CN111350097A - Preparation method of heating film - Google Patents
Preparation method of heating film Download PDFInfo
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- CN111350097A CN111350097A CN202010235043.3A CN202010235043A CN111350097A CN 111350097 A CN111350097 A CN 111350097A CN 202010235043 A CN202010235043 A CN 202010235043A CN 111350097 A CN111350097 A CN 111350097A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
- D21F11/00—Processes for making continuous lengths of paper, or of cardboard, or of wet web for fibre board production, on paper-making machines
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
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Abstract
The invention relates to a preparation method of a heating film. The method comprises the following steps: putting the whisker carbon nano tube into an Acheson graphitizing furnace, and treating by adopting a heat treatment process to obtain a heat-treated whisker carbon nano tube; soaking the whisker carbon nano tube subjected to heat treatment in fatty acid for a set time to obtain a whisker carbon nano tube subjected to soaking treatment; ball-milling the soaked whisker carbon nano tube, mixing the ball-milled whisker carbon nano tube with a dispersing agent and a solvent, and grinding the mixture by a sand mill to obtain a dispersion liquid of the whisker carbon nano tube; mixing the whisker carbon nanotube dispersion liquid with high-temperature-resistant organic fiber slurry to obtain mixed slurry; and (3) making and drying the mixed slurry, and then carrying out hot-pressing and crosslinking molding to obtain the heating film. The invention can reduce the power attenuation of the heating element.
Description
Technical Field
The invention relates to the field of preparation of heating elements, in particular to a preparation method of a heating film.
Background
With the development of scientific technology and industrial production, the heating element is widely applied to the fields of heat exchange engineering, heating engineering, electronic information and the like, and meanwhile, people put forward new requirements on the heating element and hope that the heating element has excellent comprehensive performance. Most of the traditional heating bodies are PTC ceramic heating bodies, electric heating wire heating bodies, quartz tube heating bodies and carbon fiber heating bodies, and the traditional heating bodies firstly need to be heated to radiate heat outwards. Due to the continuity of temperature, the thermal radiation wave emitted by the infrared radiation device is continuous electromagnetic wave, the infrared thermal wave part of the infrared radiation device comprises mixed waves of near infrared, intermediate infrared, far infrared and the like, the far infrared wave radiation cannot be singly provided, the proportion of the far infrared wave is low, and the requirement of high infrared wave band radiation cannot be met. In addition, the heating elements have low heating speed in different degrees, consume energy, have short heating life and large power attenuation, and are difficult to apply or have high application cost in a certain field.
Disclosure of Invention
The invention aims to provide a preparation method of a heating film, which is used for reducing the power attenuation of a heating body.
In order to achieve the purpose, the invention provides the following scheme:
a method for preparing a heat-generating film comprises the following steps:
putting the whisker carbon nano tube into an Acheson graphitizing furnace, and treating by adopting a heat treatment process to obtain a heat-treated whisker carbon nano tube;
soaking the whisker carbon nano tube subjected to heat treatment in fatty acid for a set time to obtain a whisker carbon nano tube subjected to soaking treatment;
ball-milling the soaked whisker carbon nano tube, mixing the ball-milled whisker carbon nano tube with a dispersing agent and a solvent, and grinding the mixture by a sand mill to obtain a dispersion liquid of the whisker carbon nano tube;
mixing the whisker carbon nanotube dispersion liquid with high-temperature-resistant organic fiber slurry to obtain mixed slurry;
and (3) making and drying the mixed slurry, and then carrying out hot-pressing and crosslinking molding to obtain the heating film.
Optionally, the length of the whisker carbon nanotube is 1-30 μm.
Optionally, the heat treatment temperature in the heat treatment process is 2800-3000 ℃; the heat treatment time in the heat treatment process is 5-30 days.
Optionally, the set time range is 12-24 hours.
Optionally, the soaking the whisker carbon nanotube after the heat treatment in fatty acid for a set time to obtain the whisker carbon nanotube after the soaking treatment specifically includes:
soaking the whisker carbon nano tube subjected to heat treatment in fatty acid for a set time;
washing the soaked whisker carbon nano tube with clean water;
and drying the washed whisker carbon nano tube at 100-150 ℃ to obtain the soaked whisker carbon nano tube.
Optionally, the dispersant is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, CMC, and alcohols.
Optionally, the mass ratio of the dispersing agent to the whisker carbon nanotube ranges from 0.05:1 to 0.2: 1.
Optionally, the solvent is deionized water, purified water, tap water or alcohols.
Optionally, the mixing of the whisker carbon nanotube dispersion liquid and the high-temperature resistant organic fiber slurry to obtain a mixed slurry further includes:
soaking the high-temperature resistant organic fiber in fatty acid for a set time, mixing the high-temperature resistant organic fiber with a fluffing agent and part of water, and sequentially fluffing and pulping to obtain the high-temperature resistant organic fiber pulp.
Optionally, the high-temperature resistant organic fiber is one or more of aramid chopped fiber, aramid fibrid, aramid pulp fiber, polyimide fiber and poly-p-phenylene benzobisoxazole fiber.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
1) the efficiency is higher, more energy-conserving: the heating characteristics of the raw materials are completely different from those of the traditional heating body, the heat conversion rate is higher, and the energy is not consumed; the conversion of electric energy into heat energy is completed instantly, the input electric energy is all emitted in the form of far infrared electromagnetic waves (heat waves) to heat the surrounding air instantly, and the unique properties enable the far infrared material of the invention to have the characteristics of high energy efficiency, high heating speed, more energy saving and the like.
2) No power attenuation and longer service life: the material of the invention can be used for a long time due to the particularity of the material structure and the heating mechanism. The carbon-carbon covalent bond vibrates to generate phonon oscillation and instantly emit far infrared electromagnetic waves, the carbon-carbon covalent bond in the whisker carbon nano tube is the bond with the strongest bonding force among atoms, and the carbon-carbon bond cannot be damaged when the carbon-carbon covalent bond is used in air at the temperature of below 700 ℃. After electrification, the energy of the electrons is completely converted into covalent bond oscillation, and the energy level of the destruction of the covalent bond cannot be reached. Therefore, the heating film manufactured by the invention has long service life and no attenuation of power.
3) Flexibility, processability, acid and alkali resistance and corrosion resistance: the material is a flexible film material, the thickness can be controlled to be 50-200um according to the requirement, the material can be subjected to mechanical processing such as folding, thermoplastic forming, cutting, dripping and drilling, and is acid-base-resistant and corrosion-resistant.
4) The material has low density and is lighter: the material has small density, the gram weight per square meter is 100-200g, the device is not influenced by the volume, and the application field is wider.
5) Has good physical therapy characteristics: only emits pure far infrared rays without near infrared rays and middle infrared rays, the far infrared wave band is 2-20um, the peak value is 9-10um, and the far infrared wave band is a physical therapy wave band required by a human body and has no damage to the human body.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a schematic flow chart of a method for producing a heat-generating film according to example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the whisker carbon nanotube of example 1 of the invention;
FIG. 3 is an X-ray diffraction pattern of a whisker carbon nanotube of example 1 of the invention;
FIG. 4 is a scanning electron micrograph of a heat-generating film prepared in example 1 of the present invention before and after hot pressing;
FIG. 5 is a relative radiation energy spectrum of the heat-generating film of example 1 of the present invention;
FIG. 6 is a diagram showing a heat-generating film in example 1 of the present invention;
fig. 7 is a far infrared heating demonstration diagram of the heating film of example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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 invention.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1
Fig. 1 is a schematic flow chart of a method for producing a heat-generating film according to embodiment 1 of the present invention. As shown in fig. 1, the preparation process of this example is:
step 100: and (3) placing the whisker carbon nano tube in an Acheson graphitizing furnace, and treating by adopting a heat treatment process to obtain the whisker carbon nano tube after heat treatment. The heat treatment process in this example was: and (3) carrying out heat treatment for 5-30 days in a high-temperature vacuum environment at 2800-3000 ℃ to ensure that carbon atoms obtain enough energy, rearranging the carbon atoms, returning the carbon atoms to the state with the lowest energy of a system, and having a six-membered ring arrangement structure, thereby greatly improving the crystallinity and the thermal stability of the whisker carbon nanotube, eliminating surface defects and reducing the surface energy. The high-temperature long-time graphitization treatment causes the surface energy of the whisker carbon nano tube to be reduced, the surface has very strong hydrophobic performance, the wetting angle is close to 180 degrees, and the whisker carbon nano tube has extremely high purity and crystallinity.
Fig. 2 is a scanning electron microscope image of the whisker carbon nanotube in example 1 of the invention, and fig. 3 is an X-ray diffraction pattern of the whisker carbon nanotube in example 1 of the invention. As shown in fig. 2 and fig. 3, the whisker carbon nanotube of the present embodiment has a linear structure, a length of 1 to 30 μm, a crystallinity of 98%, and a high far infrared emissivity and a high electrothermal conversion efficiency.
Step 200: and soaking the whisker carbon nano tube subjected to heat treatment in fatty acid for a set time to obtain the whisker carbon nano tube subjected to soaking treatment. In the embodiment, the set time is 12-24 hours, and the whisker carbon nanotube after heat treatment is soaked in fatty acid for 12-24 hours, so that the hydrophobic property of the whisker carbon nanotube is further enhanced. After soaking, the mixture can be washed by clean water for 3-5 times and then dried in a drying box at 100-150 ℃.
Step 300: and performing ball milling treatment on the soaked whisker carbon nano tube, mixing the ball milled whisker carbon nano tube with a dispersing agent and a solvent, and then grinding the mixture by a sand mill to obtain a whisker carbon nano tube dispersion liquid. In the embodiment, the dispersing agent is one or more of Sodium Dodecyl Sulfate (SDS), Sodium Dodecyl Benzene Sulfonate (SDBS), polyvinylpyrrolidone (PVP), CMC, and alcohols (ethylene glycol), and the mass ratio of the dispersing agent to the whisker carbon nanotube is 0.05: 1-0.2: 1, and more preferably 0.1: 1-0.15: 1. In this embodiment, the solvent is deionized water, purified water, tap water or alcohol, preferably ethanol. The invention has no special requirement on the dosage of the solvent, and only serves as a fiber carrier, and can uniformly disperse the whisker carbon nanotube and the high-temperature resistant fiber into suspension.
Step 400: and mixing the whisker carbon nanotube dispersion liquid with the high-temperature-resistant organic fiber slurry to obtain mixed slurry. In this embodiment, a double-planetary mixer is used to mix the mixture of the whisker carbon nanotube dispersion liquid and the high-temperature resistant organic fiber slurry.
In this embodiment, the high-temperature resistant organic fiber is one or a mixture of several of aramid chopped fiber, aramid fibrid, aramid pulp fiber, Polyimide (PI) fiber, and poly (p-Phenylene Benzobisoxazole) (PBO) fiber. The preparation process of the high-temperature resistant organic fiber slurry comprises the following steps: soaking the high-temperature resistant organic fiber in fatty acid for 12-24 hours, washing for 3-5 times, mixing with a defibering agent and part of water, and sequentially performing defibering and pulping to obtain the high-temperature resistant organic fiber pulp with the strong hydrophobic surface.
Step 500: and (3) making and drying the mixed slurry, and then carrying out hot-pressing and glue-linking molding to obtain the heating film. Specifically, the flexible high-temperature-resistant far infrared heating film can be obtained by adopting a special paper machine for papermaking, drying and then carrying out hot-pressing crosslinking molding. Fig. 4 is scanning electron micrographs before and after hot pressing of the heating film prepared in example 1 of the present invention, wherein the left part is the scanning electron micrograph before hot pressing, the right part is the scanning electron micrograph after hot pressing, and fig. 5 is the relative radiation energy spectrum of the heating film of example 1 of the present invention. As shown in fig. 4 and 5, the heating film prepared by the embodiment has higher efficiency and is more energy-saving, the conversion of electric energy into heat energy is completed instantly, all the input electric energy is emitted in the form of far-infrared electromagnetic waves (heat waves), the ambient air is heated instantly, and the temperature can be raised to a set temperature (45 ℃ -500 ℃) within 1 second, so that the far-infrared material has the characteristics of high energy efficiency, high heating speed, more energy saving and the like.
In this embodiment, after the whisker carbon nanotube and the high temperature resistant organic fiber are treated by soaking in fatty acid, the hydrophobic properties of the two are increased, and the surfaces of the two materials are both strongly hydrophobic. In water, the whisker carbon nano tube needs to be adsorbed on the surface of the high-temperature resistant fiber to reduce the surface energy, so that the retention rate and the water filtration performance of the whisker carbon nano tube during later papermaking can be greatly improved, the distribution uniformity of the whisker carbon nano tube is facilitated, the whisker carbon nano tube is not easy to fall off, and the like, and the loss of the whisker carbon nano tube in the manufacturing process of a film is avoided.
Utilize whisker carbon nanotube and high temperature resistant organic fiber complex to make flexible high temperature resistant phonon to vibrate the film that generates heat in this embodiment, it generates heat and vibrates the production by the phonon, and the frequency range of its vibrations is in 2 ~ 20um, and this wave band belongs to the far infrared wave band, and the electric energy converts heat energy into with the form of pure far infrared. The electro-far infrared emission performance of the carbon material is determined by the crystallinity of the material, and the high-crystallinity whisker carbon nano tube can generate phonon oscillation with the wavelength of 2-20 um. The common carbon nano tube has more surface defects and very low crystallinity, phonon oscillation cannot be generated when the common carbon nano tube is electrified, electric energy is mainly consumed in the mode of resistance heating, the generated heat waves comprise near infrared and intermediate infrared, the occupied ratio and the intensity of the far infrared are very low, the electric energy is essentially the same as the heating mechanism of a resistance wire, the self temperature is higher than the ambient temperature, heat radiation can be generated under the condition to heat other objects, the spectrum of the heat radiation is a continuous spectrum, and the wavelength coverage range can theoretically range from 0 to infinity. Generally, heat radiation is mainly based on visible light and infrared light having a relatively long wavelength, depending on the temperature of the heating element. Therefore, since the heating mechanism is completely different from that of the whisker carbon nanotube, the common carbon material does not have the property of emitting heat in a pure far infrared band.
Fig. 6 is a real diagram of the heating film of embodiment 1 of the present invention, and fig. 7 is a far infrared heating demonstration diagram of the heating film of embodiment 1 of the present invention. As shown in fig. 6 and 7, the heat-generating film prepared in this example had the following characteristics: the resistivity rho is 0.01-0.1 omega cm. After the power is on, the carbon-carbon covalent bond vibrates to generate phonon oscillation to emit electromagnetic waves in a far infrared wave band, the device has the advantages of pure far infrared emission function (2-20 mu m), no self heating, no energy consumption, conversion of most of electric energy into far infrared electromagnetic wave radiation, instant electric heating conversion, extremely high heating speed, high heating rate of 200 plus materials per second, electric heating conversion efficiency of more than 99 percent, working temperature of 300 plus materials of 500 ℃, high strength, high temperature resistance, acid and alkali resistance, flexible processing and the like.
Example 2
And (3) placing the whisker carbon nano tube in an Acheson graphitizing furnace, and placing the whisker carbon nano tube in a 2800-DEG argon-protected high-temperature environment for 5 days to obtain the high-purity high-crystallinity whisker carbon nano tube. The length of the whisker carbon nanotube in the embodiment is 4-6 μm.
Soaking the whisker carbon nanotube in fatty acid for 12 hours to make the whisker carbon nanotube more hydrophobic, washing the whisker carbon nanotube with clean water for 5 times, and drying the whisker carbon nanotube in a drying box at 100 ℃.
Ball-milling the whisker carbon nanotube in a ball mill at the rotating speed of 1000r/min, mixing the whisker carbon nanotube with polyvinylpyrrolidone and water, and grinding the mixture for 30min by a sand mill to obtain a whisker carbon nanotube dispersion liquid; wherein the ratio of the whisker carbon nanotube to the polyvinylpyrrolidone to the water is 5: 1: 94.
soaking aramid chopped fibers and aramid fibrids in fatty acid for 12 hours, washing for 3-5 times, mixing with polyoxyethylene and part of water, and sequentially defibering and pulping to obtain high-temperature-resistant organic fiber pulp;
and mixing the obtained whisker carbon nanotube dispersion liquid with the high-temperature-resistant organic fiber slurry, and then stirring the obtained mixture by a double-planet stirrer to obtain mixed slurry.
And (3) making and drying the obtained mixed slurry by a special paper machine, and then carrying out hot press molding to obtain the flexible high-temperature-resistant phonon oscillation heating film.
The parameters of the heat-generating film produced in this example are shown in table 1.
TABLE 1 exothermic film parameters
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A method for preparing a heating film is characterized by comprising the following steps:
putting the whisker carbon nano tube into an Acheson graphitizing furnace, and treating by adopting a heat treatment process to obtain a heat-treated whisker carbon nano tube;
soaking the whisker carbon nano tube subjected to heat treatment in fatty acid for a set time to obtain a whisker carbon nano tube subjected to soaking treatment;
ball-milling the soaked whisker carbon nano tube, mixing the ball-milled whisker carbon nano tube with a dispersing agent and a solvent, and grinding the mixture by a sand mill to obtain a dispersion liquid of the whisker carbon nano tube;
mixing the whisker carbon nanotube dispersion liquid with high-temperature-resistant organic fiber slurry to obtain mixed slurry;
and (3) making and drying the mixed slurry, and then carrying out hot-pressing and crosslinking molding to obtain the heating film.
2. The method for producing a heat-generating thin film according to claim 1, wherein the length of the whisker carbon nanotube is 1 to 30 μm.
3. The method for preparing a heat-generating film according to claim 1, wherein the heat treatment temperature in the heat treatment process is 2800 to 3000 ℃; the heat treatment time in the heat treatment process is 5-30 days.
4. The method for producing a heat-generating film according to claim 1, wherein the set time is in a range of 12 to 24 hours.
5. The method for preparing a heating film according to claim 1, wherein the step of immersing the heat-treated whisker carbon nanotube in fatty acid for a set time to obtain the immersed whisker carbon nanotube specifically comprises:
soaking the whisker carbon nano tube subjected to heat treatment in fatty acid for a set time;
washing the soaked whisker carbon nano tube with clean water;
and drying the washed whisker carbon nano tube at 100-150 ℃ to obtain the soaked whisker carbon nano tube.
6. The method of claim 1, wherein the dispersant is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, CMC, and alcohols.
7. The method for producing a heat-generating thin film according to claim 1, wherein the mass ratio of the dispersant to the whisker carbon nanotube is in a range of 0.05:1 to 0.2: 1.
8. The method for preparing a heat-generating film according to claim 1, wherein the solvent is deionized water, purified water, tap water or alcohols.
9. The method for preparing a heat-generating film according to claim 1, wherein the mixing of the whisker carbon nanotube dispersion liquid and the high-temperature resistant organic fiber slurry to obtain a mixed slurry further comprises:
soaking the high-temperature resistant organic fiber in fatty acid for a set time, mixing the high-temperature resistant organic fiber with a fluffing agent and part of water, and sequentially fluffing and pulping to obtain the high-temperature resistant organic fiber pulp.
10. The method for producing a heat-generating film according to claim 9, wherein the high-temperature-resistant organic fiber is one or more of an aramid chopped fiber, an aramid fibrid, an aramid pulp fiber, a polyimide fiber, and a polyparaphenylene benzobisoxazole fiber.
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| CN113784468B (en) * | 2021-09-10 | 2024-03-12 | 四川普利司德高分子新材料有限公司 | Heating material and application thereof, conductive heating film and manufacturing method thereof |
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Effective date of registration: 20230518 Address after: 450000 Henan Xinbo Mining Equipment Technology Co., Ltd., Industrial Agglomeration Zone, Dengfeng City, Zhengzhou City, Henan Province (Jiaohe Village, Zhongyue District) Patentee after: HENAN KELAIWEI NANO CARBON MATERIAL Co.,Ltd. Address before: 330000 west of Jinsha 3rd road and south of Fushan 1st Road, Xiaolan economic and Technological Development Zone, Nanchang County, Nanchang City, Jiangxi Province Patentee before: JIANGXI KELAIWEI CARBON NANO MATERIALS Co.,Ltd. |