown in Figure 8, Cement Composite Treated by Plasma
After, MCF still has stable three-dimensional netted nano-porous structure, and substantial amounts of nano-Ag particles is uniformly distributed
At cancellated duct inwall, its average particulate diameter is about 6 nanometers.After Cement Composite Treated by Plasma,
Nano-porous materials has the effect of excellence to metal load.
Embodiment 8, the catalytic performance of MCF-Ag
With 4-nitrophenol reduction reaction as model reaction, investigate the catalytic performance of MCF-Ag.Weigh 0.
04 gram of sodium borohydride, in being dissolved in after the deionized water of 4 milliliters, is 0.5 mmoles with 15 milliliters of concentration
You/liter 4-nitrophenol solution mixing.Use ultraviolet-visible detection reactivity, take 3 milliliters of boron
Sodium hydride and the mixed solution of 4-nitrophenol, put into Ultraviolet Detector, gathers initial 4-nitrophenol
Absworption peak, when not adding MCF-Ag catalyst, uv absorption keep constant, do not occur any
Reaction.Add a certain amount of MCF-Ag catalyst in the solution, build rapidly the lid of sample cell, open
Begin detection sample in 400 nanometers and the change of 290 nanometers absorption peaks.Result as it is shown in figure 9,
Along with the carrying out of reaction, the absworption peak of 4-nitrophenol is gradually reduced, meanwhile, and the suction of PAP
Receipts peak occurs, gradually strengthens.Therefore MCF-Ag is the catalyst of function admirable.
The beneficial effect that the present invention implements
For one-dimensional, two and three dimensions nano-porous materials, nanometer after Cement Composite Treated by Plasma, can be kept many
This body structure of Porous materials, increases quantity and the activity in inner surfaces of pores reactivity site effectively.Aobvious
Write and improve efficiency and the effect that organic functional and metal load etc. are modified.Can be widely applied to catalysis,
The multiple fields such as separation, medicine and environment.
Claims (10)
1. the plasma modification processing method of nano-porous materials inner surfaces of pores, uses
The mode of dielectric barrier discharge under normal temperature and pressure, to nano-porous materials under different atmosphere
Processing, output is 80-110 watt, and the process time is 20-40 minute, exchange
Power supply amplitude is 25-40 kilovolt, and frequency is 5-15 KHz.
2. the processing method described in claim 1, wherein the duct of nano-porous materials is
One-dimensional, two-dimentional or three dimensional structure.
3. the processing method described in claim 1, is block media electric discharge with quartz glass
Reactor cavity, is placed between two stainless steel electrodes, and height is 8-10 millimeter.
4. the processing method described in claim 1, uses oxygen, water vapour, fluoroform
Alkane, tetrafluoromethane or noble gas are atmosphere.
5. the processing method described in claim 1 or 3, wherein nano-porous materials is
SBA-15, atmosphere is oxygen, and voltage is 40 kilovolts, and frequency is 10 KHz,
Electric discharge in quartz reactor cavity, quartz reactor cavity is placed on two stainless steel electrodes
Between, distance is 8 millimeters, and output is 110 watts, and the process time is 30 minutes.
6. the processing method described in claim 1 or 3, wherein nano-porous materials is
SBA-15, atmosphere is fluoroform, and voltage is 25 kilovolts, and frequency is 15 KHz,
Discharging in quartz reactor cavity, quartz reactor cavity is placed on two rustless steel electricity
Between pole, distance is 10 millimeters, and output is 80 watts, and the process time is 40 minutes.
7. the processing method described in claim 1 or 3, wherein nano-porous materials is
GO, atmosphere is oxygen, and voltage is 30 kilovolts, and frequency is 5 KHz, at quartz
Electric discharge in reactor cavity body, quartz reactor cavity is placed between two stainless steel electrodes,
Distance is 8 millimeters, and output is 90 watts, and the process time is 20 minutes.
8. the processing method described in claim 1 or 3, wherein nano-porous materials is
MCF, atmosphere is oxygen, and voltage is 30 kilovolts, and frequency is 10 KHz, at stone
Electric discharge in English reactor cavity body, quartz reactor cavity be placed on two stainless steel electrodes it
Between, distance is 8 millimeters, and output is 100 watts, and the process time is 30 minutes.
9. method described in claim 5 product through amination modify after as gas
The purposes of adsorbent.
10. method described in claim 8 product after silver loads as the use of catalyst
On the way.
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| CN109142136B (en) * | 2018-07-25 | 2021-02-02 | 同济大学 | Device and method for measuring loading depth of functional group on surface of pore channel of modified porous material |
| CN111346620A (en) * | 2018-12-21 | 2020-06-30 | 大庆净达环保科技有限公司 | Modified material with adsorption performance, preparation method and application thereof |
| CN110327879A (en) * | 2019-06-13 | 2019-10-15 | 华中科技大学 | One kind being suitable for flue gas CO2The biomass porous carbon preparation method and product of absorption |
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| CN112973776B (en) * | 2019-12-18 | 2024-03-29 | 中国石油天然气股份有限公司 | Modification method of MCM-22 molecular sieve |
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| CN111375408B (en) * | 2020-02-15 | 2022-07-08 | 中国工程物理研究院材料研究所 | Preparation method and application of iridium oxide nanoparticle catalyst |
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