CN110540198B - Graphene oxide-based self-repairing flame-retardant composite film, preparation thereof and fire alarm - Google Patents
Graphene oxide-based self-repairing flame-retardant composite film, preparation thereof and fire alarm Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- G—PHYSICS
- G08—SIGNALLING
- G08B—SIGNALLING OR CALLING SYSTEMS; ORDER TELEGRAPHS; ALARM SYSTEMS
- G08B17/00—Fire alarms; Alarms responsive to explosion
- G08B17/06—Electric actuation of the alarm, e.g. using a thermally-operated switch
Abstract
The application belongs to the technical field of thermosensitive materials, and particularly relates to a graphene oxide-based self-repairing flame-retardant composite film, preparation thereof and a fire alarm. The application provides a preparation method of a graphene oxide-based self-repairing flame-retardant composite film, which comprises the following steps: step 1, mixing graphene oxide, a solvent and a reducing agent for partial reduction to obtain modified graphene oxide; step 2, mixing the modified graphene oxide with a conductive material, and performing film forming treatment to obtain a graphene oxide-based composite film; and 3, coating a self-repairing flame-retardant polymer on the surface of the graphene oxide-based composite film to obtain the graphene oxide-based self-repairing flame-retardant. The application provides a preparation method and application of a graphene oxide-based self-repairing flame-retardant composite film in fire alarm, which can effectively solve the problems of long response time, short service life and poor weather resistance of the conventional fire alarm.
Description
Technical Field
The application belongs to the technical field of thermosensitive materials, and particularly relates to a graphene oxide-based self-repairing flame-retardant composite film, preparation thereof and a fire alarm.
Background
Frequent fire accidents occur due to the burning of combustible materials, which not only causes huge losses of life, property and medical expenses, but also causes serious damage to the environment and climate. In order to effectively reduce the danger caused by fire, an effective method is to use a fire alarm, when a fire breaks out, the fire alarm needs to trigger an alarm quickly, so that the occurrence of fire accidents is reduced, therefore, a heat-sensitive material in the fire alarm is required to respond to heat quickly, the existing thermistor film is widely applied to the fire alarm as a good thermosensitive material, the existing thermistor film has the technical defect that the resistance of the existing thermistor film is too large after the existing thermistor film reaches a preset temperature, so that the electric conduction sensitivity of the thermistor film is low, and the alarm response time of the fire alarm manufactured by taking the thermistor film as a core is too long after the fire alarm reaches the preset temperature.
In summary, in order to effectively prevent the fire risk, it is highly desirable to develop a thermistor film and a fire alarm device that can rapidly respond in a fire, so as to improve the thermal sensitivity of the thermistor film, and to rapidly activate the thermistor film after contacting with a flame, thereby achieving the purpose of fire alarm.
Disclosure of Invention
In view of this, the application provides a graphene oxide-based self-repairing flame-retardant composite film, a preparation method thereof and a fire alarm, and can effectively solve the problems of long response time, short service life and poor weather resistance of the fire alarm caused by poor conductivity of the existing thermistor film.
The application provides a preparation method of a graphene oxide-based self-repairing flame-retardant composite film, which comprises the following steps:
step 1, mixing graphene oxide, a solvent and a reducing agent for partial reduction to obtain modified graphene oxide;
step 2, mixing the modified graphene oxide with a conductive material, and performing film forming treatment to obtain a graphene oxide-based composite film;
and 3, coating a self-repairing flame-retardant polymer on the surface of the graphene oxide-based composite film to obtain the graphene oxide-based self-repairing flame-retardant composite film.
Preferably, the reducing agent is selected from one or more of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), Polydopamine (PDA) and Polyethyleneimine (PEI).
Preferably, the mass ratio of the graphene oxide to the reducing agent is (1-10): 1. more preferably, the mass ratio of the graphene oxide to the reducing agent is 5: 1.
preferably, in step 1, the conditions for the partial reduction are: reacting for 10-15h at 60-100 ℃ under the condition of inert atmosphere. More preferably, the conditions for the partial reduction are: and reacting for 14h at 70 ℃.
Preferably, the solvent is selected from one or more of tetrahydrofuran, absolute ethanol, DMSO and DMF.
Preferably, the conductive material is selected from one or more of carbon nanotubes, two-dimensional carbon nitride compound Mxene, graphite and graphene.
Preferably, the mass ratio of the modified graphene oxide to the conductive material is (5-50): 1. most preferably, the mass ratio of the modified graphene oxide to the conductive material is 40: 1.
preferably, the self-healing flame retardant polymer is selected from the group consisting of polyborosiloxane resins.
Specifically, the preparation method of the polyborosiloxane resin comprises the following steps: reacting boric acid with hydroxy-terminated polydimethylsiloxane, reacting for two hours at room temperature, and washing to obtain the polyborosiloxane resin.
The film forming treatment is the conventional film forming method, and can be a suction filtration film forming method, or other film forming methods such as evaporation coating, vacuum rotary coating or spraying.
The graphene oxide-based self-repairing flame-retardant composite film provided by the application has the thickness of 1-5 mm.
Further, the application discloses an application of the graphene oxide-based self-repairing flame-retardant composite film or the graphene oxide-based self-repairing flame-retardant composite film prepared by the preparation method in fire alarm.
Further, the application also provides a fire alarm, which comprises the graphene oxide-based self-repairing flame-retardant composite film or the graphene oxide-based self-repairing flame-retardant composite film prepared by the preparation method.
The fire alarm circuit assembly can be formed by connecting a power supply, a switch, a buzzer or an alarm lamp or a buzzing alarm lamp and the graphene oxide-based self-repairing flame-retardant composite film in series through a wire.
The purpose of this application is to there is the problem that response time is long and life is short in current fire alarm, through adopting the fire-retardant complex film of oxidation graphite alkene base selfreparing to use in fire alarm, solves these problems. The invention discovers that after the oxygen-containing functional group on the surface of the graphene oxide falls off, the graphene oxide can be converted from an insulating state to a conductive state, but because the thermal stability of the epoxy group of the graphene oxide is higher, the required thermal reduction temperature is also higher, and when the graphene oxide falls off under the high-temperature condition (200 ℃ C. and 300 ℃ C.), the oxygen-containing functional group of the graphene oxide needs to fall off for a longer time, so that the thermal sensitivity of the graphene oxide is low, and the current requirement is not met. Therefore, the graphene oxide is modified by the reducing agent with lower reducibility at low temperature, so that partial reduction of the graphene oxide can be realized, partial epoxy groups of the graphene oxide are opened after the graphene oxide is partially reduced, other functional groups of the graphene oxide are not modified, the epoxy groups of the graphene oxide are opened, then, a conductive material is added, partial thermal reduction graphene oxide sheets in the graphene oxide can be connected with each other to form a conductive network, and the graphene oxide is rapidly reduced under the flame condition, so that an alarm is rapidly generated, and the purpose of fire alarm is achieved. In addition, the polyborosiloxane resin is coated on the surface of the prepared graphene oxide-based composite film, so that the flame retardant effect and the self-repairing performance of the polyborosiloxane can be exerted, the internal graphene oxide can be protected from being damaged by the external environment, the structural integrity of the graphene oxide-based composite film can be ensured in a high-temperature environment, in addition, the graphene oxide-based composite film can be protected from being damaged due to the self-repairing performance, and the service life of the graphene oxide-based composite film can be prolonged.
The invention also provides application of the graphene oxide and the self-repairing flame-retardant composite film in fire alarm, so that the sensitivity of the fire alarm can be greatly improved, and the service life of the fire alarm can be prolonged due to the self-repairing performance and the flame-retardant performance.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
Fig. 1 is a microscopic morphology of a graphene oxide-based self-repairing flame-retardant composite film provided in embodiment 1 of the present application before flame combustion;
fig. 2 is a microscopic morphology of the graphene oxide-based self-repairing flame-retardant composite film provided in embodiment 1 of the present application after flame combustion;
fig. 3 is a shape of a crack produced by an external force of the graphene oxide-based self-repairing flame-retardant composite film provided in embodiment 1 of the present application;
fig. 4 is a self-repaired morphology of the graphene oxide-based self-repair flame-retardant composite film provided in embodiment 1 of the present application;
fig. 5 is an assembly schematic diagram of a fire alarm provided by an embodiment of the application.
Detailed Description
The application provides a graphene oxide-based self-repairing flame-retardant composite film, a preparation method thereof and a fire alarm, which are used for solving the technical problems of long response time, short service life and poor weather resistance of the conventional fire alarm.
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Among them, the graphene oxide used in the following examples is conventional graphene oxide, for example, graphene oxide conventionally prepared by Hummers method.
Example 1
The embodiment of the application provides a first graphene oxide-based self-repairing flame-retardant composite film and a first temperature detector, and the method comprises the following specific steps:
1. selecting the following components in a mass ratio of 5: respectively ultrasonically dispersing the graphene oxide of 1 and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) in tetrahydrofuran to obtain a graphene oxide solution and a DOPO solution, introducing nitrogen or argon as a shielding gas at 70 ℃, mixing the graphene oxide solution and the DOPO solution for partial reduction, and reacting for 14 hours to obtain the modified graphene oxide.
2. Selecting the materials with the mass ratio of 40: 1, respectively dispersing the modified graphene oxide and the carbon nano tube in an aqueous solution, mixing, and performing suction filtration to form a film, thus obtaining the graphene oxide-based composite film.
3. Preparation of polyborosiloxane resin: reacting boric acid with hydroxy-terminated polydimethylsiloxane, reacting for two hours at room temperature, and then washing to obtain polyborosiloxane resin; and coating a layer of polyborosiloxane resin on the surface of the graphene oxide-based composite film to prepare the graphene oxide-based self-repairing flame-retardant composite film.
4. Referring to fig. 5, fig. 5 is an assembly schematic diagram of a fire alarm provided in an embodiment of the present application, in which a dc voltage-stabilized power supply 1, a switch 2, a graphene oxide-based self-repairing flame-retardant composite film 3 obtained in step 3, and an alarm lamp 4 are sequentially connected in series through a wire to assemble the fire alarm.
Example 2
The embodiment of the application provides a second graphene oxide-based self-repairing flame-retardant composite film and a second fire alarm, and the method comprises the following specific steps:
1. selecting the materials with the mass ratio of 10: respectively ultrasonically dispersing the graphene oxide and Polydopamine (PDA) of the step 1 in DMSO to obtain a graphene oxide solution and a PDA solution, introducing nitrogen or argon as a protective gas at 60 ℃, mixing the graphene oxide solution and the PDA solution for partial reduction, and reacting for 10 hours to obtain the modified graphene oxide.
2. Selecting modified graphene oxide and Mxene with the mass ratio of 10:1, respectively dispersing the modified graphene oxide and the Mxene in an aqueous solution, mixing, and performing suction filtration to form a film, thus obtaining the graphene oxide-based composite film.
3. Preparation of polyborosiloxane resin: reacting boric acid with hydroxy-terminated polydimethylsiloxane, reacting for two hours at room temperature, and then washing to obtain polyborosiloxane resin; and coating a layer of polyborosiloxane resin on the surface of the graphene oxide-based composite film to prepare the graphene oxide-based self-repairing flame-retardant composite film.
4. And (3) sequentially connecting the direct-current stabilized voltage supply, the switch, the graphene oxide-based self-repairing flame-retardant composite film in the step (3) and the alarm lamp in series through a wire to assemble the fire alarm.
Example 3
The embodiment of the application provides a third graphene oxide-based self-repairing flame-retardant composite film and a third fire alarm, and the method specifically comprises the following steps:
1. selecting the materials with the mass ratio of 3: respectively ultrasonically dispersing the graphene oxide and Polyethyleneimine (PEI) of 1 in DMF to obtain a graphene oxide solution and a PEI solution, introducing nitrogen or argon as a protective gas at 100 ℃, mixing the graphene oxide solution and the PEI solution for partial reduction, and reacting for 12h to obtain the modified graphene oxide.
2. Selecting modified graphene oxide and graphene with a mass ratio of 30:1, respectively dispersing the modified graphene oxide and the graphene in an aqueous solution, mixing, and performing suction filtration to form a film, thus obtaining the graphene oxide-based composite film.
3. Preparation of polyborosiloxane resin: reacting boric acid with hydroxy-terminated polydimethylsiloxane, reacting for two hours at room temperature, and then washing to obtain polyborosiloxane resin; and coating a layer of polyborosiloxane resin on the surface of the graphene oxide-based composite film to prepare the graphene oxide-based self-repairing flame-retardant composite film.
4. And (3) sequentially connecting the direct-current stabilized voltage supply, the switch, the graphene oxide-based self-repairing flame-retardant composite film in the step (3) and the alarm lamp in series through a wire to assemble the fire alarm.
Comparative example
The embodiment of the application provides a comparative product, the preparation method of which is similar to that of the comparative product 1, and the difference between the two is only that in the step 2 of the comparative example, the modified graphene oxide is dispersed in the aqueous solution, and then the modified graphene oxide is filtered and filtered to form a film, so that the graphene oxide-based composite material in a film shape is prepared, and the rest steps are consistent with those of the example 1, so that the composite film 1 and the comparative product 1 of the fire alarm are prepared.
Example 4
1. Selecting the following components in a mass ratio of 5: respectively ultrasonically dispersing the graphene oxide of 1 and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) in tetrahydrofuran to obtain a graphene oxide solution and a DOPO solution, introducing nitrogen or argon as a shielding gas at 70 ℃, mixing the graphene oxide solution and the DOPO solution for partial reduction, and reacting for 12 hours to obtain the modified graphene oxide.
2. Selecting the materials with the mass ratio of 50: 1, respectively dispersing the modified graphene oxide and the carbon nano tube in an aqueous solution, and then mixing, filtering and forming a film to obtain the film-shaped graphene oxide-based composite material.
3. Preparation of polyborosiloxane resin: reacting boric acid with hydroxy-terminated polydimethylsiloxane, reacting for two hours at room temperature, and then washing to obtain polyborosiloxane resin; and coating a layer of polyborosiloxane resin on the surface of the graphene oxide-based composite film to prepare the graphene oxide-based self-repairing flame-retardant composite film.
4. And (3) sequentially connecting the direct-current voltage-stabilized power supply, the switch, the graphene oxide-based self-repairing flame-retardant composite film in the step (3) and the alarm lamp in series through a wire to assemble the fire alarm temperature detector.
The embodiment of the application provides sensitivity for detecting a temperature detector, microscopic morphology of a graphene oxide-based self-repairing flame-retardant composite film and self-repairing performance of the graphene oxide-based self-repairing flame-retardant composite film, and the method comprises the following specific steps:
1. the sensitivity of the fire alarm prepared in examples 1 to 4 and the comparative fire alarm prepared in the comparative example 1 was tested using a dc regulated power supply of APS3005Si (ATTEN), the sensitivity of the fire alarm prepared in examples 1 to 3 was tested using an electrical signal of the graphene oxide-based self-healing flame-retardant composite film in flame, the selected voltage was 3V, the sensitivity of the fire alarm was analyzed by the light emission of the alarm lamp, the test was started, the graphene oxide-based self-healing flame-retardant composite film prepared in examples 1 to 4 and the composite film 1 prepared in the comparative example were ignited by flame, the response time of the light emission of the alarm lamp and the value of the resistance after ignition were calculated, and the results are shown in table 1.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example | |
| Response time/s | 35 | 42 | 37 | 43 | 80 |
| Resistance omega | 65 | 71 | 90 | 123 | 1000 |
2. Field Emission Scanning Electron Microscope (FESEM): the model of a field emission scanning electron microscope used for testing is NOVA NanoSEM430 (netherlands), and the microscopic appearances of the graphene oxide-based self-repairing flame-retardant composite film prepared in example 1 before and after ignition are tested, and the results are shown in fig. 1 and fig. 2, where fig. 1 is the microscopic appearance of the graphene oxide-based self-repairing flame-retardant composite film provided in example 1 of the present application before flame combustion, and fig. 2 is the microscopic appearance of the graphene oxide-based self-repairing flame-retardant composite film provided in example 1 of the present application after flame combustion. The result shows that the surface of the graphene oxide-based self-repairing flame-retardant composite film after flame combustion becomes more compact, and the compact carbon layer is formed after the polyborosiloxane resin on the surface layer is combusted.
3. Self-repairing performance test: and (3) scribing a crack on the surface of the graphene oxide-based self-repairing flame-retardant composite film by using a knife, and observing the change condition of the crack on the surface. As shown in fig. 3 and 4, fig. 3 is a shape of a crack produced by an external force of the graphene oxide-based self-repairing flame retardant composite film provided in embodiment 1 of the present application, and fig. 4 is a shape of the graphene oxide-based self-repairing flame retardant composite film provided in embodiment 1 of the present application after self-repairing. The result shows that the graphene oxide-based self-repairing flame-retardant composite film of the embodiment 1 can repair cracks and shows self-repairing performance.
The foregoing is only a preferred embodiment of the present application and it should be noted that those skilled in the art can make several improvements and modifications without departing from the principle of the present application, and these improvements and modifications should also be considered as the protection scope of the present application.
Claims (7)
1. A preparation method of a graphene oxide-based self-repairing flame-retardant composite film for a fire alarm is characterized by comprising the following steps of:
step 1, mixing graphene oxide, a solvent and a reducing agent for partial reduction to obtain modified graphene oxide; the reducing agent is selected from one or more of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, polydopamine and polyethyleneimine; the conditions for the partial reduction are: reacting for 10-15h at 60-100 ℃ under the condition of inert atmosphere; the solvent is selected from one or more of tetrahydrofuran, absolute ethyl alcohol, DMSO and DMF;
step 2, mixing the modified graphene oxide with a conductive material, and performing film forming treatment to obtain a graphene oxide-based composite film;
and 3, coating a self-repairing flame-retardant polymer on the surface of the graphene oxide-based composite film to obtain the graphene oxide-based self-repairing flame-retardant composite film.
2. The preparation method according to claim 1, wherein the mass ratio of the graphene oxide to the reducing agent is (1-10): 1.
3. the method according to claim 1, wherein the conductive material is selected from one or more of carbon nanotubes, two-dimensional carbon nitride Mxene, graphite, and graphene.
4. The preparation method according to claim 1, wherein the mass ratio of the modified graphene oxide to the conductive material is (5-50): 1.
5. the method of making according to claim 1, wherein the self-healing flame retardant polymer is selected from the group consisting of polyborosiloxane resins.
6. A graphene oxide-based self-repairing flame-retardant composite film is characterized by comprising the graphene oxide-based self-repairing flame-retardant composite film prepared by the preparation method of any one of claims 1 to 5.
7. A fire alarm device is characterized by comprising the graphene oxide-based self-repairing flame-retardant composite film prepared by the preparation method of any one of claims 1 to 5 or the graphene oxide-based self-repairing flame-retardant composite film of claim 6.
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| CN111411519B (en) * | 2020-03-27 | 2021-11-26 | 东华大学 | Early-warning type flame-retardant polylactic acid fabric and preparation method thereof |
| CN111662475B (en) * | 2020-06-17 | 2022-12-23 | 山东师范大学 | Intelligent early warning flame-retardant material prepared from modified high-molecular polymer, and preparation method and application thereof |
| CN112457824B (en) * | 2020-11-16 | 2022-01-14 | 中科院广州化学有限公司 | Efficient heat-conducting graphene flexible film, preparation and application in intelligent fire alarm |
| CN114141428B (en) * | 2021-11-12 | 2023-09-29 | 复旦大学 | Preparation method of ultrafast self-repairing, high-viscosity and deformable silicon rubber electrode material |
| CN114889175B (en) * | 2022-05-25 | 2023-07-18 | 福州大学 | Preparation and application of modified graphene oxide/hydroxyapatite nanowire composite paper |
| CN115353101B (en) * | 2022-08-24 | 2024-02-20 | 贵州大学 | Modified graphene oxide film with high sensitivity and high thermal stability |
| ES2957845A1 (en) * | 2023-09-21 | 2024-01-26 | Univ Madrid Politecnica | Fire alarm sensor, house and furniture comprising said sensor and method of manufacturing fire alarm sensor (Machine-translation by Google Translate, not legally binding) |
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| CN105273727A (en) * | 2015-11-25 | 2016-01-27 | 北京旭碳新材料科技有限公司 | Composition for flame-retardant composite material and graphene oxide flame-retardant film as well as preparation method and application of graphene oxide flame-retardant film |
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