CN107337802B - Gas-sensitive film sensitive to ethanol and acetone and preparation method thereof - Google Patents
Gas-sensitive film sensitive to ethanol and acetone and preparation method thereof Download PDFInfo
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- C08J2401/02—Cellulose; Modified cellulose
- C08J2401/04—Oxycellulose; Hydrocellulose
Abstract
The invention relates to the field of preparation of gas-sensitive films, in particular to a gas-sensitive film sensitive to ethanol and acetone and a preparation method thereof. The preparation method of the gas-sensitive film sensitive to ethanol and acetone comprises the following steps: firstly, coating a thermoplastic polymer nanofiber suspension on a base material, forming a layer of thermoplastic polymer film on the surface of the base material after drying, and tearing the thermoplastic polymer film from the base material; and then preparing a nano microcrystalline cellulose suspension by acid hydrolysis of cellulose, coating the nano microcrystalline cellulose suspension on the surface of the thermoplastic polymer film, and drying to obtain the gas-sensitive film sensitive to ethanol and acetone. The prepared gas-sensitive film can determine whether ethanol or acetone vapor overflows or not through macroscopic morphological change, and can respond to the ethanol vapor and the acetone vapor.
Description
Technical Field
The invention relates to the field of preparation of gas-sensitive films, in particular to a gas-sensitive film sensitive to ethanol and acetone and a preparation method thereof.
Background
The leakage of volatile solvent often appears in the laboratory, especially the solvent of packing more crude, often appears because of the damaged volatile solvent of lid volatilizees in to the air, has not only wasted the solvent, and more serious is influence laboratory operating personnel's is healthy. Common volatile solvents in a laboratory comprise ethanol and acetone, and gaseous acetone belongs to a slightly harmful pollutant and has certain damage to the nervous system of a human body. Because tiny cracks of the cover are not easy to be detected by people, if a gas-sensitive material which can respond to ethanol and acetone is arranged on a solvent bottle cover of the ethanol or the acetone, the existence of leakage of the ethanol and the acetone can be quickly judged through the form change of the gas-sensitive material. For example, in the invention patents of china, patent publication nos. CN 100401548C, CN101813654A and CN 100383995C, CN 105419784a use 9,10- (diphenyl) ethynyl anthracene, ZnO, tin oxide and other materials as responsive materials to be added into fibers or films to make the fibers or films have response capability to ethanol vapor, and all the materials are represented as impedance changes, and ethanol needs to be responded by components such as an ammeter and the like; as another example of the chinese patent, patent publication No. CN 100547389C, CN 100494993C discloses that erbium oxide powder and dysprosium oxide powder are added as responsive materials to zirconia powder and nano strontium carbonate powder to make them have acetone vapor response capability.
At present, the response to ethanol or acetone is generally the response of impedance change, whether ethanol or acetone vapor overflows cannot be determined through macroscopic morphological change, and no gas sensitive material with the response to ethanol and acetone is reported so far.
Disclosure of Invention
In order to solve the above problems, it is an object of the present invention to provide a gas-sensitive film sensitive to ethanol and acetone, which can not only determine whether ethanol or acetone vapor overflows by macroscopic morphological changes, but also respond to both ethanol vapor and acetone vapor, and a method for preparing the same.
In order to achieve the purpose, the technical scheme of the invention comprises the following steps:
the preparation method of the gas-sensitive film sensitive to ethanol and acetone comprises the following steps: firstly, coating a thermoplastic polymer nanofiber suspension on a base material, forming a layer of thermoplastic polymer film on the surface of the base material after drying, and tearing the thermoplastic polymer film from the base material; and then preparing a nano microcrystalline cellulose suspension by acid hydrolysis of cellulose, coating the nano microcrystalline cellulose suspension on the surface of the thermoplastic polymer film, and drying to obtain the gas-sensitive film sensitive to ethanol and acetone.
The better technical scheme for realizing the invention is as follows: the preparation method of the gas-sensitive film sensitive to ethanol and acetone specifically comprises the following steps:
1) preparation of thermoplastic polymer nanofiber suspension: adding the thermoplastic polymer nanofiber into the mixed solvent, and scattering the nanofiber by adopting a homogenizer to obtain a uniformly dispersed thermoplastic polymer nanofiber suspension;
2) preparing a nano microcrystalline cellulose suspension: adding cellulose into an acid solution to perform acid hydrolysis reaction on the cellulose, washing the reaction solution after the reaction is finished, and adding water to dilute the reaction solution to prepare a nano microcrystalline cellulose suspension;
3) preparing a gas-sensitive film sensitive to ethanol and acetone: coating the thermoplastic polymer nanofiber suspension on a base material, air-drying under natural conditions to form a layer of thermoplastic polymer film on the surface of the base material, tearing off the thermoplastic polymer film from the base material, coating the nano microcrystalline cellulose suspension on the surface of the thermoplastic polymer film, and air-drying under natural conditions to obtain the gas-sensitive film sensitive to ethanol and acetone.
Further, in the step 1), the thermoplastic polymer nanofiber is polyvinyl alcohol-ethylene copolymer (PVA-co-PE) nanofiber, Polyamide (PA) nanofiber, polyethylene terephthalate (PET) nanofiber or Polyurethane (PU) nanofiber, the mass percentage concentration of the thermoplastic nanofiber suspension is 0.8% -3%, the mixed solvent is an alcohol-water mixed solution, the mass ratio of alcohol to water is 7: 3-5: 5, and the alcohol is one of n-propanol, isopropanol, n-butanol or tert-butanol.
Further, in the step 2), the cellulose is cotton, wood pulp or sisal; the acid solution is 60-70 wt% of sulfuric acid solution, the mass ratio of cellulose to the acid solution is 1: 8-9, the temperature of acid hydrolysis reaction is 45-55 ℃, the time is 30-50 min, the washing process comprises the steps of firstly centrifuging the reaction solution, washing with pure water, and then dialyzing with the pure water until the pH value is stable, wherein the mass percentage concentration of the nano microcrystalline cellulose suspension is 0.5-5%.
Further, in the step 3), the base material is one of PET cloth, PP melt-blown cloth, polypropylene non-woven cloth or PP non-woven cloth; the thickness of the thermoplastic polymer nanofiber suspension coated on the base material is 10-80 microns.
Among them, the preparation method of the thermoplastic polymer nanofiber is referred to the preparation method described in patents CN105148996A, CN 104014196B, CN 103884695 a. The method comprises the steps of fully melting and blending two thermodynamically incompatible polymers in a double-screw melting extruder, extruding, subjecting the blended polymer melt to the action of a shearing force and a stretching composite force field in the extruder and a spinneret to elongate and deform to form a nanofiber bundle, and finally removing the matrix polymer to obtain the thermoplastic polymer nanofiber. Taking the preparation of the polyvinyl alcohol-ethylene copolymer nano-fiber as an example, the preparation method comprises the following steps: blending polyvinyl alcohol-ethylene copolymer (PVA-co-PE) and Cellulose Acetate Butyrate (CAB), extruding by a double-screw melt extruder, and removing CAB by using acetone to obtain the polyvinyl alcohol-ethylene copolymer nanofiber.
The gas-sensitive film sensitive to the ethanol and the acetone is prepared by the preparation method of the gas-sensitive film sensitive to the ethanol and the acetone. The gas-sensitive film comprises two layers of composite films, wherein one layer is a thermoplastic polymer film, and the other layer is a nano microcrystalline cellulose film coated on the surface of the thermoplastic polymer film.
The gas-sensitive film sensitive to ethanol and acetone is applied to the gas-sensitive flexible sensor of ethanol and acetone. The method for preparing the flexible sensor is different from the conventional flexible sensor, and the sensitive film of the conventional flexible sensor is an impedance sensitive film and needs to be added with an electrode, an ammeter and the like. The gas-sensitive film prepared by the invention is placed in a breathable protective shell, the breathable protective shell provided with the gas-sensitive film is placed above a bottle cap, and whether the ethanol or the acetone leaks or not can be quickly judged by observing the bending change of the gas-sensitive film.
The principle that the gas-sensitive film prepared by the invention can realize sensitive response to ethanol and acetone is that cellulose is a linear polymer formed by connecting D-glucopyranosyl as a basic structural unit through β -1, 4 glycosidic bonds, the cellulose is treated by means of common acid hydrolysis method, alkali method, biological enzymolysis method, mechanical physical treatment method and the like, a non-crystallization area in the cellulose structure can be removed, so that nano microcrystalline cellulose is prepared, the nano microcrystalline cellulose is used as a novel functional polymer material and has the properties of excellent physical property, large specific surface area, high crystallinity, good biocompatibility and the like.
The invention has the advantages that:
1, because pure nanocrystalline cellulose is very brittle and poor in flexibility after being formed into a film, the nanocrystalline cellulose suspension is coated on the surface of a thermoplastic nanofiber film, so that the thermoplastic nanofiber film has the flexibility of thermoplastic nanofibers and the humidity response performance of nanocrystalline cellulose.
2, the nano microcrystalline cellulose and the thermoplastic nanofiber are both in a nano level, and after the nano microcrystalline cellulose is coated on the surface of the thermoplastic nanofiber membrane, the thermoplastic nanofiber membrane has certain holes and larger specific surface area and is more sensitive to the overflow of ethanol and acetone steam.
3, the prepared gas-sensitive film has high sensitivity and very short response time, and the recovery speed is very quick when the environment is not changed.
Drawings
FIG. 1 is a SEM image of a gas-sensitive film sensitive to ethanol and acetone prepared in example 1 at a magnification of 5000 times;
FIG. 2 is a graph showing the response time and recovery time of the gas-sensitive film sensitive to ethanol and acetone prepared in example 2; in the figure, ethanol steam stimulation is given at 0-2s, and the ethanol steam stimulation is removed after 2 s;
FIG. 3 is a graph of the cycle performance of the ethanol and acetone sensitive gas sensitive film of example 2 responding 20 times to ethanol vapor;
FIG. 4 is a photograph showing the rapid response of the gas-sensitive film sensitive to ethanol and acetone prepared in example 1 to acetone vapor; FIG. 4A is a plan view of the gas-sensitive film just after being placed on a beaker containing acetone, and FIG. 4B is a curved view of the gas-sensitive film after 1.5s, with a bending angle of 55 °;
fig. 5 is a photograph showing the rapid response of the gas-sensitive film sensitive to ethanol and acetone prepared in example 2 to ethanol vapor. Fig. 5A is a flat view of the gas-sensitive film immediately after being placed on an ethanol beaker, and fig. 5B is a curved view of the gas-sensitive film after 2s, with a bending angle of 65 °.
Detailed Description
For a better understanding of the present invention, reference will now be made in detail to the present invention, examples of which are illustrated in the accompanying drawings.
Example 1
The preparation method of the gas-sensitive film sensitive to ethanol and acetone comprises the following steps:
1) preparation of thermoplastic polymer nanofiber suspension: adding PVA-co-PE nano-fibers into an alcohol-water mixed solution, wherein the alcohol-water mixed solution is a mixed solution of n-propanol and water, and the mass ratio of the n-propanol to the water is 7:3, and scattering the nano-fibers by adopting a homogenizer to obtain a uniformly dispersed thermoplastic polymer nano-fiber suspension; the mass percentage concentration of the thermoplastic nanofiber suspension is 0.8%;
2) preparing a nano microcrystalline cellulose suspension: adding cotton into 60 wt% sulfuric acid solution to perform acid hydrolysis reaction on the cotton, wherein the mass ratio of the cotton to the 60 wt% sulfuric acid solution is 1:8, the temperature of the acid hydrolysis reaction is 45 ℃, the time is 30min, after the reaction is finished, centrifuging the reaction solution, washing the reaction solution with pure water, dialyzing the reaction solution with pure water until the pH value is stable, and finally adding water to dilute the reaction solution to obtain nano microcrystalline cellulose suspension with the mass percentage concentration of 0.5%;
3) preparing a gas-sensitive film sensitive to ethanol and acetone: coating the thermoplastic polymer nanofiber suspension on PET cloth, wherein the thickness of the thermoplastic polymer nanofiber suspension coated on the PET cloth is 10 microns, air-drying under natural conditions to form a layer of thermoplastic polymer film on the surface of the PET cloth, tearing off the thermoplastic polymer film from the PET cloth, coating the nanocrystalline cellulose suspension on the surface of the thermoplastic polymer film, and air-drying under natural conditions to obtain the gas-sensitive film sensitive to ethanol and acetone.
Referring to fig. 1, the gas-sensitive film sensitive to ethanol and acetone obtained in this example 1 is a field emission scanning electron micrograph magnified 5000 times.
The gas-sensitive film sensitive to ethanol and acetone obtained in this example 1 was tested in an acetone vapor environment, and as shown in fig. 4, the response time was 1.5s, the maximum bending angle was 55 °, and the recovery time was 4 s. Fig. 4 illustrates that the response speed and recovery speed of the gas sensitive film are both relatively fast.
Example 2
The preparation method of the gas-sensitive film sensitive to ethanol and acetone comprises the following steps:
1) preparation of thermoplastic polymer nanofiber suspension: adding the PA nano-fiber into an alcohol-water mixed solution, wherein the alcohol-water mixed solution is a mixed solution of isopropanol and water, the mass ratio of the isopropanol to the water is 6:4, and scattering the nano-fiber by adopting a homogenizer to obtain a uniformly dispersed thermoplastic polymer nano-fiber suspension; the mass percentage concentration of the thermoplastic nanofiber suspension is 1%;
2) preparing a nano microcrystalline cellulose suspension: adding wood pulp into 62 wt% sulfuric acid solution to perform acid hydrolysis reaction on the wood pulp, wherein the mass ratio of the wood pulp to the 62 wt% sulfuric acid solution is 1:8.75, the temperature of the acid hydrolysis reaction is 47 ℃, the time is 35min, after the reaction is finished, centrifuging the reaction solution, washing the reaction solution with pure water, dialyzing the reaction solution with the pure water until the pH value is stable, and finally adding water to dilute the reaction solution to obtain 1.0% mass percent of nano microcrystalline cellulose suspension;
3) preparing a gas-sensitive film sensitive to ethanol and acetone: coating the thermoplastic polymer nanofiber suspension on a PP melt-blown fabric, drying the thermoplastic polymer nanofiber suspension coated on the PP melt-blown fabric in air under the natural condition that the thickness of the thermoplastic polymer nanofiber suspension is 30 mu m, forming a layer of thermoplastic polymer film on the surface of the PP melt-blown fabric, tearing the thermoplastic polymer film from the PP melt-blown fabric, coating the nano microcrystalline cellulose suspension on the surface of the thermoplastic polymer film, and drying in air under the natural condition to obtain the gas-sensitive film sensitive to ethanol and acetone.
As shown in fig. 5, the gas-sensitive film sensitive to ethanol and acetone obtained in this example 2 was tested in an ethanol solution environment, and the response time was 2s, the maximum bending angle was 65 °, and the recovery time was 3 s.
FIG. 2, a graph of response time and recovery time for the gas sensitive film sensitive to ethanol and acetone prepared in example 2; in the figure, ethanol steam stimulation is given at 0-2s, and the ethanol steam stimulation is removed after 2 s;
as shown in fig. 3, in the embodiment 2, after the gas-sensitive film sensitive to ethanol and acetone is flattened and the ethanol vapor stimulation is given to reach the maximum bending angle, the gas-sensitive film recovers to be flat after the ethanol vapor stimulation is removed, which is defined as a cycle, and after 20 cycles, the gas-sensitive film still maintains good response capability.
Example 3
The preparation method of the gas-sensitive film sensitive to ethanol and acetone comprises the following steps:
1) preparation of thermoplastic polymer nanofiber suspension: adding PET (polyethylene terephthalate) nano fibers into an alcohol-water mixed solution, wherein the alcohol-water mixed solution is a mixed solution of n-butyl alcohol and water, and the mass ratio of the n-butyl alcohol to the water is 5:5, and scattering the nano fibers by adopting a homogenizer to obtain a uniformly dispersed thermoplastic polymer nano fiber suspension; the mass percentage concentration of the thermoplastic nanofiber suspension is 3%;
2) preparing a nano microcrystalline cellulose suspension: adding sisal hemp into a 65 wt% sulfuric acid solution to perform acid hydrolysis reaction on the sisal hemp, wherein the mass ratio of the sisal hemp to the 65 wt% sulfuric acid solution is 1:9, the temperature of the acid hydrolysis reaction is 50 ℃, the time is 40min, after the reaction is finished, centrifuging the reaction solution, washing the reaction solution with pure water, dialyzing the reaction solution with the pure water until the pH value is stable, and finally adding water to dilute the reaction solution to obtain a nano microcrystalline cellulose suspension liquid with the mass percentage concentration of 2.0%;
3) preparing a gas-sensitive film sensitive to ethanol and acetone: coating the thermoplastic polymer nanofiber suspension on a polypropylene non-woven fabric, drying the thermoplastic polymer nanofiber suspension coated on the polypropylene non-woven fabric in air under the natural condition that the thickness of the thermoplastic polymer nanofiber suspension is 50 microns, forming a layer of thermoplastic polymer film on the surface of the polypropylene non-woven fabric, tearing the thermoplastic polymer film from the polypropylene non-woven fabric, coating the nano microcrystalline cellulose suspension on the surface of the thermoplastic polymer film, and drying in air under the natural condition to obtain the air-sensitive film sensitive to ethanol and acetone.
The nano microcrystalline cellulose nanofiber composite membrane obtained in the embodiment is tested in an environment of 8mL acetone vapor, the response time is 1.6s, the maximum bending angle is 95 degrees, and the recovery time is 6 s.
Example 4
The preparation method of the gas-sensitive film sensitive to ethanol and acetone comprises the following steps:
1) preparation of thermoplastic polymer nanofiber suspension: adding PU nano-fiber into an alcohol-water mixed solution, wherein the alcohol-water mixed solution is a mixed solution of tert-butyl alcohol and water, and the mass ratio of the tert-butyl alcohol to the water is 5:5, and scattering the nano-fiber by adopting a homogenizer to obtain a uniformly dispersed thermoplastic polymer nano-fiber suspension; the mass percentage concentration of the thermoplastic nanofiber suspension is 3%;
2) preparing a nano microcrystalline cellulose suspension: adding sisal hemp into a 68 wt% sulfuric acid solution to perform acid hydrolysis reaction on the sisal hemp, wherein the mass ratio of the sisal hemp to the 68 wt% sulfuric acid solution is 1:8.75, the temperature of the acid hydrolysis reaction is 50 ℃, the time is 45min, after the reaction is finished, centrifuging the reaction solution, washing the reaction solution with pure water, dialyzing the reaction solution with the pure water until the pH value is stable, and finally adding water to dilute the reaction solution to obtain a nano microcrystalline cellulose suspension with the mass percentage concentration of 3.0%;
3) preparing a gas-sensitive film sensitive to ethanol and acetone: coating the thermoplastic polymer nanofiber suspension on a PP non-woven fabric, drying the thermoplastic polymer nanofiber suspension coated on the PP non-woven fabric in air under the natural condition that the thickness of the thermoplastic polymer nanofiber suspension is 60 mu m, forming a layer of thermoplastic polymer film on the surface of the PP non-woven fabric, tearing off the thermoplastic polymer film from the PP non-woven fabric, coating the nanocrystalline cellulose suspension on the surface of the thermoplastic polymer film, and drying in air under the natural condition to obtain the gas-sensitive film sensitive to ethanol and acetone.
The nano microcrystalline cellulose nanofiber composite membrane obtained in the embodiment is tested in the environment of 10mL of ethanol steam, the response time is 1.0s, the maximum bending angle is 100 degrees, and the recovery time is 3 s.
Example 5
The preparation method of the gas-sensitive film sensitive to ethanol and acetone comprises the following steps:
1) preparation of thermoplastic polymer nanofiber suspension: adding PVA-co-PE nano-fibers into an alcohol-water mixed solution, wherein the alcohol-water mixed solution is a mixed solution of tert-butyl alcohol and water, and the mass ratio of the alcohol to the water is 5:5, and scattering the nano-fibers by adopting a homogenizer to obtain a uniformly dispersed thermoplastic polymer nano-fiber suspension; the mass percentage concentration of the thermoplastic nanofiber suspension is 3%;
2) preparing a nano microcrystalline cellulose suspension: adding cotton into 70 wt% sulfuric acid solution to perform acid hydrolysis reaction on the cotton, wherein the mass ratio of the cotton to the 70 wt% sulfuric acid solution is 1:8.75, the temperature of the acid hydrolysis reaction is 55 ℃, the time is 50min, after the reaction is finished, centrifuging the reaction solution, washing the reaction solution with pure water, dialyzing the reaction solution with pure water until the pH value is stable, and finally adding water to dilute the reaction solution to obtain 5.0% mass percent nano microcrystalline cellulose suspension;
3) preparing a gas-sensitive film sensitive to ethanol and acetone: coating the thermoplastic polymer nanofiber suspension on a PP non-woven fabric, drying the thermoplastic polymer nanofiber suspension coated on the PP non-woven fabric in air under the natural condition that the thickness of the thermoplastic polymer nanofiber suspension is 80 microns, forming a layer of thermoplastic polymer film on the surface of the PP non-woven fabric, tearing off the thermoplastic polymer film from the PP non-woven fabric, coating the nanocrystalline cellulose suspension on the surface of the thermoplastic polymer film, and drying in air under the natural condition to obtain the air-sensitive film sensitive to ethanol and acetone.
The nano microcrystalline cellulose nanofiber composite membrane obtained in the embodiment is tested in the environment of 10mL of ethanol steam, the response time is 0.8s, the maximum bending angle is 110 degrees, and the recovery time is 2 s.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (1)
1. The application of a gas-sensitive film sensitive to ethanol and acetone in the aspect of a gas-sensitive flexible sensor for ethanol and acetone;
the preparation method of the gas-sensitive film sensitive to ethanol and acetone comprises the following steps:
1) preparation of thermoplastic polymer nanofiber suspension: adding the thermoplastic polymer nanofiber into the mixed solvent, and scattering the nanofiber by adopting a homogenizer to obtain a uniformly dispersed thermoplastic polymer nanofiber suspension;
2) preparing a nano microcrystalline cellulose suspension: adding cellulose into an acid solution to perform acid hydrolysis reaction on the cellulose, washing the reaction solution after the reaction is finished, and adding water to dilute the reaction solution to prepare a nano microcrystalline cellulose suspension;
3) preparing a gas-sensitive film sensitive to ethanol and acetone: coating the thermoplastic polymer nanofiber suspension on a base material, air-drying under natural conditions to form a layer of thermoplastic polymer film on the surface of the base material, tearing off the thermoplastic polymer film from the base material, coating the nanocrystalline cellulose suspension on the surface of the thermoplastic polymer film, and air-drying under natural conditions to obtain an air-sensitive film sensitive to ethanol and acetone;
in the step 1), the thermoplastic polymer nanofiber is polyvinyl alcohol-ethylene copolymer nanofiber, polyamide nanofiber, polyethylene terephthalate nanofiber or polyurethane nanofiber, the mass percentage concentration of the thermoplastic nanofiber suspension is 0.8-3%, the mixed solvent is an alcohol-water mixed solution, the mass ratio of alcohol to water is 7: 3-5: 5, and the alcohol is one of n-propanol, isopropanol, n-butanol or tert-butanol;
in the step 2), the cellulose is cotton, wood pulp or sisal; the acid solution is a 60-70 wt% sulfuric acid solution, the mass ratio of the cellulose to the acid solution is 1: 8-9, the temperature of the acid hydrolysis reaction is 45-55 ℃, the time is 30-50 min, the washing process comprises the steps of firstly centrifuging the reaction solution, washing with pure water, and then dialyzing with pure water until the pH value is stable, wherein the mass percentage concentration of the nano microcrystalline cellulose suspension is 0.5-5%;
in the step 3), the base material is one of PET cloth, PP melt-blown cloth, polypropylene non-woven fabric or PP non-woven fabric; the thickness of the thermoplastic polymer nanofiber suspension coated on the base material is 10-80 microns.
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