CN104458815A - High-molecular gas sensitive material as well as preparation method and application thereof - Google Patents
High-molecular gas sensitive material as well as preparation method and application thereof Download PDFInfo
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- CN104458815A CN104458815A CN201410764983.6A CN201410764983A CN104458815A CN 104458815 A CN104458815 A CN 104458815A CN 201410764983 A CN201410764983 A CN 201410764983A CN 104458815 A CN104458815 A CN 104458815A
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Abstract
The invention belongs to the field of gas sensitive materials, and particularly relates to a high-molecular gas sensitive material as well as a preparation method and application thereof. The invention provides the high-molecular gas sensitive material which is a composite material having a conductive network structure and prepared from electro-woven nylon nanometer fiber films modified by conductive fillers. The high-molecular gas sensitive material disclosed by the invention can be used for solving the problem of impossible coexistence of high responsibility and good reversibility and is quite high in responsibility, response rate, resilience speed and recycle rate.
Description
Technical field
The invention belongs to gas sensitive field, be specifically related to a kind of macromolecule gas sensitive and its production and use.
Background technology
Advanced chemical gas test material, need possess low detection extreme value, high responsiveness and the speed of response, good recovery and good physical characteristics (pliable and tough, light etc.) simultaneously.The rigid materials such as traditional chemical gas sensitive material often makes conductive filler by conductor oxidate, quartzy, ceramic do substrate.This inorganic composite materials has higher responsiveness to chemical gas, but the pliability of its high processing temperature and difference greatly limit the application of this material; In addition, this sensitive material is general lower to organic gas response intensity.
Conductive polymer composite (CPC) refers to macromolecular material to be matrix, add various conductive filler through dispersion, mixing, the shaping heterogeneous compound system with conducting function obtained, it has many excellent specific properties of macromolecular material, can in the larger context according to using the electricity, mechanics and other performances that need to regulate material, cost is lower, be easy to shaping and produce in a large number, thus attracts widespread attention.CPC has the physical phenomenon of many uniquenesses, and as resistance versus temperature, pressure, gas concentration susceptibility, current-voltage non-linear behavior, current noise, electric charge dielectric properties are to the dependence etc. of frequency.This makes conductive polymer composite have very high actual application value as a kind of functional high molecule material, also has very high theoretical research to be worth.
The physical property that CPC is good and the sensitivity characteristic to organic gas thereof, make it be widely used in chemical gas detection field.Wherein, the appearance of the process technology such as rotary coating, ink jet printing in recent years, make nano material (carbon nano-tube (CNTs), Graphene (GNPs)) that different pliability substrate (polyethylene terephthalates can be distributed in well, polyamide, paper etc.) on; Lower processing temperature and simple processing technology make these methods be widely used in the production of flexible gas Sensitive Apparatus.As, " Journal of The American Chemical Society " is called 134 (4553) names in 2012 preparation method disclosing a kind of advanced toxic gas detector part in the document of " Flexible, All-Organic Chemiresistor for Detecting Chemically Aggressive Vapors ": be distributed at the bottom of cellulose base with ink jet printing method CNTs.This compound substance is to harmful gas (Cl
2, NO
2) show excellent selectivity and stability, but the slower speed of response becomes the common problem of this type of material, this strongly limits the application of this flexible substrates compound substance in organic gas context of detection.
For CPC gas sensitive material, the contradiction between responsiveness and recovery exists always: interaction strong between chemical gas and compound substance is the origin cause of formation of high-responsivity and the high speed of response; But, strong interaction substantially prolongs the turnaround time of material, even can destroy the structure of material, material recycling rate of waterused is declined, so how to make the responsiveness of material, the speed of response and recovery rate work in coordination with important topic that raising is CPC gas sensitive material field always.
Summary of the invention
The present invention is directed to above-mentioned defect, a kind of new polymeric gas sensitive material is provided, solve the difficult problem that high responsiveness and good recovery can not possess simultaneously; Prepare the polymeric gas sensitive material that responsiveness, the speed of response, recovery rate and recycling rate of waterused are all very high.
The technical scheme that the present invention takes is as follows:
First technical matters to be solved by this invention is to provide a kind of macromolecule gas sensitive, and described macromolecule gas sensitive is the compound substance with conductive network structure that conductive filler and electrospinning nylon nano fiber film are formed.
Described electrospinning nylon nano fiber film is selected from least one in electrospinning nylon 6 (PA6) nano fibrous membrane, electrospinning nylon66 fiber (PA66) nano fibrous membrane, electrospinning nylon 1010 (PA1010) nano fibrous membrane, electrospinning NYLON610 (PA610) nano fibrous membrane or electrospinning nylon 1212 (PA1212) nano fibrous membrane; Described conductive filler is selected from least one in graphene nanometer sheet, carbon black, carbon fiber or carbon nano-tube.In the present invention, described electrospinning nylon nano fiber film is Static Spinning nylon nano fiber film; Electrostatic spinning nano fiber film is namely by tunica fibrosa prepared by electrostatic spinning.
Preferably, the thickness of described electrospinning nylon nano fiber film is 0.3-3 μm, and tunica fibrosa mean diameter is 100-400nm, and tunica fibrosa aperture is 1-6 μm.
Further, the preparation method of described electrospinning nylon nano fiber film is: first nylon and formic acid are mixed with the spinning liquid that mass concentration is 15-25%; Then gained spinning liquid is obtained electrospinning nylon nano fiber film by electrostatic spinning; Wherein, electrospinning condition is: interelectrode distance is 15-30cm, and voltage is 15-35KV, spinning time 1.5-5 hour.
Preferably, the method that conductive filler and electrospinning nylon nano fiber film form compound substance is: conductive filler is distributed in electrospinning nylon nano fiber surface by the mode of ultrasonic disperse, the method of ultrasonic disperse is: first conductive filler is mixed the conductive filler dispersion liquid that obtained mass concentration is 0.03-0.2% with deionized water, then electrospinning nylon nano fiber film is placed in conductive filler dispersion liquid ultrasonic process 2-10min.
Preferably, the mass concentration of described conductive filler dispersion liquid is 0.1%.
Preferred, in conductive filler dispersion liquid, the average-size of conductive filler must not be greater than 5 μm.
Preferably, described electrospinning nylon nano fiber film is PA6 nano fibrous membrane, and described conductive filler is graphene nanometer sheet.
Preferred, the sheet number of plies of described graphene nanometer sheet is less than 30, and thickness is less than 20nm, and purity is greater than 99.5wt%.
Preferably, when described electrospinning nylon nano fiber film is PA6 nano fibrous membrane, the preparation method of described PA6 nano fibrous membrane is: first mixed with formic acid by PA6, within 1-2.5 hour, obtains PA6 solution in 65-75 DEG C of stirring; Then gained PA6 solution is obtained PA6 nano fibrous membrane by electrostatic spinning.
Preferred, when described electrospinning nylon nano fiber film is PA6 nano fibrous membrane, described electrospinning condition is: interelectrode distance is 25cm, and voltage is 30KV, 3 hours spinning time; Receiving trap is the cylinder having copper mesh coated.
Second technical matters that the present invention will solve is to provide the preparation method of above-mentioned macromolecule gas sensitive, electrospinning nylon nano fiber film is placed in conductive filler dispersion liquid ultrasonic process 2-10min, then washs, is drying to obtain macromolecule gas sensitive; Wherein, the preparation method of described conductive filler dispersion liquid is: after conductive filler and deionized water are mixed in 0-5 DEG C of environment ultrasonic disperse 1.5-3.5 hour, ultrasonic power is 285W-570W.
Preferably, in said method, electrospinning nylon nano fiber film is placed in the ultrasonic process of conductive filler dispersion liquid to carry out at ice-water bath.
Preferably, in said method, electrospinning nylon nano fiber film be placed in conductive filler dispersion liquid ultrasonic after, after repeatedly rinsing 2-5 time with deionized water, namely natural drying secures satisfactory grades sub-gas sensitive.
The 3rd technical matters that the present invention will solve is to provide the purposes of above-mentioned macromolecule gas sensitive: macromolecule gas sensitive of the present invention is for detecting polar gas.
Further, described polar gas comprises formic acid, acetic acid, methyl alcohol, ethanol or ammonia.
Beneficial effect of the present invention:
The present invention is with conductive filler, nylon for raw material, makes conductive filler be distributed in nylon fiber surface, form good conductive network, prepare novel nano gas sensitive material by the method for electrostatic spinning and ultrasonic disperse.
The present invention has the following advantages:
1, conductive filler/nylon composite materials of the present invention is as gas sensitive material, and because conductive filler and electrospinning fibre all have less size, therefore compound substance possesses great specific surface area and porosity, and energy and ambient atmos atmosphere interact rapidly; Therefore, ensure that the responsiveness of compound substance, the speed of response dexterously, recovery rate and recycling rate of waterused improve simultaneously.
2, because conductive filler is attached to electrospinning nylon fiber surface, the electric conductivity of compound substance strengthens greatly.
3, the gas sensitive material thickness that obtains of the inventive method is adopted to only have 1.7 μm, soft and light.
4, job operation of the present invention is simple, utilizes job operation of the present invention, remains the pliability of electrospinning nylon nano fiber film, substantially increase the range of application of conductive filler/nylon composite materials.
Accompanying drawing illustrates:
Fig. 1: Fig. 1 a is scanning electron microscope (SEM) picture of the embodiment of the present invention 1 gained Static Spinning PA6 nanofiber, Fig. 1 b is the SEM picture of embodiment 1 gained GNPs/PA6 compound substance, Fig. 1 c, Fig. 1 e are the local SEM picture of GNPs/PA6 compound substance, and Fig. 1 d, Fig. 1 f are respectively the enlarged drawing of Fig. 1 c, Fig. 1 e.
The time m-resistance curve of Fig. 2: under the formic acid atmosphere of variable concentrations, GNPs/PA6.
Fig. 3: under the different organic gas atmosphere of 500ppm, the time m-resistance curve of GNPs/PA6.
Fig. 4: under the different organic gas atmosphere of 500ppm, the response time to different organic gas of GNPs/PA6 and turnaround time.
Fig. 5: under the different organic gas atmosphere of 500ppm, the response intensity to different organic gas of GNPs/PA6.
Embodiment
First technical matters to be solved by this invention is to provide a kind of macromolecule gas sensitive, and described macromolecule gas sensitive is the compound substance with conductive network structure that conductive filler modifies the formation of electrospinning nylon nano fiber film.Conductive filler can be evenly distributed on the material with conductive network structure that electrospinning nylon nano fiber film surface is formed.
Second technical matters that the present invention will solve is to provide the preparation method of above-mentioned macromolecule gas sensitive, electrospinning nylon nano fiber film is placed in conductive filler dispersion liquid ultrasonic process 2-10min, then washs, is drying to obtain macromolecule gas sensitive; Wherein, the preparation method of described conductive filler dispersion liquid is: after conductive filler and deionized water are mixed in 0-5 DEG C of environment ultrasonic disperse 1.5-3.5 hour, ultrasonic power is 285W-570W.
The 3rd technical matters that the present invention will solve is to provide the purposes of above-mentioned macromolecule gas sensitive: macromolecule gas sensitive of the present invention is for detecting polar gas.
In the present invention, with electrospinning nylon nano fiber film for substrate, then conductive filler is evenly distributed on electrospinning nylon nano fiber film surface, makes it form conductive network structure.
Proposition electrospinning nylon nano fiber film of the present invention does substrate, electrospinning nylon nano fiber is modified with conductive filler, increase the contact area of compound substance and extraneous atmosphere by improving the specific surface area of compound substance, thus shorten compound substance response time of atmosphere, the raising compound substance responsiveness of atmosphere and the speed of response to external world to external world.The porosity that electrospinning nylon nano fiber is larger and the great specific surface area of ultrafine fiber considerably increase the contact area of nylon fiber and extraneous atmosphere.Nylon fiber rapid spatial expansion in solvent gas atmosphere, being overlapped on by destruction to a certain degree in very short time between fiber surface conductive filler, composite material resistance improves rapidly; Thus, compound substance has very high responsiveness and the speed of response to solvent gas atmosphere.In air atmosphere, porosity larger between nylon fiber and the great specific surface area of ultrafine fiber impel organic gas to depart from compound substance, and the material electrical property of composite wood is able to rapid reply.The method that the present invention proposes is dexterously by improving the specific surface area of compound substance, thus greatly increase the contact area of compound substance and extraneous atmosphere, shorten the response time of compound substance atmosphere to external world, improve the speed of response of compound substance atmosphere to external world, solve the difficult problem that high responsiveness and good recovery can not possess simultaneously; Prepare the gas sensitive material that responsiveness, the speed of response, recovery rate and recycling rate of waterused are all very high.
The preparation of embodiment 1 macromolecule gas sensing property material
Preparation method: concrete preparation process is as follows:
(1) configuration of PA6 formic acid solution: mixed in the round-bottomed flask of 50ml with 5ml formic acid by 1.5g nylon 6, then 75 DEG C of mechanical blendings 1.5 hours, is configured to nylon 6 solution that massfraction is 20%.
(2) electrostatic spinning: step 1 gained PA6 solution is under the effect of high-pressure electrostatic, Taylor cone can be formed at spinning nozzle place, when electric field intensity reaches a critical value, electric field force just can overcome the surface tension of liquid, forms one charged injection stream at spinning nozzle place; In course of injection, because the surface area of injection stream increases rapidly, solvent volatilizees, and fiber solidifying and unordered shape is arranged on gathering-device, thus to obtain thickness be 0.3-3 μm, and tunica fibrosa mean diameter is 100-400nm, and tunica fibrosa aperture is 1-6 μm of nanofiber; Electrospinning parameters: interelectrode distance is 25cm, voltage is 30KV; Receiving trap is copper mesh.
(3) prepare GNPs dispersion liquid: in ice-water bath, GNPs is placed in deionized water for ultrasonic and disperses 1 hour, form the dispersion liquid (mass concentration of dispersion liquid is 0.1%) of GNPs.
(4) GNPs/PA6 conductive network is prepared: in ice-water bath, PA6 tunica fibrosa is placed in the ultrasonic process of scattered GNPs dispersion liquid 3 minutes, place it in natural drying in air subsequently, (thickness distribution is at 0.3-3 μm to make GNPs/PA6 conducing composite material; Average thickness is 1.7 μm).
Fig. 1 a is scanning electron microscope (SEM) figure of PA6 electrospun fibers film, and from Fig. 1 a: PA6 fiber evenly and smooth surface, fiber morphology is better; The SEM picture of Fig. 1 b:GNPs/PA6, is distributed on PA6 fiber from Fig. 1 b: GNPs, and between hole, distribution is few; The local SEM picture of Fig. 1 c, Fig. 1 e:GNPs/PA6, Fig. 1 d, Fig. 1 f are respectively the enlarged drawing of Fig. 1 c, Fig. 1 e, from Fig. 1 c, Fig. 1 d, Fig. 1 e, have defined good connection between Fig. 1 f: GNPs and fiber.
Performance test:
The formic acid atmosphere 150s that embodiment 1 gained compound substance is placed in variable concentrations is placed on air atmosphere 150s, loop test like this; The concentration of formic acid is respectively 25ppm, 50ppm, 100ppm, 200ppm, 500ppm, 1000ppm, surveys the change of its electrical property.
Fig. 2 is the time m-resistance curve of embodiment 1 gained gas sensitive under the formic acid atmosphere of variable concentrations.As shown in Figure 2: after being placed in formic acid atmosphere, the resistance of gas sensitive can increase sharply; After being placed in air atmosphere, the resistance of gas sensitive can be replied rapidly.And the linear relationship that the responsiveness of sensitive material and formic acid gas concentration are proportionate.
Embodiment 1 gained GNPs/PA6 gas sensitive is placed in ethanol, methylene chloride, cyclohexane, in the atmosphere of ethyl acetate 500ppm, research m-resistance behavior at that time.Fig. 3 is the time m-resistance curve of gas sensitive under the different organic gas atmosphere of 500ppm.As shown in Figure 3: for different gas, the selectivity of the response difference of sensitive material very greatly namely sensitive material is good.
The response time to different organic gas that Fig. 4 is embodiment 1 gained gas sensitive under the different organic gas atmosphere of 500ppm and turnaround time.As shown in Figure 3: for gas with various, the response time of sensitive material is different with turnaround time, but speed of response entirety is very fast.
Fig. 5 is the response intensity to different organic gas of embodiment 1 gained gas sensitive under the different organic gas atmosphere of 500ppm.As shown in Figure 3: for gas with various, the responsiveness of sensitive material is different, and the selectivity further illustrating sensitive material is good.
Found by above-mentioned experiment, the method that invention proposes ensure that responsiveness, the speed of response of compound substance dexterously, and recovery rate and recycling rate of waterused improve simultaneously.Simple job operation and the excellent flexibility of compound substance will be conducive to reducing the production cost of material and applying of material.In addition, the present invention directly uses the Graphene of reduction, and can realize GNPs and PA6 and well combine, and simplifies process largely, reduces processing cost.
Claims (10)
1. macromolecule gas sensitive, is characterized in that, described macromolecule gas sensitive is the compound substance with conductive network structure that conductive filler and electrospinning nylon nano fiber film are formed.
2. macromolecule gas sensitive according to claim 1, it is characterized in that, described electrospinning nylon nano fiber film is selected from least one in electrospinning nylon 6/nanometer tunica fibrosa, electrospinning nylon66 fiber nano fibrous membrane, electrospinning nylon 1010 nano fibrous membrane, electrospinning NYLON610 nano fibrous membrane or electrospinning nylon 1212 nano fibrous membrane; Described conductive filler is selected from least one in graphene nanometer sheet, carbon black, carbon fiber or carbon nano-tube; Preferably, the thickness of described electrospinning nylon nano fiber film is 0.3-3 μm, and tunica fibrosa mean diameter is 100-400nm, and tunica fibrosa aperture is 1-6 μm.
3. macromolecule gas sensitive according to claim 1 and 2, is characterized in that, the preparation method of described electrospinning nylon nano fiber film is: first nylon and formic acid are mixed with the spinning liquid that mass concentration is 15-25%; Then gained spinning liquid is obtained electrospinning nylon nano fiber film by electrostatic spinning; Wherein, electrospinning condition is: interelectrode distance is 15-30cm, and voltage is 15-35KV, spinning time 1.5-5 hour.
4. the macromolecule gas sensitive according to any one of claims 1 to 3, it is characterized in that, the method that conductive filler and electrospinning nylon nano fiber film form compound substance is: conductive filler is distributed in electrospinning nylon nano fiber surface by the mode of ultrasonic disperse, the method of ultrasonic disperse is: first conductive filler is mixed the conductive filler dispersion liquid that obtained mass concentration is 0.03-0.2% with deionized water, then electrospinning nylon nano fiber film is placed in conductive filler dispersion liquid ultrasonic process 2-10min.
5. the macromolecule gas sensitive according to any one of Claims 1 to 4, is characterized in that, the mass concentration of described conductive filler dispersion liquid is 0.1%, and in described conductive filler dispersion liquid, the average-size of conductive filler is not more than 5 μm.
6. the macromolecule gas sensitive according to any one of claim 2 ~ 5, is characterized in that, described electrospinning nylon nano fiber film is electrospinning PA6 nano fibrous membrane, and described conductive filler is graphene nanometer sheet; Preferably, the sheet number of plies of described graphene nanometer sheet is less than 30, and thickness is less than 20nm, and purity is greater than 99.5wt%.
7. macromolecule gas sensitive according to claim 6, is characterized in that, the preparation method of described electrospinning PA6 nano fibrous membrane is: first mixed with formic acid by PA6, within 1-2.5 hour, obtains PA6 solution in 65-75 DEG C of stirring; Then gained PA6 solution is obtained electrospinning PA6 nano fibrous membrane by electrostatic spinning.
8. the preparation method of the macromolecule gas sensitive described in any one of claim 1 ~ 7, is characterized in that, electrospinning nylon nano fiber film is placed in conductive filler dispersion liquid ultrasonic process 2-10min, then washs, is drying to obtain macromolecule gas sensitive; Wherein, the preparation method of described conductive filler dispersion liquid is: after conductive filler and deionized water are mixed in 0-5 DEG C of environment ultrasonic disperse 1.5-3.5 hour, ultrasonic power is 285W-570W.
9. the preparation method of macromolecule gas sensitive according to claim 8, is characterized in that, electrospinning nylon nano fiber film is placed in the ultrasonic process of conductive filler dispersion liquid to carry out at ice-water bath.
10. macromolecule gas sensitive is for detecting polar gas, and described macromolecule gas sensitive is the macromolecule gas sensitive described in any one of claim 1 ~ 7, or the macromolecule gas sensitive adopting the method described in claim 8 or 9 obtained; Described polar gas comprises formic acid, acetic acid, methyl alcohol, ethanol or ammonia.
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| CN107189354A (en) * | 2017-07-07 | 2017-09-22 | 齐鲁工业大学 | A kind of graphene nanometer sheet strengthens the preparation method of carbon fibre composite |
| CN107254158A (en) * | 2017-06-09 | 2017-10-17 | 扬州大学 | Electrical-conductive nanometer composite cellulosic membrane with gas sensitive effect and preparation method thereof |
| CN107966478A (en) * | 2016-10-19 | 2018-04-27 | 华邦电子股份有限公司 | Sensor array, its manufacture method and method for sensing |
| CN110757908A (en) * | 2019-07-12 | 2020-02-07 | 大连工业大学 | Method for synergistically toughening carbon fiber epoxy composite material by using porous nanofiber membrane |
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Inventor after: Dai Kun Inventor after: Li Yong Inventor after: Xu Zhuoyan Inventor after: Wang Yalong Inventor after: Di Wei Inventor after: Liu Chuntai Inventor after: Zheng Guoqiang Inventor before: Dai Kun Inventor before: Li Yong Inventor before: Xu Zhuoyan Inventor before: Wang Yalong Inventor before: Di Wei Inventor before: Liu Chuntai Inventor before: Zheng Guoqiang Inventor before: Shen Changyu |
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Application publication date: 20150325 |