CN109810295B - Preparation method of humidity-sensitive sensing film - Google Patents
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Abstract
The invention relates to a humidity-sensitive sensing film and discloses a preparation method of the humidity-sensitive sensing film. The preparation method comprises the steps of taking valeryl chloride as a modifier, and carrying out modification treatment on cellulose in an ionic liquid solution of 1-ethyl-3-methylimidazole acetate to prepare water-soluble cellulose acetate WSCA; preparing the water-soluble cellulose acetate into a cellulose aqueous solution, preparing graphene oxide into a solution, and adding the solution into the prepared cellulose solution to obtain a cellulose/graphene oxide uniform mixed solution; and adding a reducing reagent into the cellulose/graphene oxide mixed solution, and processing the obtained reduced graphene oxide/cellulose aqueous solution to obtain the flexible rGO/WSCA humidity-sensitive sensing membrane. The humidity sensitive membrane has the advantages of difficult falling, no damp stagnation, good humidity sensitivity, environment-friendly material and the like.
Description
Technical Field
The invention relates to a humidity-sensitive sensing film, in particular to a preparation method of the humidity-sensitive sensing film.
Background
Humidity, a physical quantity representing the degree of dryness of the atmosphere, is closely related to human survival and social activities, and with the continuous advance of the degree of modernization, a completely humidity-independent field is difficult to find. The measurement and control of humidity plays an important role in many fields such as industrial and agricultural production, food production and storage, aerospace, medical equipment and the like. Therefore, various instruments and devices for monitoring humidity have been developed, and humidity detection and control are being performed in many fields of production and life. The traditional humidity-sensitive meter and humidity-sensitive material have the problems of humidity-sensitive defect, complex preparation process, high cost and the like, and are difficult to meet the working requirements of various fields. In recent years, the electric signal humidity-sensitive sensing membrane material has been widely developed and applied due to the advantages of real-time monitoring, visual reflection of new signals, sensitive detection and the like. Among them, reduced graphene oxide (rGO) is a hot spot for the research of humidity-sensitive sensing films due to its high conductivity, high specific surface area, etc.
Researches find that pure rGO is difficult to combine with water molecules due to low content of oxygen-containing functional groups, so that the humidity sensitivity is poor, the prepared sensing film cannot form an independently supported sensing film due to poor strength, a substrate is usually required to be combined, and the sensing film combined with the substrate can cause the humidity sensitive film to fall off after being used for a long time, so that the development of the graphene sensing film is limited; in addition, researchers also adopt polyvinyl alcohol containing rich hydroxyl groups and rGO to combine to prepare a humidity-sensitive sensing membrane, the rich hydroxyl groups in the polyvinyl alcohol can provide water molecule binding sites and can form hydrogen bonds with reduced graphene oxide, so that the strength and humidity-sensitive performance of the obtained humidity-sensitive membrane material are improved, but the polyvinyl alcohol has irritation and is harmful to the body after being absorbed, belongs to 3 types of carcinogens, has development concepts which are not in line with green health, and cannot be applied to the fields of food, health medical treatment and the like; the existing humidity-sensitive sensing membrane also has the following technical problems, for example, the existing sensing membrane is difficult to realize the rapid expansion and contraction of the composite membrane in the process of moisture absorption and dehumidification, so that the phenomenon of humidity stagnation occurs; the existing humidity sensitive sensing membrane has the defects of poor humidity sensitivity, dispersion stability of the rGO aqueous solution and the like. In view of the above, the present invention provides a method for preparing a moisture-sensitive sensing film.
Disclosure of Invention
In order to solve the defects that the humidity sensitive membrane in the prior art is easy to fall off, easy to generate a damp stagnation phenomenon, poor in humidity sensitivity, and not environment-friendly enough in materials, the invention provides a preparation method of a humidity sensitive sensing membrane.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a humidity sensitive sensing film comprises the following steps:
S1modifying cellulose in 1-ethyl-3-methylimidazole acetate serving as an ionic liquid solution by using valeryl chloride as a modifier to prepare water-soluble cellulose acetate WSCA;
S2preparing the water-soluble cellulose acetate into a cellulose aqueous solution, preparing graphene oxide into a graphene oxide aqueous solution, and adding the prepared graphene oxide aqueous solution into the cellulose solution to obtain a cellulose/graphene oxide uniform mixed solution;
S3adding a reducing reagent into the cellulose/graphene oxide mixed solution, and reducing under the condition that water-soluble cellulose acetate is used as a dispersion system to obtain a reduced graphene oxide (rGO)/cellulose aqueous solution;
S4and carrying out ultrasonic vibration treatment on the reduced graphene oxide/cellulose aqueous solution, and then carrying out suction filtration and drying to obtain the flexible rGO/WSCA humidity-sensitive sensing membrane.
The reaction conditions in the S1 provided by the invention are that the reaction temperature is 60-80 ℃ and the reaction time is 8-12 h.
Preferably, in S1, 0.5-1ml of the modifier valeryl chloride is added per 10g of the ionic liquid 1-ethyl-3-methylimidazole acetate; the cellulose accounts for 2-5% of the mass of the ionic liquid 1-ethyl-3-methylimidazole acetate.
Preferably, in the step S2, the mass concentration of the cellulose aqueous solution is 0.5 to 2%, the concentration of the graphene oxide aqueous solution is 0.25 to 2.5mg/mL, and the mass of the graphene oxide is 0.5 to 40% of the mass of the cellulose.
Preferably, the reducing agent is vitamin C, and the concentration of the vitamin C is 0.3-0.5 mg/ml.
Preferably, in the step S3, the reduction reaction is carried out under stirring conditions of an oil bath at 80 ℃ for 3 hours at a stirring speed of 800 rpm.
Preferably, the drying temperature of S4 is 60 ℃ and the drying time is 30 min.
The invention also provides the humidity-sensitive sensing membrane prepared by the preparation method.
The invention also applies the humidity sensitive sensing film in the preparation of humidity sensitive indicating materials.
The WSCA and rGO provided by the invention have various irreplaceable advantages when being applied to a humidity-sensitive composite membrane: firstly, the modified reagent provided by the invention has the reactivity, the substitution degree can be just in the water-soluble range, the modified reagent has proper low substitution degree, the molecular structure has the characteristic of low substitution degree due to the uniform distribution of the substituent groups, the free hydroxyl on the cellulose molecular structure is reserved to the maximum extent, and in the rGO/WSCA humidity-sensitive composite membrane, on one hand, the hydrophilic hydroxyl in the WSCA molecule provides a binding site for the binding of water molecules, so that the humidity sensitivity of the composite membrane is improved; on the other hand, hydroxyl in WSCA molecules can also form a three-dimensional space network structure with residual oxygen-containing groups in rGO through hydrogen bond interaction, so that the rapid expansion and contraction of the composite membrane are realized in the moisture absorption-dehumidification process, and the wet hysteresis phenomenon is reduced, so that the low substitution value has key effects on the combination with the rGO and the improvement of the moisture sensitivity characteristic; secondly, the molecular structure of WSCA can be regarded as a dispersant with hydrophilic hydroxyl and hydrophobic methyl, on one hand, the hydrophobic end of the surface can be combined with the hydrophobic plane of the rGO sheet layer, and on the other hand, the hydrophilic hydroxyl can be combined with the oxygen-containing group on the surface of the rGO by the action of hydrogen bonds, so that the dispersion stability of the rGO aqueous solution is improved, and in addition, the viscosity of the WSCA aqueous solution is very low, the low viscosity characteristic is very beneficial to the dispersion of the rGO and the blending action of the rGO, so that the product is easy to form a film, the film strength is good, and the product can bear the special working requirements of; thirdly, in the rGO/WSCA humidity-sensitive composite membrane, WSCA is as the humidity sensing layer, rGO is as the resistance conversion layer, and the assembled composite membrane can be regarded as the interconnected micro-conductor and directly used for humidity-sensitive materials without adding any substrate or supporting electrode, so that the problem of detection failure caused by the falling of the humidity-sensitive coating from the substrate or the supporting electrode due to long-time use can be avoided, and the detection stability of the humidity sensor is improved.
Drawings
FIG. 1 is a transmission electron microscope photograph of reduced graphene oxide and an aqueous solution of water-soluble cellulose acetate of example 2;
FIG. 2 is an SEM picture of the rGO/WSCA composite membrane of example 2, (a) a sectional view; (b) a surface map;
FIG. 3 is a photograph of the rGO/WSCA composite membrane of example 2;
FIG. 4 is a humidity sensitive picture of the rGO/WSCA composite membrane of example 2.
Detailed Description
The invention discloses a preparation method of a humidity-sensitive sensing film, and a person skilled in the art can appropriately improve process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications which would be obvious to those skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
EXAMPLE 1 preparation of Water-soluble cellulose acetate
Slowly dripping 1.8mL of valeryl chloride into 30g of ionic liquid 1-ethyl-3-methylimidazole acetate, soaking 1.00g of cotton linter cellulose into the solvent system, magnetically stirring at 70 ℃ in an oil bath to obtain a transparent, viscous and completely dissolved cellulose solution, and reacting for 12 hours at 70 ℃ under the condition of continuous magnetic stirring. After the reaction is finished, pouring the system into 200ml of ethanol to terminate the reaction, then repeatedly washing with a large amount of ethanol, filtering until the ionic liquid and the unreacted reagent are washed clean, obtaining a pure cellulose product, and dissolving the pure cellulose product in water by verification.
Comparative example 1 selection of modifier and Ionic liquid
Slowly dripping 1.8mL of valeryl chloride into 30g of ionic liquid 1-butyl-3-methylimidazolium acetate, soaking 1.00g of cellulose into the solvent system, magnetically stirring at 70 ℃ in an oil bath to obtain a transparent, viscous and completely dissolved cellulose solution, and keeping the temperature at 70 ℃ for reaction for 12 hours under the condition of continuous magnetic stirring. After the reaction is finished, slowly pouring the system into 200ml of ethanol to terminate the reaction, then repeatedly washing with a large amount of ethanol, and filtering until the ionic liquid and the unreacted reagent are washed clean, so as to obtain a pure cellulose product, wherein the product is verified to be insoluble in water.
Comparative example 2 selection of modifier and Ionic liquid
Slowly dripping 1.8mL of valeryl chloride into 30g of ionic liquid 1-allyl-3-methylimidazole acetate, soaking 1.00g of cellulose into the solvent system, magnetically stirring at 70 ℃ in an oil bath to obtain a transparent, viscous and completely dissolved cellulose solution, and reacting for 12 hours at 70 ℃ under the condition of continuous magnetic stirring. After the reaction is finished, slowly pouring the system into 200ml of ethanol to terminate the reaction, then repeatedly washing with a large amount of ethanol, and filtering until the ionic liquid and the unreacted reagent are washed clean, so as to obtain a pure cellulose product, wherein the product is verified to be insoluble in water.
Comparative example 3 selection of modifier and Ionic liquid
Slowly dripping 1.8mL of benzoyl chloride into 30g of ionic liquid 1-ethyl-3-methylimidazole acetate, soaking 1.00g of cellulose into the solvent system, magnetically stirring at 70 ℃ in an oil bath to obtain a transparent, viscous and completely dissolved cellulose solution, and keeping the temperature of 70 ℃ for reaction for 12 hours under the condition of continuous magnetic stirring. After the reaction is finished, slowly pouring the system into 200ml of ethanol to terminate the reaction, then repeatedly washing with a large amount of ethanol, and filtering until the ionic liquid and the unreacted reagent are washed clean, so as to obtain a pure cellulose product, wherein the product is verified to be insoluble in water.
As can be seen from comparative examples 1 and 2, the cellulose products obtained in comparative examples 1 and 2 were insoluble in water, that is, the cellulose obtained was not a low-substituted water-soluble cellulose acetate, i.e., the 1-allyl-3-methylimidazolyl acetate and 1-butyl-3-methylimidazolyl acetate systems, and the low-substituted water-soluble cellulose acetate could not be obtained. As can be seen from comparative example 3, the cellulose product obtained in comparative example 3 was insoluble in water, that is, cellulose was not a low-substituted water-soluble cellulose acetate.
From the comparison results of example 1 and comparative examples 1-3, although the acyl chloride with similar structure can not acetylate cellulose with the intermediate anhydride generated by the anion of the similar ionic liquid, so as to obtain the cellulose acetate with low substitution degree in one step, the technical proposal provided by the invention uses the intermediate anhydride generated by the anion of the valeryl chloride and the ionic liquid 1-ethyl-3-methylimidazole acetate to acetylate the cellulose, and the obtained intermediate anhydride has proper reaction activity.
EXAMPLE 2 preparation of moisture-sensitive sensing film
S1Slowly dripping 1.8mL of valeryl chloride into 30g of ionic liquid 1-ethyl-3-methylimidazole acetate, soaking 1.00g of cotton linter cellulose into the solvent system, magnetically stirring at 70 ℃ in an oil bath to obtain a transparent, viscous and completely dissolved cellulose solution, and keeping the temperature of 70 ℃ for reaction for 12 hours under the condition of continuous magnetic stirring. After the reaction is finished, pouring the system into 200ml of ethanol to terminate the reaction, and then repeatedly washing and filtering by using a large amount of ethanol until the ionic liquid and the unreacted reagent are washed clean to obtain a pure cellulose acetate product;
S2preparing a certain mass of WSCA into 10mL of 1% aqueous solution, weighing 0.0025g of rGO to prepare into 0.25mg/mL aqueous solution, adding the graphene aqueous solution into the prepared WSCA solution, and carrying out ultrasonic treatment on the rGO/WSCA aqueous solution for 30 min;
S3adding 0.006g of vitamin C powder (0.3mg/mL) into an rGO/WSCA aqueous solution, adding the prepared aqueous solution into a three-neck flask, and stirring at the rotation speed of 800rpm for 3 hours under the condition of an oil bath at the temperature of 80 ℃ to obtain a reduced graphene oxide/water-soluble cellulose acetate aqueous solution;
S4after ultrasonic treatment, carrying out suction filtration on the reduced graphene oxide/water-soluble cellulose acetate aqueous solution by using an inorganic filter membrane to form a membrane, after the suction filtration is finished, putting the filter membrane into an oven for drying at 60 ℃ for 30min, and then soaking the filter membrane into an acetone solution until the reduced graphene oxide/water-soluble cellulose acetate is soaked until the reduced graphene oxide/water-soluble cellulose acetate isThe graphene oxide/water-soluble cellulose acetate aqueous solution humidity-sensitive sensing membrane is obtained by dropping the cellulose composite membrane from the filter membrane.
Connecting the prepared rGO/WSCA humidity-sensitive sensing membrane to an electrochemical workstation through a platinum sheet electrode for humidity-sensitive test:
as can be seen from figure 1, WSCA and reduced graphene oxide sheet layers are tightly combined together, and the results are consistent with the results of the previous analysis, and the WSCA and the reduced graphene oxide sheet layers have a hydrogen bonding effect, so that the preparation of the high-strength rGO/WSCA composite membrane is facilitated.
Fig. 2 shows that the surface of the composite film was very smooth, and no fibrous structure and phase separation state were observed. This indicates that the cellulose has completely dissolved and that the cellulose and graphene are very well fused together. The section observation of the composite film shows that the section of the composite film presents a very obvious layered brick-mud structure, graphene sheets are well dispersed in cellulose, and in the film forming process, the graphene sheets are self-assembled to form a regular layered structure.
FIG. 3 shows that the rGO/WSCA composite membrane has good flexibility and mechanical strength.
FIG. 4 shows that the rGO/WSCA humidity-sensitive composite membrane has high humidity sensitivity and low humidity stagnation.
EXAMPLE 3 preparation of moisture-sensitive sensing film
S1Slowly dripping 1.5mL of valeryl chloride into 30g of ionic liquid 1-ethyl-3-methylimidazole acetate, soaking 0.6g of woody cellulose into the solvent system, magnetically stirring at 63 ℃ in an oil bath to obtain a transparent, viscous and completely dissolved cellulose solution, and keeping the temperature for reaction for 9 hours under the condition of continuous magnetic stirring. After the reaction is finished, pouring the system into 200ml of ethanol to terminate the reaction, and then repeatedly washing and filtering by using a large amount of ethanol until the ionic liquid and the unreacted reagent are washed clean to obtain a pure cellulose acetate product;
S2preparing a certain mass of WSCA into 20mL of 0.5% aqueous solution, weighing 0.0005g of rGO into 0.25mg/mL aqueous solution, adding the graphene aqueous solution into the prepared aqueous solutionPerforming ultrasonic treatment on the rGO/WSCA aqueous solution for 30 min;
S3adding 0.0088g of vitamin C powder (0.4mg/mL) into an rGO/WSCA aqueous solution, adding the prepared aqueous solution into a three-neck flask, and stirring for 3 hours at the stirring speed of 800rpm under the condition of an oil bath at the temperature of 80 ℃ to obtain a reduced graphene oxide/water-soluble cellulose acetate aqueous solution;
S4and after ultrasonic treatment, performing suction filtration on the reduced graphene oxide/water-soluble cellulose acetate aqueous solution by using an inorganic filter membrane to form a membrane, after the suction filtration is finished, putting the filter membrane into an oven for drying at 60 ℃ for 30min, and then soaking the filter membrane into an acetone solution until the reduced graphene oxide/water-soluble cellulose acetate composite membrane falls off from the filter membrane to obtain the reduced graphene oxide/water-soluble cellulose acetate aqueous solution humidity-sensitive sensing membrane.
EXAMPLE 4 preparation of moisture-sensitive sensing film
S1Slowly dripping 3mL of valeryl chloride into 30g of ionic liquid 1-ethyl-3-methylimidazole acetate, soaking 1.5g of herbaceous cellulose into the solvent system, magnetically stirring at 55 ℃ in an oil bath to obtain a transparent, viscous and completely dissolved cellulose solution, and keeping the temperature of 55 ℃ for reaction for 6 hours under the condition of continuous magnetic stirring. After the reaction is finished, slowly pouring the system into 200ml of ethanol to terminate the reaction, and then repeatedly washing and filtering by using a large amount of ethanol until the ionic liquid and the unreacted reagent are washed clean, so as to obtain a pure cellulose acetate product;
S2preparing a certain mass of WSCA into 5mL of 2% aqueous solution, weighing 0.04g of rGO to prepare into 2.5mg/mL aqueous solution, adding the graphene aqueous solution into the prepared WSCA solution, and carrying out ultrasonic treatment on the rGO/WSCA aqueous solution for 30 min;
S3adding 0.0105g of vitamin C powder (0.5mg/mL) into the rGO/WSCA aqueous solution, adding the prepared aqueous solution into a three-neck flask, stirring for 3 hours at the temperature of 80 ℃ under an oil bath condition, wherein the stirring speed is 800rpm, and obtaining a reduced graphene oxide/water-soluble cellulose acetate aqueous solution;
S4after ultrasonic treatment, inorganic material is adoptedAnd carrying out suction filtration on the reduced graphene oxide/water-soluble cellulose acetate aqueous solution by using a filter membrane to form a membrane, after the suction filtration is finished, putting the filter membrane into an oven for drying at 60 ℃ for 30min, and then soaking the filter membrane into an acetone solution until the reduced graphene oxide/water-soluble cellulose acetate composite membrane falls off from the filter membrane to obtain the reduced graphene oxide/water-soluble cellulose acetate aqueous solution humidity-sensitive sensing membrane.
EXAMPLE 5 preparation of moisture-sensitive sensing film
S1Slowly dripping 1.8mL of valeryl chloride into 30g of ionic liquid 1-ethyl-3-methylimidazole acetate, soaking 1.00g of cotton linter cellulose into the solvent system, magnetically stirring at 70 ℃ in an oil bath to obtain a transparent, viscous and completely dissolved cellulose solution, and keeping the temperature of 70 ℃ for reaction for 12 hours under the condition of continuous magnetic stirring. After the reaction is finished, pouring the system into 200ml of ethanol to terminate the reaction, and then repeatedly washing and filtering by using a large amount of ethanol until the ionic liquid and the unreacted reagent are washed clean to obtain a pure cellulose acetate product;
S2preparing a certain mass of WSCA into 5mL of 2% aqueous solution, weighing 0.02g of rGO to prepare into 2.5mg/mL aqueous solution, adding the graphene aqueous solution into the prepared WSCA solution, and carrying out ultrasonic treatment on the rGO/WSCA aqueous solution for 30 min;
S3adding 0.0065g of vitamin C powder (0.5mg/mL) into a rGO/WSCA aqueous solution, adding the prepared aqueous solution into a three-neck flask, stirring for 3 hours at the temperature of 80 ℃ under an oil bath condition, wherein the stirring speed is 800rpm, and obtaining a reduced graphene oxide/water-soluble cellulose acetate aqueous solution;
S4and after ultrasonic treatment, performing suction filtration on the reduced graphene oxide/water-soluble cellulose acetate aqueous solution by using an inorganic filter membrane to form a membrane, after the suction filtration is finished, putting the filter membrane into an oven for drying at 60 ℃ for 30min, and then soaking the filter membrane into an acetone solution until the reduced graphene oxide/water-soluble cellulose acetate composite membrane falls off from the filter membrane to obtain the reduced graphene oxide/water-soluble cellulose acetate aqueous solution humidity-sensitive sensing membrane.
EXAMPLE 6 preparation of moisture-sensitive sensing film
S1Slowly dripping 1.8mL of valeryl chloride into 30g of ionic liquid 1-ethyl-3-methylimidazole acetate, soaking 1.00g of cotton linter cellulose into the solvent system, magnetically stirring at 70 ℃ in an oil bath to obtain a transparent, viscous and completely dissolved cellulose solution, and keeping the temperature of 70 ℃ for reaction for 12 hours under the condition of continuous magnetic stirring. After the reaction is finished, pouring the system into 200ml of ethanol to terminate the reaction, and then repeatedly washing and filtering by using a large amount of ethanol until the ionic liquid and the unreacted reagent are washed clean to obtain a pure cellulose acetate product;
S2taking a certain mass of WSCA to prepare 10mL of 1% aqueous solution, weighing 0.01g of rGO to prepare 2.5mg/mL aqueous solution, adding the graphene aqueous solution into the prepared WSCA solution, and carrying out ultrasonic treatment on the rGO/WSCA aqueous solution for 30 min;
S3adding 0.0056g of vitamin C powder (0.5mg/mL) into a rGO/WSCA aqueous solution, adding the prepared aqueous solution into a three-neck flask, and stirring for 3 hours at the temperature of 80 ℃ in an oil bath at the stirring speed of 800rpm to obtain a reduced graphene oxide/water-soluble cellulose acetate aqueous solution;
S4and after ultrasonic treatment, performing suction filtration on the reduced graphene oxide/water-soluble cellulose acetate aqueous solution by using an inorganic filter membrane to form a membrane, after the suction filtration is finished, putting the filter membrane into an oven for drying at 60 ℃ for 30min, and then soaking the filter membrane into an acetone solution until the reduced graphene oxide/water-soluble cellulose acetate composite membrane falls off from the filter membrane to obtain the reduced graphene oxide/water-soluble cellulose acetate aqueous solution humidity-sensitive sensing membrane.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a humidity-sensitive sensing film is characterized by comprising the following steps:
S1modifying cellulose in 1-ethyl-3-methylimidazole acetate serving as an ionic liquid solution by using valeryl chloride as a modifier to prepare water-soluble cellulose acetate WSCA;
S2preparing the water-soluble cellulose acetate into a cellulose aqueous solution, preparing graphene oxide into a graphene oxide aqueous solution, and adding the prepared graphene oxide aqueous solution into the cellulose solution to obtain a cellulose/graphene oxide uniform mixed solution;
S3adding a reducing reagent into the cellulose/graphene oxide mixed solution, and reducing under the condition that water-soluble cellulose acetate is used as a dispersion system to obtain a reduced graphene oxide (rGO)/cellulose aqueous solution;
S4and carrying out ultrasonic vibration treatment on the reduced graphene oxide/cellulose aqueous solution, and then carrying out suction filtration and drying to obtain the flexible rGO/WSCA humidity-sensitive sensing membrane.
2. The method of claim 1, wherein S is1The reaction conditions in (1) are that the reaction temperature is 55-70 ℃ and the reaction time is 6-12 h.
3. The method according to claim 1, wherein 0.5 to 1ml of valeryl chloride as said modifier is added to 10g of 1-ethyl-3-methylimidazolium acetate as said ionic liquid in S1.
4. The method of claim 1, wherein: the cellulose accounts for 2-5% of the mass of the ionic liquid 1-ethyl-3-methylimidazole acetate.
5. The method of claim 1, wherein S is2In the method, the mass concentration of the cellulose aqueous solution is 0.5-2%, the concentration of the graphene oxide aqueous solution is 0.25-2.5mg/mL, and the mass of the graphene oxide is 0.5-40% of the mass of the cellulose.
6. The method of claim 1, wherein the reducing agent is vitamin C, and the concentration of vitamin C is 0.3 to 0.5 mg/ml.
7. The production process according to claim 1, wherein in the step S3, the reduction reaction is carried out under stirring conditions of an oil bath at 80 ℃ for 3 hours at a rotation speed of 800 rpm.
8. The method according to claim 1, wherein the drying temperature of S4 is 60 ℃ and the drying time is 30 min.
9. A moisture-sensitive sensing film produced by the production method as set forth in any one of claims 1 to 8.
10. Use of the moisture-sensitive sensing film according to claim 9 for the preparation of a moisture-sensitive indicator material.
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| CN110790974A (en) * | 2019-11-25 | 2020-02-14 | 华南理工大学 | Cellulose-graphene aerogel material applied to field of gas detection and preparation method thereof |
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| CN113189048A (en) * | 2021-04-27 | 2021-07-30 | 武汉理工大学 | Long-period fiber grating NH3 gas sensor based on graphene oxide/cellulose acetate |
| CN113943439B (en) * | 2021-05-08 | 2022-12-02 | 天津科技大学 | Method for preparing GO/rGO micro-wrinkle humidity-sensitive film by using biodegradable shape memory material |
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