CN106442497A - Preparation method of porphyrin/nano porous fiber membrane hydrogen chloride gas sensor - Google Patents
Preparation method of porphyrin/nano porous fiber membrane hydrogen chloride gas sensor Download PDFInfo
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- CN106442497A CN106442497A CN201610841765.7A CN201610841765A CN106442497A CN 106442497 A CN106442497 A CN 106442497A CN 201610841765 A CN201610841765 A CN 201610841765A CN 106442497 A CN106442497 A CN 106442497A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/783—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour for analysing gases
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
The invention relates to a preparation method of a porphyrin/nano porous fiber membrane hydrogen chloride gas sensor. The preparation method is characterized in that a nano porous fiber membrane with graded nano pores is directly spun on the fiber surface by a 'one-step' electrostatic spinning technology. The porphyrin/nano porous fiber membrane prepared by the method has high detection sensitivity on hydrogen chloride gas while the minimum detection limit is 34ppb; the sensing response is fast that color change can be generated in 1s, and the color change is visible by naked eyes without depending on other devices; and moreover, the porphyrin/nano porous fiber membrane realizes repeated use and real-time detection and has broad application prospects in the fields such as environmental protection, chemical control, household alarm, food preservation, aerospace and public security and customs.
Description
Technical field
The invention belongs to gas sensing techniques field is and in particular to a kind of porphyrin/nano-porous fiber film hydrogen chloride gas
The preparation method of sensor.
Technical background
Hydrogen chloride (HCl) is the product of conventional industrial chemicals and chemical process, for example：Chloride waste is when burning
90% all can be converted to HCl gas.And HCl gas has high excitant and corrosivity, pollute the environment and damage health,
Therefore at-once monitor is carried out to the HCl gas concentration in environment most important.Now, HCl gas has become as countries in the world ring
One of first-selected monitoring object of indusrial toxic harmful waste gas of border protective tissue.The U.S. is classified as HCl as the work that environmental protection must be surveyed
Industry toxic and harmful；The HCl gas content of European regulation industry and waste incineration discharge not can exceed that 10mg m-3；China
《Discharge standard of air pollutants》(GB 16297-1996) also specify HCl gas highest permission concentration of emission
2.3mg·m-3.So, develop a kind of highly sensitive HCl gas sensing material and there is very high practical significance.
At present, the detection method of HCl gas mainly has AAS and ion selective electrode method, however it is necessary that the valency of dependence
Lattice are expensive, the detecting instrument of complex operation, and do not enable real-time online detection.Therefore, in the urgent need to developing a kind of Gao Ling
Sensitivity, quick response, portable gas sensor simple to operate, cheap, in real time, quickly and accurately detects HCl
Gas.
Content of the invention
The purpose of the present invention be using a kind of simply effectively and the controlled method of electrostatic spinning of technique to prepare porphyrin/nanometer many
Hole tunica fibrosa, and for making gas sensor to verify its HCl Leakage inspection and warning aspect in the industrial production
Application.The present invention pass through by have excellent electromagnetically, the porphyrin chemical combination of the characteristic such as light sensitivity and chemical catalysis activity
Thing is dissolved in the mode in electrostatic spinning liquid, causes, based on solvent-nonsolvent, the mechanism that is separated, has prepared porphyrin/nanoporous
Tunica fibrosa, drastically increases the sensitivity of sensor and the response speed accelerating sensor, further promotes such sensing
Device is in the application of field of industrial production.
Sensor obtained by the present invention, in addition to having the advantage of high sensitivity, quick response, also has good choosing
Selecting property, repeatability and moisture-resistant degree interference.The detection to HCl gas in room temperature of this sensor is limited to 34ppb, to concentration is
The HCl gas response time of 100ppm is less than 1s, and reaches in 5s and be responsive to peak response.Therefore, it can to HCl gas
Leakage is quickly detected and is reported to the police.
A kind of preparation method of the HCl gas sensor of porphyrin/nano-porous fiber film provided by the present invention, including such as
Lower step：
(1) a certain amount of solubility porphyrins is added in high polymeric solution, be stirred at room temperature to being completely dissolved, obtain
Electrostatic spinning liquid；By in the spinning solution being obtained injection electrostatic spinning apparatus, in room temperature, relative humidity is 10-90%, and voltage is
14-25kV, spinning speed is 0.5-1.5mL h-1, receiving range be 10-25cm under the conditions of carry out " one-step method " electrostatic spinning,
Prepare porphyrin/nano-porous fiber film.
Described soluble porphyrins is four (to amino) phenyl porphyrin, tetraphenylporphyrin, four (para hydroxybenzenes
Base) porphyrin；High polymer is polystyrene, polymethyl methacrylate；Described high polymeric solution solvent for use is oxolane, N,
Dinethylformamide；The ratio that described solvent uses is 1: 1-9: 1；The concentration of described high polymeric solution is about 10-
30w.t.%；The addition of described porphyrins is 1.0-3.0mg mL-1；
(2) above-mentioned prepared porphyrin/nano-porous fiber film is placed in vacuum drying oven, at 40 DEG C, 12- is dried
After 36h, it is cut into the sheet material of certain size, thus obtaining porphyrin/nano-porous fiber film HCl gas sensor.
The mechanism of the present invention can be regarded as：It is molten that soluble porphyrins is dissolved in high polymer/solvent/non-solvent ternary
Carry out electrostatic spinning in liquid, using the quick volatilization of solvent in spinning process, so that jet is produced thermodynamic instability and be separated,
Then, high polymer " concentrated phase " place becomes continuous fibrous body, and " dilute phase " place then forms the micropore of fiber surface, is homogeneously born
Carry the nano-porous fiber film of porphyrin.
The gas of the porphyrin/nano-porous fiber film HCl gas sensor of present invention preparation detects that mechanism is：Porphyrin
It is the molecule of a big π key with 26 electronics in 24 centers, its molecule is planar structure, there is big ring rigid stable construct
With plane conjugated nature, the energy level difference reduction between MO highest occupied molecular orbital energy level and minimum orbital energy level, its transmission
Electronics more quickly and effectively, central nitrogen atom has lone pair electrons, can be coordinated with H+, thus planar structure is destroyed.So
When detecting HCl gas, obvious color change and the change of absorption spectrum can occur.And this complexation reaction is reversible reaction,
So the porphyrin being obtained by the present invention/nano-porous fiber film HCl gas sensor can be reused, greatly reduce reality
Cost during the use of border and the secondary pollution to environment.
Compared with prior art advantages of the present invention is as follows：
(1) present invention adopts " one-step method " electrostatic spinning technique, causes the mechanism that is separated, Direct Spinning according to solvent-nonsolvent
Make the nano-porous fiber film that fiber surface has classifying nano hole.Achieved porphyrin and height by way of solution blending
Polymers is homogeneously blended into fibre.The porphyrin prepared by the method/nano-porous fiber film shows fabulous pliability, and porphyrin
Molecule be evenly distributed in fiber surface so that tunica fibrosa colour developing uniformly, color saturation is high, facilitate look at color change and
Accurately measure spectrum information.
(2) HCl gas sensor provided by the present invention adopts porphyrin/nano-porous fiber film is sensing material, than general
The specific surface area of logical solid membrane improves the 1-2 order of magnitude, increases the interaction with tested substance for the porphyrin, and gas diffusion
Speed, improves detection sensitivity and sensing response speed, to the detection range of HCl gas extensively, 34ppb-3000ppm with
On.
(3) HCl gas sensor provided by the present invention is reusable, and 10- extensive to ambient humidity accommodation
90%, color change naked eyes are visible, need not rely on miscellaneous equipment, low cost of manufacture, can carry out real-time detection.
Brief description
Fig. 1 is the ESEM schematic diagram of the embodiment of the present invention 1 mesoporphyrin/pipe/polyhenylethylene nano porous fiber film.
Fig. 2 is that the embodiment of the present invention 1 mesoporphyrin/pipe/polyhenylethylene nano porous fiber film is contacted with variable concentrations HCl gas
Uv-visible absorption spectra change schematic diagram after 30s.
Fig. 3 is the embodiment of the present invention 3 mesoporphyrin/pipe/polyhenylethylene nano porous fiber film is the HCl gas of 100ppm with concentration
Body contacts the change of sensitivity schematic diagram after different time.
Specific embodiment
Embodiment 1
Weigh 1.0g polystyrene (PS) powder and add oxolane (THF) and DMF (DMF) volume
Ratio, in the mixed solvent for 4: 1, stirs under normal temperature and is completely dissolved to PS, obtains the PS/THF/DMF that concentration is 20w.t.% molten
Liquid.Then, weigh 0.013g tetra- (to amino) phenyl porphyrin, be slowly added into while stirring in PS solution obtained above, often
Lower stirring to the porphyrin of temperature is completely dissolved, prepared spinning solution.Above-mentioned spinning solution is added in electrostatic spinning apparatus, spinning condition
For：Room temperature, relative humidity 50%, spinning voltage 18kV, receiving range 18cm, spinning speed 1.0mL h-1, spin certain time
Prepare thickness and be about 0.1mm porphyrin/pipe/polyhenylethylene nano porous fiber film.Porphyrin/pipe/polyhenylethylene nano the porous that will be obtained
Tunica fibrosa contacts 5s at room temperature with the HCl gas of 100ppm concentration, and the color of tunica fibrosa is changed into green from pink.
Embodiment 2
Take 1.0g PS powder to be added in the THF/DMF mixed solvent for 1: 1 for the volume ratio, be continuously stirring to it completely molten
Solution, makes the PS solution liquid that concentration is 10w.t.%, adds 0.01g tetraphenylporphyrin, stir to dissolving, prepared spinning
Liquid.Above-mentioned spinning solution is added in electrostatic spinning apparatus, spinning condition is：Room temperature, relative humidity 70%, spinning voltage
14kV, receiving range 10cm, spinning speed 0.5mL h-1, spin out porphyrin/PS nano-porous fiber air-sensitive color-changing membrane；Put again
12h is dried in 40 DEG C of vacuum drying ovens, is then cut into the disk of a diameter of 1cm, make porphyrin/pipe/polyhenylethylene nano porous fine
Dimension film HCl gas sensor.Sample is placed in an airtight sensing chamber, is passed through the HCl that concentration is 0-100ppm successively
Gas, in room temperature, under the conditions of relative humidity is 50%, allows sample and HCl gas haptoreaction 30s, and with EVOLUTION 220
The uv-visible absorption spectra of type uv-visible absorption spectra instrument (Thermo, USA) test sample.Sample is connect with HCl gas
After touching reaction, continuously it is passed through N in sensing chamber2Carry out HCl gas De contamination, be passed through 1min every time, in triplicate to sample
Color and uv-visible absorption spectra recover.The sensor being obtained using the present invention detect HCl gas when, its ultraviolet-
Visible absorption spectra there occurs significant changes.Constantly increase with HCl gas concentration, script TPP Soret band at 418nm
The intensity of characteristic absorption peak is gradually reduced, and red shift occurs, and after red shift 24nm, creates a new absorption at 442nm
Peak, meanwhile, the absorption peak strength of this new generation increases with the increase of HCl gas concentration.
Embodiment 3
Take 1.0g PS powder to be added in the mixed solvent of THF/DMF for 9: 1 for the volume ratio, be continuously stirring to it complete
Dissolving, makes the PS solution liquid that concentration is 30w.t.%, adds 0.01g tetraphenylporphyrin, stir to dissolving, prepared spinning
Liquid.Above-mentioned spinning solution is added in electrostatic spinning apparatus, spinning condition is：Room temperature, relative humidity 30%, spinning voltage
15kV, receiving range 20cm, spinning speed 1.0mL h-1, spin out porphyrin/PS nano-porous fiber air-sensitive color-changing membrane.To make
The nano-porous fiber film obtaining contacts 5s with the HCl gas of 100ppm concentration at room temperature, and the color of tunica fibrosa is by pink discoloration
For green.
Embodiment 4
Weigh 1.0g polymethyl methacrylate (PMMA) particle and add dichloromethane and DMF volume
Ratio, in the mixed solvent for 4: 1, stirs under normal temperature and is completely dissolved to PMMA, obtains the PMMA solution that concentration is 20w.t.%.So
Afterwards, weigh 0.02g tetra- (p-hydroxybenzene) porphyrin, be slowly added into while stirring in PMMA solution obtained above, under normal temperature
Stir and be completely dissolved to porphyrin, prepared spinning solution.Above-mentioned spinning solution is added in electrostatic spinning apparatus, spinning condition is：Room
Temperature, relative humidity 90%, spinning voltage 25kV, receiving range 20cm, spinning speed 1.5mL h-1, spinning certain time preparation
Go out thickness and be about 0.1mm porphyrin/PMMA nano-porous fiber film；It is placed in 40 DEG C of vacuum drying ovens again and 12h is dried, be then cut into
The disk of a diameter of 1cm, makes porphyrin/PMMA nano-porous fiber film HCl gas sensor.By sample be placed on one close
In the sensing chamber closing, be passed through the HCl gas that concentration is 100ppm, in room temperature, under the conditions of relative humidity is 50%, allow sample with
HCl gas haptoreaction 0-30s, and tested not with EVOLUTION 220 type uv-visible absorption spectra instrument (Thermo, USA)
Uv-visible absorption spectra with sample under the reaction time.After sample and HCl gas haptoreaction, continuous in sensing chamber
It is passed through N2Carry out HCl gas De contamination, be passed through 1min every time, in triplicate to color and the ultraviolet-ray visible absorbing light of sample
Spectrum is recovered.The sensor being obtained using the present invention only needs 5s just can reach peak response to the response time of HCl gas, contact
When time is about 1s, just can substantially observe its color and the change of absorption spectrum, response speed is extremely quickly it is adaptable to HCl
Real-time, the quick detection of gas.
Claims (1)
1. a kind of preparation method of porphyrin/nano-porous fiber film HCl gas sensor is it is characterised in that include following walking
Suddenly：
(1) a certain amount of solubility porphyrins is added in high polymeric solution, be stirred at room temperature to being completely dissolved, obtain electrostatic
Spinning solution；By in the spinning solution being obtained injection electrostatic spinning apparatus, in room temperature, relative humidity is 10-90%, and voltage is 14-
25kV, spinning speed is 0.5-1.5mL h-1, receiving range be 10-25cm under the conditions of carry out " one-step method " electrostatic spinning, preparation
Porphyrin/nano-porous fiber film；
Described soluble porphyrins is four (to amino) phenyl porphyrin, tetraphenylporphyrin, four (p-hydroxybenzene) porphin
Quinoline；
Described high polymer is polystyrene, polymethyl methacrylate；
Described high polymeric solution solvent for use is dichloromethane, oxolane, DMF；
The ratio that described solvent uses is 1: 1-9: 1；
The concentration of described high polymeric solution is about 10-30w.t.%；
The addition of described porphyrins is 1.0-3.0mg mL-1；
(2) above-mentioned prepared porphyrin/nano-porous fiber film is placed in vacuum drying oven, at 40 DEG C, 12-36h is dried
Afterwards, it is cut into the sheet material of certain size, thus obtaining porphyrin/nano-porous fiber film HCl gas sensor.
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| CN201610841765.7A CN106442497A (en) | 2016-09-21 | 2016-09-21 | Preparation method of porphyrin/nano porous fiber membrane hydrogen chloride gas sensor |
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| CN201610841765.7A CN106442497A (en) | 2016-09-21 | 2016-09-21 | Preparation method of porphyrin/nano porous fiber membrane hydrogen chloride gas sensor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109975283A (en) * | 2019-04-10 | 2019-07-05 | 内蒙古农业大学 | Visual indicating label of a kind of identification Meat and preparation method thereof and application |
| CN110006886A (en) * | 2019-04-24 | 2019-07-12 | 江苏大学 | A kind of nanosizing color sensitive sensor and its method for differentiating wheat moulding ability |
| CN116609401A (en) * | 2023-07-21 | 2023-08-18 | 南方电网数字电网研究院有限公司 | HCl sensor, doped carbon nanotube material, preparation method and application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109975283A (en) * | 2019-04-10 | 2019-07-05 | 内蒙古农业大学 | Visual indicating label of a kind of identification Meat and preparation method thereof and application |
| CN110006886A (en) * | 2019-04-24 | 2019-07-12 | 江苏大学 | A kind of nanosizing color sensitive sensor and its method for differentiating wheat moulding ability |
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| CN116609401A (en) * | 2023-07-21 | 2023-08-18 | 南方电网数字电网研究院有限公司 | HCl sensor, doped carbon nanotube material, preparation method and application |
| CN116609401B (en) * | 2023-07-21 | 2024-01-23 | 南方电网数字电网研究院有限公司 | HCl sensor, doped carbon nanotube material, preparation method and application |
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