CN107337802A - Air-sensitive film sensitive to ethanol and acetone and preparation method thereof - Google Patents

Air-sensitive film sensitive to ethanol and acetone and preparation method thereof Download PDF

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Publication number
CN107337802A
CN107337802A CN201710350814.1A CN201710350814A CN107337802A CN 107337802 A CN107337802 A CN 107337802A CN 201710350814 A CN201710350814 A CN 201710350814A CN 107337802 A CN107337802 A CN 107337802A
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sensitive
air
acetone
ethanol
thermoplastic polymer
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CN107337802B (en
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王栋
朱青
王文
钟卫兵
金玉霞
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Donghua University
Wuhan Textile University
National Dong Hwa University
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Donghua University
Wuhan Textile University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04Coating
    • C08J7/0427Coating with only one layer of a composition containing a polymer binder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00Processes for applying liquids or other fluent materials
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2329/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/02Homopolymers or copolymers of unsaturated alcohols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04Polyurethanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2401/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2401/02Cellulose; Modified cellulose
    • C08J2401/04Oxycellulose; Hydrocellulose

Abstract

The present invention relates to the preparation field of air-sensitive film, more particularly to a kind of air-sensitive film sensitive to ethanol and acetone and preparation method thereof.The preparation method of the air-sensitive film sensitive to ethanol and acetone, comprises the following steps:First, by thermoplastic polymer nanofiber's fibrous suspension coated on base material, dry rear substrate surface forms one layer of thermoplastic polymer film, thermoplastic polymer film of being torn from base material;Then nano micro crystal cellulose suspension is made by acid hydrolyzed cellulose, nano micro crystal cellulose suspension is coated on thermoplastic polymer film surface, the air-sensitive film sensitive to ethanol and acetone is produced after drying.Obtained air-sensitive film can not only determine whether the spilling of ethanol or acetone steam by the metamorphosis of macroscopic view, and can respond alcohol vapour and can response acetone steam.

Description

Air-sensitive film sensitive to ethanol and acetone and preparation method thereof
Technical field
The present invention relates to the preparation field of air-sensitive film, more particularly to a kind of air-sensitive film sensitive to ethanol and acetone and Its preparation method.
Background technology
The leakage of volatile solvent, the especially simpler and cruder solvent of packing ratio often occur in laboratory, often occurs Because lid breakage volatile solvent volatilizees into air, solvent is not only wasted, more seriously influences laboratory operation personnel Health.The common volatile solvent in laboratory has ethanol and acetone, and gaseous state acetone belongs to negligible risk polluter, right The nervous system of human body has certain injury.Because small lid crack is not easy to be therefore easily perceived by humans, if can be in the molten of ethanol or acetone One gas sensitive that can respond ethanol and can response acetone is installed, you can pass through the metamorphosis of gas sensitive on agent bottle cap Rapidly determine whether the leakage of ethanol and acetone.Such as Chinese invention patent, patent announcement number is CN 100401548C, CN 101813654A, CN 100383995C, CN 105419784A etc. utilize 9,10- (diphenyl) acetenyls anthracene, ZnO, tin oxide It is added to Deng material as response material in fiber or film and makes it have to alcohol vapour responding ability, all shows as impedance Change, the unit response ethanol such as galvanometer need to be passed through;And for example Chinese invention patent, patent announcement number be CN 100547389C, It is added to Zirconium oxide powder and nanometer as response material by the use of erbium oxide powder, dysprosia powder in CN 100494993C Made it have in strontium carbonate powder to acetone steam responding ability.
At present, the response to ethanol or acetone generally is the response of impedance variations, can not pass through the metamorphosis of macroscopic view Determine whether that ethanol or acetone steam overflow, and be not up to the present documented also that all there is ethanol and acetone and ring The gas sensitive of answering property.
The content of the invention
To solve problem above, it is an object of the invention to provide a kind of air-sensitive film sensitive to ethanol and acetone and its system Preparation Method, the air-sensitive film can not only determine whether the spilling of ethanol or acetone steam by the metamorphosis of macroscopic view, and Alcohol vapour and can response acetone steam can be responded.
To achieve the above object, the technical scheme designed by the present invention includes:
The preparation method of the air-sensitive film sensitive to ethanol and acetone, comprises the following steps:First, by thermoplastic polymer Nanofiber suspension is torn coated in one layer of thermoplastic polymer film of rear substrate surface formation on base material, is dried from base material Lower thermoplastic polymer film;Then nano micro crystal cellulose suspension is made by acid hydrolyzed cellulose, nano microcrystalline is fine Tie up plain suspension and be coated on thermoplastic polymer film surface, the air-sensitive film sensitive to ethanol and acetone is produced after drying.
Realizing the present invention preferably technical scheme is:The preparation method of the air-sensitive film sensitive to ethanol and acetone, specifically Comprise the following steps:
1) thermoplastic polymer nanofiber's fibrous suspension is prepared:Thermoplastic polymer nanofiber's fiber is added to mixed solvent In, nanofiber is broken up using homogenizer, obtains finely dispersed thermoplastic polymer nanofiber's fibrous suspension;
2) nano micro crystal cellulose suspension is prepared:Cellulose is added in acid solution anti-to cellulose progress sour water solution Should, after completion of the reaction, obtained nano micro crystal cellulose suspension will be diluted with water after reaction solution washes clean;
3) air-sensitive film sensitive to ethanol and acetone is prepared:Thermoplastic polymer nanofiber's fibrous suspension is coated in base On material, air-dried under natural conditions, substrate surface forms one layer of thermoplastic polymer film, thermoplastic polymer of being torn from base material Sodium rice microcrystalline cellulose suspension is coated on thermoplastic polymer film surface after film, air-dried under natural conditions, is produced pair The air-sensitive film of ethanol and acetone sensitivity.
Further, in the step 1), thermoplastic polymer nanofiber's fiber 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 thermoplastic nanofibers' fibrous suspension is 0.8%-3%, and the mixed solvent is Alcohol-water mixture, and the mass ratio of alcohol and water is 7:3~5:5, the alcohol is in normal propyl alcohol, isopropanol, n-butanol or the tert-butyl alcohol One kind.
Further, in the step 2), cellulose is cotton, wood pulp or sisal hemp;The acid solution is 60~70wt% Sulfuric acid solution, the mass ratio of the cellulose and acid solution is 1:8~9, the temperature of acid hydrolytic reaction is 45~55 DEG C, the time For 30~50min, the process of the washing is that pure water is used after first reaction solution is centrifuged, and then with pure water dialyse directly Untill pH is stable, the mass percentage concentration of the nano micro crystal cellulose suspension is 0.5%~5%.
Further, in the step 3), base material is one in PET cloth, PP fusion spray cloths, nonwoven polypropylene fabric or PP non-woven fabrics Kind;The thickness of thermoplastic polymer nanofiber's fibrous suspension coated on base material is 10 μm~80 μm.
Wherein, preparation method the referenced patent CN105148996A, CN 104014196 of thermoplastic polymer nanofiber's fiber Preparation method described in the A of B, CN 103884695.Melted using two kinds of mutual exclusive polymer of thermodynamics in twin-screw Abundant melt blending in extruder, extrusion, the polymer melt of blending is in extruder and spinning head by shearing force and stretching The effect of compound force field and elongation strain, form bundles of nanofibers, finally, remove matrix polymer, obtain thermoplastic polymer Nanofiber.Exemplified by preparing polyvinyl alcohol-ethylene copolymer nanofiber, preparation method is:Polyvinyl alcohol-ethylene is copolymerized Thing (PVA-co-PE) is blended with acetylbutyrylcellulose (CAB), is extruded through twin-screw melt extruder, recycles acetone to remove CAB produces polyvinyl alcohol-ethylene copolymer nanofiber.
The air-sensitive film sensitive to ethanol and acetone, it is by the preparation of the above-mentioned air-sensitive film sensitive to ethanol and acetone Method is prepared.The air-sensitive film includes two layers of laminated film, and one layer is thermoplastic polymer film, and another layer is to be coated in The nano micro crystal cellulose film on thermoplastic polymer film surface.
The air-sensitive film sensitive to ethanol and acetone of the present invention is in terms of the air-sensitive flexible sensor of ethanol and acetone Application.The method and Traditional flexible transducer production method for preparing flexible sensor differ, Traditional flexible sensor it is quick Film is felt for impedance sensitive film, it is necessary to add electrode, galvanometer etc..The air-sensitive film of the present invention is flexible in the air-sensitive of ethanol and acetone Application in terms of sensor, specifically air-sensitive film produced by the present invention can be placed in ventilative protection in the application that reagent bottle covers In shell, and the ventilative containment vessel equipped with the air-sensitive film is placed in above bottle cap, by observing the bending change of air-sensitive film i.e. The leakage of ethanol or acetone can quickly be determined whether.
Air-sensitive film produced by the present invention can be realized is to the principle of ethanol and the sensitive response of acetone:Cellulose is by D- pyrroles Glucopyranoside base is basic structural unit, the linear polymeric connected and composed by β-Isosorbide-5-Nitrae glycosidic bond.Conventional acid-hydrolysis method, alkali The means such as method, biologic enzymolysis method, mechanical-physical processing method handle cellulose, can remove noncrystalline domain in cellulosic structure from And nano micro crystal cellulose is prepared, nano micro crystal cellulose has physics and chemistry as a kind of emerging functional high molecule material The properties such as excellent performance, specific surface area are big, crystallinity is high, good biocompatibility.In addition, nano micro crystal cellulose surface exposes Great amount of hydroxy group, reducing end under neutral hydroxyl isoreactivity group, hydrophily is preferable, when film side is by alcohol vapour and acetone steam During stimulation, the side humidity step-down, the hydrone that Hydrogenbond is produced with the hydroxyl on nano micro crystal cellulose is reduced, and volume becomes It is small, so as to drive whole composite nano-fiber membrane to the curving without ethanol or acetone steam.
The advantage of the invention is that:
1, due to highly brittle after pure nano micro crystal cellulose film forming, pliability is poor, therefore nano micro crystal cellulose is hanged Supernatant liquid is coated in the surface of thermoplastic nanofibers' fiber membrane, makes it have the pliability of thermoplastic nanofibers' fiber and has nanometer The humidity response performance of microcrystalline cellulose.
2, nano micro crystal cellulose and thermoplastic nanofibers' fiber are all Nano grades, and nano micro crystal cellulose is coated in thermoplastic Behind property nano fibrous membrane surface, there is certain hole, specific surface area is bigger, quicker to the spilling of ethanol and acetone steam Sense.
3, obtained air-sensitive film high sensitivity, the response time is very short, and when environment does not change, resume speed is non- It is often rapid.
Brief description of the drawings
Fig. 1 is the field emission scanning electron microscope photo of the obtained air-sensitive film sensitive to ethanol and acetone of embodiment 1, is amplified Multiple is 5000 times;
Fig. 2 is the response time and recovery time of the obtained air-sensitive film sensitive to ethanol and acetone of embodiment 2;In figure Alcohol vapour stimulation is given in 0-2s, removes alcohol vapour stimulation after 2s;
Fig. 3 is the circulation that the obtained air-sensitive film sensitive to ethanol and acetone of embodiment 2 responds 20 times to alcohol vapour Performance map;
Fig. 4 is fast-response energy of the obtained air-sensitive film sensitive to ethanol and acetone of embodiment 1 to acetone steam Photo;Fig. 4 A are that the air-sensitive film has just been put equipped with the smooth figure on acetone beaker, and the air-sensitive film is curved after Fig. 4 B are 1.5s Diagram, its bending angle are 55 °;
Fig. 5 is fast-response energy of the obtained air-sensitive film sensitive to ethanol and acetone of embodiment 2 to alcohol vapour Photo.Fig. 5 A are that the air-sensitive film has just been put equipped with the smooth figure on ethanol beaker, and Fig. 5 B are the bending of the air-sensitive film after 2s Figure, its bending angle are 65 °.
Embodiment
To more fully understand the present invention, invention is described in detail below with reference to accompanying drawing and instantiation.
Embodiment 1
The preparation method of the air-sensitive film sensitive to ethanol and acetone, comprises the following steps:
1) thermoplastic polymer nanofiber's fibrous suspension is prepared:PVA-co-PE nanofibers are added to alcohol-water mixture In, alcohol-water mixture is the mixed liquor of normal propyl alcohol and water, and the mass ratio of normal propyl alcohol and water is 7:3, using homogenizer by nanometer Fabric thrashing, obtain finely dispersed thermoplastic polymer nanofiber's fibrous suspension;The quality of thermoplastic nanofibers' fibrous suspension Percentage concentration is 0.8%;
2) nano micro crystal cellulose suspension is prepared:Cotton is added in 60wt% sulfuric acid solution and acid is carried out to cotton The mass ratio of hydrolysis, cotton and 60wt% sulfuric acid solution is 1:8, the temperature of acid hydrolytic reaction is 45 DEG C, and the time is 30min, after completion of the reaction, pure water is used after first reaction solution is centrifuged, then carries out dialysis untill pH is stable with pure water, Finally it is diluted with water the nano micro crystal cellulose suspension that obtained mass percentage concentration is 0.5%;
3) air-sensitive film sensitive to ethanol and acetone is prepared:Thermoplastic polymer nanofiber's fibrous suspension is coated in On PET cloth, the thickness coated in thermoplastic polymer nanofiber's fibrous suspension on PET cloth is 10 μm, is air-dried under natural conditions, PET cloth surface forms one layer of thermoplastic polymer film, sodium rice crystallite is fine after thermoplastic polymer film of being torn from PET cloth Tie up plain suspension and be coated on thermoplastic polymer film surface, air-dried under natural conditions, produce the gas sensitive to ethanol and acetone Sensitive film.
Such as Fig. 1, the Flied emission that the air-sensitive film sensitive to ethanol and acetone that the present embodiment 1 obtains amplifies 5000 times scans Electromicroscopic photograph.
The air-sensitive film sensitive to ethanol and acetone that the present embodiment 1 is obtained tries in the environment of acetone steam Test, with reference to shown in Fig. 4, its response time is 1.5s, and maximum bending angle is 55 °, recovery time 4s.Fig. 4 illustrates that air-sensitive is thin The response speed and resume speed of film are all than very fast.
Embodiment 2
The preparation method of the air-sensitive film sensitive to ethanol and acetone, comprises the following steps:
1) thermoplastic polymer nanofiber's fibrous suspension is prepared:PA nanofibers are added in alcohol-water mixture, alcohol water Mixed liquor is the mixed liquor of isopropanol and water, and the mass ratio of isopropanol and water is 6:4, nanofiber is beaten using homogenizer Dissipate, obtain finely dispersed thermoplastic polymer nanofiber's fibrous suspension;The quality percentage of thermoplastic nanofibers' fibrous suspension is dense Spend for 1%;
2) nano micro crystal cellulose suspension is prepared:Wood pulp is added in 62wt% sulfuric acid solution and acid is carried out to wood pulp The mass ratio of hydrolysis, wood pulp and 62wt% sulfuric acid solution is 1:8.75, the temperature of acid hydrolytic reaction is 47 DEG C, and the time is 35min, after completion of the reaction, pure water is used after first reaction solution is centrifuged, then carries out dialysis untill pH is stable with pure water, Finally it is diluted with water the nano micro crystal cellulose suspension that obtained mass percentage concentration is 1.0%;
3) air-sensitive film sensitive to ethanol and acetone is prepared:Thermoplastic polymer nanofiber's fibrous suspension is coated in PP On fusion spray cloth, the thickness coated in thermoplastic polymer nanofiber's fibrous suspension on PP fusion spray cloths is 30 μm of natural conditions leewards Dry, PP fusion spray cloths surface forms one layer of thermoplastic polymer film, will after thermoplastic polymer film of being torn from PP fusion spray cloths Sodium rice microcrystalline cellulose suspension is coated on thermoplastic polymer film surface, air-dries, is produced to ethanol and third under natural conditions The sensitive air-sensitive film of ketone.
Such as Fig. 5, the air-sensitive film sensitive to ethanol and acetone that the present embodiment 2 obtains is carried out in the environment of ethanol solution Experiment, its response time are 2s, and maximum bending angle is 65 °, recovery time 3s.
Such as Fig. 2, the response time and recovery time of the obtained air-sensitive film sensitive to ethanol and acetone of embodiment 2 scheme; Alcohol vapour stimulation is given in figure in 0-2s, removes alcohol vapour stimulation after 2s;
Such as Fig. 3, the air-sensitive film sensitive to ethanol and acetone that the present embodiment 2 obtains is given alcohol vapour when smooth and stimulated After reach and remove air-sensitive film after alcohol vapour stimulates after maximum bend angle and recover smooth, a circulation is defined as, by 20 Individual circulation, the air-sensitive film still keeps preferable responding ability.
Embodiment 3
The preparation method of the air-sensitive film sensitive to ethanol and acetone, comprises the following steps:
1) thermoplastic polymer nanofiber's fibrous suspension is prepared:PET nanofibers are added in alcohol-water mixture, alcohol water Mixed liquor is the mixed liquor of n-butanol and water, and the mass ratio of n-butanol and water is 5:5, nanofiber is beaten using homogenizer Dissipate, obtain finely dispersed thermoplastic polymer nanofiber's fibrous suspension;The quality percentage of thermoplastic nanofibers' fibrous suspension is dense Spend for 3%;
2) nano micro crystal cellulose suspension is prepared:Sisal hemp is added in 65wt% sulfuric acid solution and acid is carried out to sisal hemp The mass ratio of hydrolysis, sisal hemp and 65wt% sulfuric acid solution is 1:9, the temperature of acid hydrolytic reaction is 50 DEG C, and the time is 40min, after completion of the reaction, pure water is used after first reaction solution is centrifuged, then carries out dialysis untill pH is stable with pure water, Finally it is diluted with water the nano micro crystal cellulose suspension that obtained mass percentage concentration is 2.0%;
3) air-sensitive film sensitive to ethanol and acetone is prepared:Thermoplastic polymer nanofiber's fibrous suspension is coated in third On synthetic fibre non-woven fabrics, the thickness coated in thermoplastic polymer nanofiber's fibrous suspension in nonwoven polypropylene fabric is 50 μm of natural conditions Lower to air-dry, nonwoven polypropylene fabric surface forms one layer of thermoplastic polymer film, thermoplastic polymer of being torn from nonwoven polypropylene fabric Sodium rice microcrystalline cellulose suspension is coated on thermoplastic polymer film surface after film, air-dried under natural conditions, is produced pair The air-sensitive film of ethanol and acetone sensitivity.
The nano micro crystal cellulose nano-fiber composite film that the present embodiment obtains is tried in the environment of 8mL acetone steams Test, its response time is 1.6s, and maximum bending angle is 95 °, recovery time 6s.
Embodiment 4
The preparation method of the air-sensitive film sensitive to ethanol and acetone, comprises the following steps:
1) thermoplastic polymer nanofiber's fibrous suspension is prepared:PU nanofibers are added in alcohol-water mixture, alcohol water Mixed liquor is the mixed liquor of the tert-butyl alcohol and water, and the mass ratio of the tert-butyl alcohol and water is 5:5 are broken up nanofiber using homogenizer, Obtain finely dispersed thermoplastic polymer nanofiber's fibrous suspension;The mass percentage concentration of thermoplastic nanofibers' fibrous suspension is 3%;
2) nano micro crystal cellulose suspension is prepared:Sisal hemp is added in 68wt% sulfuric acid solution and acid is carried out to sisal hemp The mass ratio of hydrolysis, sisal hemp and 68wt% sulfuric acid solution is 1:8.75, the temperature of acid hydrolytic reaction is 50 DEG C, and the time is 45min, after completion of the reaction, pure water is used after first reaction solution is centrifuged, then carries out dialysis untill pH is stable with pure water, Finally it is diluted with water the nano micro crystal cellulose suspension that obtained mass percentage concentration is 3.0%;
3) air-sensitive film sensitive to ethanol and acetone is prepared:Thermoplastic polymer nanofiber's fibrous suspension is coated in PP On non-woven fabrics, the thickness coated in thermoplastic polymer nanofiber's fibrous suspension on PP non-woven fabrics is 60 μm of natural conditions leewards Dry, PP nonwoven surfaces form one layer of thermoplastic polymer film, will after thermoplastic polymer film of being torn from PP non-woven fabrics Sodium rice microcrystalline cellulose suspension is coated on thermoplastic polymer film surface, air-dries, is produced to ethanol and third under natural conditions The sensitive air-sensitive film of ketone.
The nano micro crystal cellulose nano-fiber composite film that the present embodiment obtains is carried out in the environment of 10mL alcohol vapours Experiment, its response time are 1.0s, and maximum bending angle is 100 °, recovery time 3s.
Embodiment 5
The preparation method of the air-sensitive film sensitive to ethanol and acetone, comprises the following steps:
1) thermoplastic polymer nanofiber's fibrous suspension is prepared:PVA-co-PE nanofibers are added to alcohol-water mixture In, alcohol-water mixture is the mixed liquor of the tert-butyl alcohol and water, and the mass ratio of alcohol and water is 5:5 are beaten nanofiber using homogenizer Dissipate, obtain finely dispersed thermoplastic polymer nanofiber's fibrous suspension;The quality percentage of thermoplastic nanofibers' fibrous suspension is dense Spend for 3%;
2) nano micro crystal cellulose suspension is prepared:Cotton is added in 70wt% sulfuric acid solution and acid is carried out to cotton The mass ratio of hydrolysis, cotton and 70wt% sulfuric acid solution is 1:8.75, the temperature of acid hydrolytic reaction is 55 DEG C, and the time is 50min, after completion of the reaction, pure water is used after first reaction solution is centrifuged, then carries out dialysis untill pH is stable with pure water, Finally it is diluted with water the nano micro crystal cellulose suspension that obtained mass percentage concentration is 5.0%;
3) air-sensitive film sensitive to ethanol and acetone is prepared:Thermoplastic polymer nanofiber's fibrous suspension is coated in PP On non-woven fabrics, the thickness coated in thermoplastic polymer nanofiber's fibrous suspension on PP non-woven fabrics is 80 μm of natural conditions leewards Dry, PP nonwoven surfaces form one layer of thermoplastic polymer film, will after thermoplastic polymer film of being torn from PP non-woven fabrics Sodium rice microcrystalline cellulose suspension is coated on thermoplastic polymer film surface, air-dries, is produced to ethanol and third under natural conditions The sensitive air-sensitive film of ketone.
The nano micro crystal cellulose nano-fiber composite film that the present embodiment obtains is carried out in the environment of 10mL alcohol vapours Experiment, its response time are 0.8s, and maximum bending angle is 110 °, recovery time 2s.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.

Claims (7)

  1. A kind of 1. preparation method of the air-sensitive film sensitive to ethanol and acetone, it is characterised in that:Comprise the following steps:First, Thermoplastic polymer nanofiber's fibrous suspension is thin coated in rear substrate surface one layer of thermoplastic polymer of formation on base material, is dried Film, thermoplastic polymer film of being torn from base material;Then nano micro crystal cellulose suspension is made by acid hydrolyzed cellulose, Nano micro crystal cellulose suspension is coated on thermoplastic polymer film surface, produced after drying sensitive to ethanol and acetone Air-sensitive film.
  2. 2. the preparation method of the air-sensitive film sensitive to ethanol and acetone according to claim 1, it is characterised in that:Specifically Comprise the following steps:
    1) thermoplastic polymer nanofiber's fibrous suspension is prepared:Thermoplastic polymer nanofiber's fiber is added in the mixed solvent, Nanofiber is broken up using homogenizer, obtains finely dispersed thermoplastic polymer nanofiber's fibrous suspension;
    2) nano micro crystal cellulose suspension is prepared:Cellulose is added in acid solution acid hydrolytic reaction is carried out to cellulose, After completion of the reaction, obtained nano micro crystal cellulose suspension will be diluted with water after reaction solution washes clean;
    3) air-sensitive film sensitive to ethanol and acetone is prepared:Thermoplastic polymer nanofiber's fibrous suspension is coated in base material On, air-dried under natural conditions, substrate surface forms one layer of thermoplastic polymer film, and thermoplastic polymer of being torn from base material is thin Nano micro crystal cellulose suspension is coated on thermoplastic polymer film surface after film, air-dries, is produced to second under natural conditions The air-sensitive film of alcohol and acetone sensitivity.
  3. 3. the preparation method of the air-sensitive film sensitive to ethanol and acetone according to claim 2, it is characterised in that:It is described In step 1), thermoplastic polymer nanofiber's fiber is polyvinyl alcohol-ethylene copolymer nanofiber, polyamide nanofiber, gathered Ethylene glycol terephthalate nanofiber or polyurethane nanofiber, the quality percentage of thermoplastic nanofibers' fibrous suspension Concentration is 0.8%-3%, and the mixed solvent is alcohol-water mixture, and the mass ratio of alcohol and water is 7:3~5:5, the alcohol is One kind in normal propyl alcohol, isopropanol, n-butanol or the tert-butyl alcohol.
  4. 4. the preparation method of the air-sensitive film sensitive to ethanol and acetone according to claim 2, it is characterised in that:It is described In step 2), cellulose is cotton, wood pulp or sisal hemp;The acid solution be 60~70wt% sulfuric acid solution, the cellulose Mass ratio with acid solution is 1:8~9, the temperature of acid hydrolytic reaction is 45~55 DEG C, and the time is 30~50min, the washing Process be that pure water is used after first reaction solution is centrifuged, then with pure water carry out dialysis until pH stably untill, the nanometer The mass percentage concentration of microcrystalline cellulose suspension is 0.5%~5%.
  5. 5. the preparation method of the air-sensitive film sensitive to ethanol and acetone according to claim 2, it is characterised in that:It is described In step 3), base material is one kind in PET cloth, PP fusion spray cloths, nonwoven polypropylene fabric or PP non-woven fabrics;It is described to be coated on base material The thickness of thermoplastic polymer nanofiber's fibrous suspension is 10 μm~80 μm.
  6. A kind of 6. air-sensitive film sensitive to ethanol and acetone, it is characterised in that:It is by any one of Claims 1 to 5 institute The preparation method for stating the air-sensitive film sensitive to ethanol and acetone is prepared.
  7. It is 7. a kind of as claimed in claim 6 to ethanol and the air-sensitive film of acetone sensitivity in the flexible biography of the air-sensitive of ethanol and acetone Application in terms of sensor.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109397825A (en) * 2018-12-03 2019-03-01 武汉市银莱制衣有限公司 The MXene based composites and preparation method thereof for having mine toxic dust gas alarm and filtering function
CN111282120A (en) * 2020-02-28 2020-06-16 苏州科技城医院 Emergency atomizer for diabetes patients
CN113624807A (en) * 2021-06-30 2021-11-09 杭州电子科技大学 Preparation of tin oxide and SO by low-temperature hydrothermal reaction of nano-cellulose2Method for gas sensor
CN114481447A (en) * 2022-01-25 2022-05-13 苏州艾美医疗用品有限公司 Production equipment and production process of medical non-woven fabric

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009139362A (en) * 2007-12-10 2009-06-25 Korea Electronics Telecommun Nano-crystalline composite-oxide thin film, environmental gas sensor equipped with it, and its manufacturing method
CN106000120A (en) * 2016-06-07 2016-10-12 东华大学 Preparation method for three-dimensional-network-shaped gradient composite functional film, and product thereof
CN106362601A (en) * 2016-09-28 2017-02-01 扬州云彩新材料科技有限公司 Nano fiber membrane filtering material with antibacterial function and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009139362A (en) * 2007-12-10 2009-06-25 Korea Electronics Telecommun Nano-crystalline composite-oxide thin film, environmental gas sensor equipped with it, and its manufacturing method
CN106000120A (en) * 2016-06-07 2016-10-12 东华大学 Preparation method for three-dimensional-network-shaped gradient composite functional film, and product thereof
CN106362601A (en) * 2016-09-28 2017-02-01 扬州云彩新材料科技有限公司 Nano fiber membrane filtering material with antibacterial function and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
明悦: "纳米微晶纤维素的制备及其在拒水整理中的应用", 《纺织学报》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109397825A (en) * 2018-12-03 2019-03-01 武汉市银莱制衣有限公司 The MXene based composites and preparation method thereof for having mine toxic dust gas alarm and filtering function
CN111282120A (en) * 2020-02-28 2020-06-16 苏州科技城医院 Emergency atomizer for diabetes patients
CN111282120B (en) * 2020-02-28 2022-08-30 苏州科技城医院 Emergency atomizer for diabetes patients
CN113624807A (en) * 2021-06-30 2021-11-09 杭州电子科技大学 Preparation of tin oxide and SO by low-temperature hydrothermal reaction of nano-cellulose2Method for gas sensor
CN113624807B (en) * 2021-06-30 2024-03-29 杭州电子科技大学 Tin oxide and SO prepared by low-temperature hydrothermal reaction of nanocellulose 2 Method for gas sensor
CN114481447A (en) * 2022-01-25 2022-05-13 苏州艾美医疗用品有限公司 Production equipment and production process of medical non-woven fabric

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