CN115627040B - Composite material resistant to low temperature of-50 ℃ for sealing, preparation method and sensor - Google Patents
Composite material resistant to low temperature of-50 ℃ for sealing, preparation method and sensor Download PDFInfo
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- CN115627040B CN115627040B CN202211363270.XA CN202211363270A CN115627040B CN 115627040 B CN115627040 B CN 115627040B CN 202211363270 A CN202211363270 A CN 202211363270A CN 115627040 B CN115627040 B CN 115627040B
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000007789 sealing Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229920001973 fluoroelastomer Polymers 0.000 claims abstract description 17
- HFJRKMMYBMWEAD-UHFFFAOYSA-N dodecanal Chemical compound CCCCCCCCCCCC=O HFJRKMMYBMWEAD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000002105 nanoparticle Substances 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical group CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- SHFJWMWCIHQNCP-UHFFFAOYSA-M hydron;tetrabutylazanium;sulfate Chemical compound OS([O-])(=O)=O.CCCC[N+](CCCC)(CCCC)CCCC SHFJWMWCIHQNCP-UHFFFAOYSA-M 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- ZFVMWEVVKGLCIJ-UHFFFAOYSA-N bisphenol AF Chemical compound C1=CC(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C=C1 ZFVMWEVVKGLCIJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000012459 cleaning agent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000003566 sealing material Substances 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 10
- 239000011159 matrix material Substances 0.000 abstract description 4
- 125000000217 alkyl group Chemical group 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000012767 functional filler Substances 0.000 abstract 1
- 239000013096 zirconium-based metal-organic framework Substances 0.000 abstract 1
- 230000004048 modification Effects 0.000 description 16
- 238000012986 modification Methods 0.000 description 16
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 3
- 239000012621 metal-organic framework Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- GPNNOCMCNFXRAO-UHFFFAOYSA-N 2-aminoterephthalic acid Chemical compound NC1=CC(C(O)=O)=CC=C1C(O)=O GPNNOCMCNFXRAO-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920006247 high-performance elastomer Polymers 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000013212 metal-organic material Substances 0.000 description 1
- 239000013105 nano metal-organic framework Substances 0.000 description 1
- 239000013289 nano-metal-organic framework Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions 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 a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions 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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions 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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D11/00—Component parts of measuring arrangements not specially adapted for a specific variable
- G01D11/24—Housings ; Casings for instruments
- G01D11/26—Windows; Cover glasses; Sealings therefor
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised 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 a halogen; Derivatives of such polymers
- C08J2327/02—Characterised 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 a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised 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 a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2487/00—Characterised by the use of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Sealing Material Composition (AREA)
Abstract
The application belongs to the technical field of sealing composite materials, and in particular relates to a composite material for sealing, which is resistant to low temperature of minus 50 ℃, wherein a modified nano zirconium-based metal-organic framework material (UiO-66-NH) is introduced into a fluororubber matrix by a solution blending method 2 ) For functional filler preparation, benefits from modified UiO-66-NH 2 The polar effect of alkyl long-chain dodecanal grafted on the outer surface of the particles is low, the compatibility between the particles and the fluororubber matrix is improved, and the composite material has excellent bonding strength and mechanical property at low temperature. The application also provides a preparation method of the composite material and a sensor using the composite material. The method is suitable for being used in a low-temperature environment in the power industry.
Description
Technical Field
The application belongs to the technical field of electronic product sealing composite materials, and particularly discloses a sealing composite material resistant to low temperature of-50 ℃, a preparation method thereof and a sensor using the sealing composite material resistant to low temperature of-50 ℃.
Background
Protection and sealing are critical processes in the sensor manufacturing process, and improper handling may cause sensor failure or errors beyond the allowable range. Taking a weighing sensor as an example, if the protection sealing effect is poor, the resistance strain gauge and the strain adhesive can easily absorb moisture in the air, so that conduction among the strain gauge wire grids or wire grid corrosion is likely to be caused, and meanwhile, the sizes of a substrate, a wire grid, an adhesive layer among the substrates and the like of the adhered strain gauge can also be changed, so that insulation resistance, adhesive strength and rigidity are reduced, and the resistance value of the strain gauge is changed, so that zero drift and poor insulation of the sensor are caused, even the sensor is disabled, therefore, the sensor must be effectively protected and sealed, so that the performances such as moisture resistance, water resistance, enzyme resistance, salt fog resistance and the like, the vibration resistance and shock resistance of the sensor are improved, and the service life of the sensor is further prolonged.
At a certain temperature, the sealing performance of the sensor sealing ring depends on the recovery degree of the sensor sealing ring after stretching and compression deformation at the temperature. With the temperature reduction, the recovery after the stretching and compression deformation is slower and slower, the material becomes hard gradually, and after passing through a leather state, the material becomes hard and brittle like glass finally, namely vitrification, and the sealing ring is cracked and aged at low temperature, so that the sealing failure is caused.
As a high-performance elastomer capable of operating under special environments such as high and low temperature, strong corrosiveness and the like, the fluororubber meets the special requirements that the common elastomer cannot be qualified, and is widely applied to the fields of national defense, industry, life and the like. Meanwhile, along with the opening of the intelligent industry age, high-precision science and technology and novel intelligent materials start to be popularized to industry, a harsh operation environment is challenged to traditional polymer-based functional materials, but as fluororubber, most of polymer-based functional materials with excellent performance cannot be qualified to ultralow temperature environments, and challenges are presented to normal operation of outdoor sensors in extremely cold weather.
Disclosure of Invention
In order to solve the technical problems listed in the background art, the application provides a preparation method of a sealing composite material resistant to low temperature of-50 ℃, which comprises the following specific technical scheme:
1-3 mmol/L of UiO-66-NH 2 Mixing the nanoparticle/ethanol dispersion with an equal volume of 0.1-0.5 mol/L dodecanal/ethanol solution, adding a catalyst, refluxing for 12-24 hours at 68-72 ℃, collecting the product, and cleaning to remove excessive dodecanal to obtain the surface-modified UiO-66-NH2 nanoparticle;
adding 10-20wt% of silane coupling agent A-1100 into 60-80wt% fluororubber/methanol solution, stirring uniformly, then sequentially adding 5-15wt% of bisphenol AF and 5-10wt% of tetrabutylammonium bisulfate, and stirring until completely dissolving; 5-30wt% of the surface modified UiO-66-NH 2 Adding the nano particles into the mixture, performing ultrasonic dispersion for 18-22min, extracting uniform dispersion liquid, and performing volatilizing and drying treatment to obtain the sealing material.
Preferably, the catalyst is glacial acetic acid.
Preferably, the cleaning agent for cleaning is absolute ethyl alcohol.
Preferably, the volatilizing and drying treatment is to pour the dispersion liquid on a horizontal stainless steel plate for film casting, and send the dispersion liquid into a blast oven for drying treatment after the solvent volatilizing is finished.
Further, the process conditions of the drying treatment are that the temperature is raised to 200 ℃ for 2 hours, and then the temperature is kept for 3.5-4.5 hours.
The application also provides a composite material for sealing, which is prepared by adopting the method and can resist the low temperature of minus 50 ℃.
Another aspect of the present application is a sensor in which a housing is sealed by using a film made of the above-described sealing composite material.
Further, the thickness of the film used in the sensor is 5-20 μm.
Compared with the prior art, the application has the following beneficial effects:
the alkyl long chain is adopted to carry out surface modification on the nano particles, so that the dispersibility of the metal organic framework material in the fluororubber solution can be obviously improved, and the compatibility between the metal organic material and the fluororubber matrix can be obviously improved.
The modified metal organic framework particles are used as functional additive materials, so that the bonding strength, mechanical properties and the like of the fluororubber at low temperature can be greatly improved.
Drawings
FIG. 1 is a diagram of UiO-66-NH before and after surface modification in the examples 2 XRD spectrum of the nanoparticle;
FIG. 2 is a schematic illustration of UiO-66-NH before and after surface modification in the examples 2 FTIR spectra of nanoparticles;
FIG. 3 is a diagram of UiO-66-NH before and after surface modification in the examples 2 SEM image of the surface of the nanoparticle;
FIG. 4 is a cross-sectional view of a sealing composite material at a low temperature of-50℃in examples.
Detailed Description
The present application will be described with reference to the drawings and the embodiments thereof, in order to make the objects, technical solutions and advantages of the present application more apparent. It will be apparent that the described embodiments are only some, but not all, embodiments of the application. Based on this embodiment, all other embodiments that a person of ordinary skill in the art would obtain without making any inventive effort are within the scope of the application. 1. UiO-66-NH 2 Is prepared from
Separately weighing zirconium tetrachloride, (ZrCl) 4 2.5mmol,0.56 g) was dissolved in 75ml of N, N-Dimethylformamide (DMF), and after completion of the dissolution by stirring, 2-amino-terephthalic acid (NH) was added 2 After BDC,2.5mmol,0.42 g) was dissolved by stirring, the reaction mixture was charged into a 100ml polytetrafluoroethylene reaction vessel and reacted for 24 hours under heating to 120℃in a forced air drying oven. After naturally cooling to room temperature, the product is centrifuged (10000 r/min,15 min) for separation and collection, and is washed with DMF and methanol for three times respectively to remove impurities in the pore canal of the material. Finally, the obtained solid powder is dried in a vacuum oven at 80 ℃ to obtain the required UiO-66-NH 2 A nanoporous material.
2. Surface modification of UiO-66-NH2
UiO-66-NH after washing with absolute ethanol 2 The nanoparticles were redispersed in absolute ethanol (2 mmol/L), sonicated for l.5 hours, and then centrifuged at a lower speed (3000 rpm) for 10 minutes to remove the larger nanoparticles. Taking supernatant, adding 0.3mol/L dodecanal/absolute ethanol solution prepared in advance in equal volume, dropwise adding a few drops of glacial acetic acid serving as a catalyst, and refluxing at 70 ℃ for 18 hours. After the reaction is finished, centrifugally collecting the obtained product, and repeatedly washing with absolute ethyl alcohol to remove excessive dodecanal, thereby obtaining the surface-modified UiO-66-NH2 nano particles.
FIG. 1 is a schematic representation of the modification of UiO-66-NH by a surface 2 XRD spectrum of nanoparticle modification, uiO-66-NH 2 The XRD spectrum of the material is consistent with that of a standard card, and the XRD spectrum of the material does not change obviously before and after modification, which shows that UiO-66-NH is used in the surface modification process 2 Is not destroyed mainly because of UiO-66-NH 2 internal-NH of structure 2 The functionalization of the groups is limited by the diffusion of the dodecanal molecules, and the modified groups are mainly distributed on the outer surface of the MOF particles, for UiO-66-NH 2 Has no influence on the crystal structure of (a). FIG. 2 is a schematic representation of the modification of UiO-66-NH by surface modification 2 The FTIR spectrogram of the nano particles is modified, the FTIR spectrogram before and after modification has two obvious differences, wherein the absorption peak at 3100cm < -1 > -3500 cm < -l > corresponds to-CH in alkane 2 Symmetrical stretching and asymmetrical stretching of the group, while the absorption peak at 1088cm-l in the light brown region belongs to C-C stretching vibration of straight-chain alkane. The spectrum analysis proves that the dodecanol molecules are successfully grafted on the UiO-66-NH through surface modification 2 Particle surface, modified UiO-66-NH is obtained 2 A particulate material.
3. Preparation of crosslinked composite materials
The fluororubber system takes bisphenol AF as a vulcanizing agent, firstly silane coupling agent A-1100 (15 wt percent by mass) is slowly added into fluororubber/methanol solution with the mass percent of 70wt percent and uniformly stirred, then bisphenol AF (10 wt percent by mass) and tetrabutylammonium bisulfate (5 wt percent by mass) are sequentially added and stirred until the materials are completely dissolved.
Surface-modified UiO-66-NH 2 Nanoparticles (mass fraction 20 wt%) were added thereto and dispersed by ultrasound for 20min to obtain a uniform dispersion. And pouring the mixed system on a horizontal stainless steel plate for casting, and obtaining the rubber compound after the solvent is volatilized. And finally, placing the prepared rubber compound in a blast oven for drying treatment under the condition that the temperature is raised to 200 ℃ for 2 hours, and then preserving heat for 4 hours at 200 ℃ to finally obtain the composite sealing film, wherein the thickness of the film is 15 mu m, and the section of the film is shown in figure 4.
SEM tests were performed to intuitively analyze the morphology and structure of the composite material, and the results are shown in fig. 3. As can be seen from the figure, uiO-66-NH before and after modification 2 The morphology of the particles did not change significantly, however, unmodified UiO-66-NH on the left 2 Compatibility with fluororubber is not good, uiO-66-NH 2 Not all of the polymer is dissolved in the fluororubber. And the right graph is modified with UiO-66-NH 2 Good compatibility with fluororubber, and modified UiO-66-NH 2 All of the particles are dissolved in the fluororubber because the compatibility between the nano metal organic framework particles and the fluororubber matrix can be improved due to the low polarity effect of the long chain alkyl.
By randomly measuring 100 UiO-66-NH in SEM images 2 The average particle size was found to be about 20nm. Such small particle sizes provide the potential for preparing composites with higher compatibility and better performance.
The composite material prepared by the method and the general composite material are subjected to performance test at the temperature of 50 ℃ below zero, and the test results are shown in the following table:
| fluororubber | Composite material of this patent | |
| Dielectric strength (kV/mm) | 28 | 39 |
| Dielectric constant (1.2 MHz) | 2.8 | 3.3 |
| Volume resistivity (Ω cm) | 1.2×10 16 | 1.8×10 16 |
| Linear expansion coefficient [ m/(m.k)] | 1.6×10 -4 | 1.2×10 -4 |
| Tensile Strength | 45.2 | 65.8 |
It can be seen that the composite material prepared by the method has higher dielectric strength, dielectric constant and volume resistivity, lower linear expansion coefficient and higher tensile strength.
The above embodiment completes the description of a composite material for sealing resistant to low temperature of-50 ℃ and a preparation method, and the sensor made of the film as a housing sealing element of the sensor is an embodiment of another technical scheme of the application, namely a sensor.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present application, and the present application is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present application has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (8)
1. The preparation method of the sealing composite material resistant to the low temperature of minus 50 ℃ is characterized by comprising the following steps:
1-3 mmol/L of UiO-66-NH 2 Mixing the nanoparticle/ethanol dispersion with an equal volume of 0.1-0.5 mol/L dodecanal/ethanol solution, adding a catalyst, refluxing for 12-24 hours at 68-72 ℃, collecting the product, and cleaning to remove excessive dodecanal to obtain the surface-modified UiO-66-NH2 nanoparticle;
adding 10-20wt% of silane coupling agent A-1100 into 60-80wt% fluororubber/methanol solution, stirring uniformly, then sequentially adding 5-15wt% of bisphenol AF and 5-10wt% of tetrabutylammonium bisulfate, and stirring until completely dissolving; 5-30wt% of the surface modified UiO-66-NH 2 Adding the nano particles into the mixture, performing ultrasonic dispersion for 18-22min, extracting uniform dispersion liquid, and performing volatilizing and drying treatment to obtain the sealing material.
2. The method for preparing the sealing composite material resistant to low temperature of-50 ℃ as claimed in claim 1, which is characterized in that: the catalyst is glacial acetic acid.
3. A method for preparing a sealing composite material resistant to low temperatures of-50 ℃ as claimed in claim 2, characterized by: the cleaning agent for cleaning is absolute ethyl alcohol.
4. A process for preparing a sealing composite resistant to low temperatures of-50 ℃ as claimed in claim 3, characterized by: and the volatilizing and drying treatment is to pour the dispersion liquid on a horizontal stainless steel plate for film casting, and send the dispersion liquid into a blast oven for drying treatment after the solvent volatilizing is finished.
5. The method for preparing the sealing composite material resistant to low temperature of-50 ℃ as claimed in claim 4, which is characterized in that: the process conditions of the drying treatment are that the temperature is raised to 200 ℃ for 2 hours, and then the temperature is kept for 3.5-4.5 hours.
6. A composite material for sealing resistant to low temperatures of-50 ℃, characterized by being prepared by the preparation method of any one of claims 1 to 5.
7. A sensor characterized in that the housing is sealed by using a film made of the composite material for sealing resistant to low temperature of-50 ℃ as claimed in claim 6.
8. A sensor as claimed in claim 7, wherein: the film thickness of the sealing composite material resistant to the low temperature of minus 50 ℃ is 5-20 mu m.
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| CN202211363270.XA CN115627040B (en) | 2022-11-02 | 2022-11-02 | Composite material resistant to low temperature of-50 ℃ for sealing, preparation method and sensor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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