CN116814005A - High-temperature-resistant silicon carbide aerogel master batch and preparation method thereof - Google Patents
High-temperature-resistant silicon carbide aerogel master batch and preparation method thereof Download PDFInfo
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- CN116814005A CN116814005A CN202310802646.0A CN202310802646A CN116814005A CN 116814005 A CN116814005 A CN 116814005A CN 202310802646 A CN202310802646 A CN 202310802646A CN 116814005 A CN116814005 A CN 116814005A
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- silicon carbide
- carbide aerogel
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- aerogel
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- 239000004964 aerogel Substances 0.000 title claims abstract description 92
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 82
- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 239000000088 plastic resin Substances 0.000 claims abstract description 40
- 239000002131 composite material Substances 0.000 claims abstract description 31
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims abstract description 12
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims abstract description 11
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000012975 dibutyltin dilaurate Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 22
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- -1 polyethylene Polymers 0.000 claims description 17
- 230000032683 aging Effects 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 239000003607 modifier Substances 0.000 claims description 11
- 239000004743 Polypropylene Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 7
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 7
- 239000003381 stabilizer Substances 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 229920000515 polycarbonate Polymers 0.000 claims description 2
- 239000004417 polycarbonate Substances 0.000 claims description 2
- 229920000379 polypropylene carbonate Polymers 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 238000009736 wetting Methods 0.000 abstract description 4
- 239000012760 heat stabilizer Substances 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 238000006068 polycondensation reaction Methods 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 3
- 230000003075 superhydrophobic effect Effects 0.000 abstract description 3
- 150000001722 carbon compounds Chemical class 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 239000004033 plastic Substances 0.000 description 11
- 229920003023 plastic Polymers 0.000 description 11
- 239000007789 gas Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 229920000049 Carbon (fiber) Polymers 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 6
- 239000004917 carbon fiber Substances 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 229920001155 polypropylene Polymers 0.000 description 6
- 239000004677 Nylon Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000002070 nanowire Substances 0.000 description 4
- 229920001778 nylon Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005844 autocatalytic reaction Methods 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000010931 ester hydrolysis Methods 0.000 description 1
- BNCWXABAKRSFNA-UHFFFAOYSA-N ethenyl trimethyl silicate Chemical compound CO[Si](OC)(OC)OC=C BNCWXABAKRSFNA-UHFFFAOYSA-N 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- NDJGGFVLWCNXSH-UHFFFAOYSA-N hydroxy(trimethoxy)silane Chemical compound CO[Si](O)(OC)OC NDJGGFVLWCNXSH-UHFFFAOYSA-N 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/977—Preparation from organic compounds containing silicon
-
- 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
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/56—Organo-metallic compounds, i.e. organic compounds containing a metal-to-carbon bond
- C08K5/57—Organo-tin compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Polymers & Plastics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a high-temperature-resistant silicon carbide aerogel master batch and a preparation method thereof, and relates to the technical field of preparation of carbon compounds from silicon dioxide. The silicon carbide aerogel master batch has high temperature resistance and superhydrophobicity, has better processability, and is convenient for use of the silicon carbide aerogel in practical application. Compared with the prior art, the invention takes vinyl trimethoxy silane and trimethoxy silane as composite precursors, prepares silicon carbide aerogel with heat resistance and thermal stability through hydrolysis, polycondensation and carbothermal reduction, and then adds the silicon carbide aerogel into plastic resin to obtain composite plastic resin for improving the high temperature resistance of the plastic resin; further carrying out surface modification, and preventing water from wetting the surface of the material when the low-surface-energy material has a micro-rough structure, so that a super-hydrophobic state is formed; and finally, adding a small amount of dibutyl tin dilaurate and an organotin heat stabilizer, mixing and granulating to obtain the high-temperature-resistant silicon carbide aerogel master batch.
Description
Technical Field
The invention relates to the technical field of preparing carbon compounds from silicon dioxide, in particular to a high-temperature-resistant silicon carbide aerogel master batch and a preparation method thereof.
Background
The aerogel has the characteristics of low density, large specific surface area, good thermal stability, excellent mechanical strength, high porosity, adjustable porous structure and pore size, and the like, and the aerogel powder has extremely small particles, extremely low density and extremely easy generation of powder floating problem, increases the use loss and difficulty, and can be made into master batches to facilitate the use of the aerogel in practical application, improve the physical strength and durability, and make the aerogel more convenient to carry, store and use. Silicon carbide aerogel is a state of silicon carbide, is a gel-like substance with high porosity and composed of silicon carbide nano particles, has low thermal expansion coefficient, high mechanical strength, good thermal shock resistance and high-temperature stability, is not easy to thermally decompose or oxidize in a high-temperature environment, and has very wide application prospects in the fields of heat, optics, acoustics, microelectronics, catalysis, aerospace, energy-saving buildings and the like.
The research and application of aerogels in plastics is still in the ongoing phase. In the aspect of mechanical properties of plastics, the aerogel is added into the plastics, so that the performances of the plastics in the aspects of strength, hardness, toughness, wear resistance and the like can be effectively improved; in the aspect of heat conduction performance and heat insulation performance of plastics, for example, aerogel is used for manufacturing heat insulation, heat insulation sponge and the like of heat insulation boxes, refrigerating boxes and freezing boxes, so that the heat insulation and heat insulation performance is improved; in terms of flame retardant properties of plastics, for example, the addition of aerogel to polyimide can significantly improve its flame retardant properties; the method also has the advantages of being widely focused and researched in the field of high-temperature materials, being applicable to preparing high-temperature heat insulation materials and being capable of remarkably improving the temperature resistance and the heat resistance of plastic resin in high-temperature environments. The use of aerogels in plastics is continually evolving and expanding, and there are many potential fields of application and research directions awaiting further exploration and development to meet the needs of different fields.
CN110305340a discloses an aerogel composite plastic master batch, and a preparation method and application thereof, the preparation method comprises the following steps: (1) Uniformly mixing the aerogel slurry with the aqueous resin emulsion to obtain an aerogel aqueous resin mixed solution; (2) Granulating the aerogel aqueous mixed solution obtained in the step (1) in a spray drying mode, and drying to obtain heat-insulating master batch; (3) And (3) mixing and granulating the resin master batch and the heat-insulating master batch obtained in the step (2) to obtain the aerogel composite plastic master batch.
CN106046766a discloses a high-strength modified nylon material for automobile plastics, which is prepared from the following raw materials in parts by weight: 100-120 parts of nylon resin, 4-6 parts of silicon carbide micro powder, 16-20 parts of polyurethane-graphene composite light foam filler, 0.5-1.5 parts of coupling agent, 1-3 parts of polyethylene wax, 0.5-1.5 parts of antioxidant, 2-4 parts of nano bamboo fiber and 1-2 parts of calcium sulfate whisker. The modified nylon material prepared by the invention has excellent physical properties and high temperature resistance, and meanwhile, the density of the nylon material is not obviously improved, so that the weight is reduced. The solutions reported in these patent documents above, in which aerogel is added as an additive to plastics, do not fully exploit the characteristics of aerogel and often do not solve various problems at the same time. In practical use, because aerogel particles are extremely small and have extremely low density, the use loss and difficulty are increased, and the aerogel performance is affected by different aerogel synthesis processes.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention aims to solve the technical problem of preparing silicon carbide aerogel, adding the silicon carbide aerogel into plastic resin to obtain a master batch with high temperature resistance and superhydrophobicity, having better processability and being convenient for use of the silicon carbide aerogel in practical application.
In order to achieve the above purpose, the invention provides a high-temperature-resistant silicon carbide aerogel master batch and a preparation method thereof. The preparation method of the silicon carbide aerogel master batch comprises the following steps:
(1) Adding vinyl trimethoxy silane, trimethoxy silane and a base catalyst into an ethanol water solution, stirring, and drying at 90-100 ℃ to obtain mixed gel for later use;
(2) Heating the mixed gel to 1500-1600 ℃ for reaction under the conditions of inert gas, vacuum pressure and heating rate, naturally cooling to room temperature, placing, and finally heating in a device at 400-600 ℃ for 2-4 hours to obtain silicon carbide aerogel;
(3) Adding silicon carbide aerogel into plastic resin, stirring, ageing at room temperature, adding absolute ethyl alcohol, ageing at 60-80 ℃, adding modifier, stirring and drying to obtain composite plastic resin at room temperature;
(4) Stirring the composite plastic resin and the stabilizer at room temperature, and granulating by using a granulator to obtain the high-temperature-resistant silicon carbide aerogel master batch.
Specifically, the preparation method of the high-temperature-resistant silicon carbide aerogel master batch comprises the following operation steps in parts by weight:
(1) Adding 3-5 parts of vinyl trimethoxy silane, 1-1.5 parts of trimethoxy silane and 0.05-1 part of base catalyst into 10-12 parts of ethanol water solution, stirring for 6-10 hours at 60-80 ℃, and drying for 5-6 hours at 90-100 ℃ to obtain mixed gel for later use;
(2) Under the conditions of inert gas, 0.1-0.2MPa of pressure and 5-10 ℃/min of heating rate, heating the mixed gel to 1500-1600 ℃ for reaction for 1-3 hours, naturally cooling to room temperature, then placing for 2-4 hours, and finally placing in a device at 400-600 ℃ for heating for 2-4 hours to obtain silicon carbide aerogel;
(3) Adding 3-5 parts of silicon carbide aerogel into 40-60 parts of plastic resin, stirring for 1-2 hours, aging for 40-48 hours at room temperature, adding 80-120 parts of absolute ethyl alcohol, aging for 5-6 hours at 60-80 ℃, adding 2-3 parts of modifier, stirring for 6-8 hours at 90-100 ℃, and drying for 2-4 hours at 90-100 ℃ to obtain composite plastic resin;
(4) Stirring 40-60 parts of composite plastic resin and 0.5-2 parts of stabilizer for 10-30 minutes at room temperature, and granulating by using a granulator to obtain the high-temperature-resistant silicon carbide aerogel master batch.
The ethanol aqueous solution in the step (1) is 70-75wt.% ethanol aqueous solution.
The alkali catalyst in the step (1) is one of potassium hydroxide, sodium hydroxide and ammonia water; preferably potassium hydroxide.
The inert gas in the step (2) is any one of argon and nitrogen.
The plastic resin in the step (3) is any one of polyethylene, polypropylene and polycarbonate; preferably polypropylene.
The modifier in the step (3) is any one of trimethylchlorosilane, methyltrimethoxysilane, methyltriethoxysilane, n-octyltriethoxysilane and polydimethylsiloxane; preferably polydimethylsiloxane.
The stabilizer in the step (4) is dibutyl tin dilaurate.
The granulation in the step (4) adopts a conventional extrusion process in the field; the temperature is not specifically described in the examples.
The vinyl trimethoxy silane has strong hydrolyzability, and is added into water to generate ester hydrolysis reaction, and the molecule of the vinyl trimethoxy silane is broken into vinyl trimethoxy silanol and formaldehyde after hydrolysis; after trimethoxysilane is hydrolyzed, the molecules of trimethoxy silane are broken into trimethoxy silanol and formaldehyde; the silanol in the hydrolysate is subjected to self-catalysis and polycondensation reaction to form a macromolecular polymer containing three elements of Si, C and O and siloxane bonds; the siloxane bond forms a firmer chemical bond between the organic matters and the inorganic matters so as to connect the carbon fiber with the siloxane and disperse the carbon fiber in the gel liquid, and the gel liquid is dried so that gas replaces liquid phase in the gel to form the solid mixed gel with the nano-porous three-dimensional network structure.
The mixed gel is subjected to carbothermal reduction to enable siloxane gel attached to the surface of the carbon fiber to be changed into silicon carbide, the silicon carbide is decomposed and releases gaseous silicon carbide and carbon monoxide along with the rising of temperature, atomic nuclei of the silicon carbide and the carbon monoxide react with each other through continuous gas, silicon carbide nano wires are formed and grow into the silicon carbide nano wires in narrow holes of the porous silicon carbide, and the silicon carbide nano wires are naturally cooled to room temperature and then placed for a period of time until a large number of intertwined silicon carbide nano wires are formed on the surface of the carbon fiber; finally, calcining to remove the free carbon fiber, thus obtaining the silicon carbide aerogel with heat resistance and thermal stability.
The plastic resin generally has good mechanical strength and physical properties, but has limited high temperature resistance, and the silicon carbide aerogel with good heat resistance and high thermal stability is added into the plastic resin to obtain the composite plastic resin for improving the high temperature resistance of the plastic resin. Further carrying out surface modification on the composite plastic resin by an environmental pressure drying method, wherein silicon carbide composite aerogel and a modifier form a three-dimensional network structure through crosslinking of silica bonds, so that the surface polarity of the composite plastic resin is reduced, and the surface energy is reduced; and finally, adding a small amount of dibutyl tin dilaurate and an organotin heat stabilizer, mixing and granulating to obtain the high-temperature-resistant silicon carbide aerogel master batch.
The invention has the beneficial effects that:
1. compared with the prior art, the invention takes vinyl trimethoxy silane and trimethoxy silane as composite precursors, and uses silanol in the hydrolysis product of the composite precursors to perform polycondensation reaction in an autocatalysis way to form solid mixed gel with a nano porous three-dimensional network structure; performing carbothermal reduction on the mixed gel to obtain a silicon carbide nanowire; finally, calcining to remove the free carbon fiber, thus obtaining the silicon carbide aerogel with heat resistance and thermal stability.
2. Compared with the prior art, the silicon carbide aerogel with good heat resistance and high thermal stability is added into the plastic resin to obtain the composite plastic resin, so as to improve the high temperature resistance of the plastic resin; further, the surface of the composite plastic resin is modified by an environmental pressure drying method, so that the surface polarity of the composite plastic resin is reduced, and when the low-surface-energy material has a micro-rough structure, the wetting of water to the surface of the material is hindered, so that a super-hydrophobic state is formed; and finally, adding a small amount of dibutyl tin dilaurate and an organotin heat stabilizer, mixing and granulating to obtain the high-temperature-resistant silicon carbide aerogel master batch.
3. According to the invention, the silicon carbide aerogel master batch is prepared by adding the silicon carbide aerogel into the plastic resin, so that the silicon carbide aerogel master batch has better processability, is convenient for use of the silicon carbide aerogel in practical application, and can be produced in a large scale.
Detailed Description
The polypropylene used in the examples was purchased from Dongguan division, hainan energy Co., ltd., in Guangdong under the trade designation 320.
The polydimethylsiloxane used in the examples was identified as basf, SI2210, and 99wt.% active ingredient.
Example 1
The preparation method of the high-temperature-resistant silicon carbide aerogel master batch comprises the following operation steps:
(1) 30g of vinyltrimethoxysilane, 10g of trimethoxysilane and 4g of potassium hydroxide are added into 120g of 75wt.% ethanol water solution, stirred for 8 hours at 70 ℃, and dried for 5 hours at 95 ℃ to obtain mixed gel for later use;
(2) Under the conditions of argon gas, 0.1MPa of pressure and 5 ℃/min of heating rate, heating the mixed gel to 1500 ℃ for reaction for 2 hours, naturally cooling to room temperature, standing for 2 hours, and finally heating in a 500 ℃ device for 3 hours to obtain silicon carbide aerogel;
(3) Adding 35g of silicon carbide aerogel into 450g of polypropylene, stirring for 1 hour, aging for 48 hours at room temperature, adding 1000g of absolute ethyl alcohol, aging for 5 hours at 65 ℃, and drying for 2 hours at 95 ℃ to obtain composite plastic resin;
(4) 460g of composite plastic resin and 15g of dibutyltin dilaurate are stirred for 30 minutes at room temperature, and a granulator is used for granulating to obtain the high-temperature-resistant silicon carbide aerogel master batch, wherein the particle size of the master batch is 3mm.
Example 2
The preparation method of the high-temperature-resistant silicon carbide aerogel master batch comprises the following operation steps:
(1) 30g of vinyltrimethoxysilane, 10g of trimethoxysilane and 4g of potassium hydroxide are added into 120g of 75wt.% ethanol water solution, stirred for 8 hours at 70 ℃, and dried for 5 hours at 95 ℃ to obtain mixed gel for later use;
(2) Under the conditions of argon gas, 0.1MPa of pressure and 5 ℃/min of heating rate, heating the mixed gel to 1500 ℃ for reaction for 2 hours, naturally cooling to room temperature, standing for 2 hours, and finally heating in a 500 ℃ device for 3 hours to obtain silicon carbide aerogel;
(3) Adding 35g of silicon carbide aerogel into 450g of polypropylene, stirring for 1 hour, aging for 48 hours at room temperature, adding 1000g of absolute ethyl alcohol, aging for 5 hours at 65 ℃, adding 14g of methyltrimethoxysilane, stirring for 6 hours at 95 ℃, and drying for 2 hours at 95 ℃ to obtain composite plastic resin;
(4) 460g of composite plastic resin and 15g of dibutyltin dilaurate are stirred for 30 minutes at room temperature, and a granulator is used for granulating to obtain the high-temperature-resistant silicon carbide aerogel master batch, wherein the particle size of the master batch is 3mm.
Example 3
The preparation method of the high-temperature-resistant silicon carbide aerogel master batch comprises the following operation steps:
(1) 30g of vinyltrimethoxysilane, 10g of trimethoxysilane and 4g of potassium hydroxide are added into 120g of 75wt.% ethanol water solution, stirred for 8 hours at 70 ℃, and dried for 5 hours at 95 ℃ to obtain mixed gel for later use;
(2) Under the conditions of argon gas, 0.1MPa of pressure and 5 ℃/min of heating rate, heating the mixed gel to 1500 ℃ for reaction for 2 hours, naturally cooling to room temperature, standing for 2 hours, and finally heating in a 500 ℃ device for 3 hours to obtain silicon carbide aerogel;
(3) Adding 35g of silicon carbide aerogel into 450g of polypropylene, stirring for 1 hour, aging for 48 hours at room temperature, adding 1000g of absolute ethyl alcohol, aging for 5 hours at 65 ℃, adding 14g of n-octyl triethoxysilane, stirring for 6 hours at 95 ℃, and drying for 2 hours at 95 ℃ to obtain composite plastic resin;
(4) 460g of composite plastic resin and 15g of dibutyltin dilaurate are stirred for 30 minutes at room temperature, and a granulator is used for granulating to obtain the high-temperature-resistant silicon carbide aerogel master batch, wherein the particle size of the master batch is 3mm.
Example 4
The preparation method of the high-temperature-resistant silicon carbide aerogel master batch comprises the following operation steps:
(1) 30g of vinyltrimethoxysilane, 10g of trimethoxysilane and 4g of potassium hydroxide are added into 120g of 75wt.% ethanol water solution, stirred for 8 hours at 70 ℃, and dried for 5 hours at 95 ℃ to obtain mixed gel for later use;
(2) Under the conditions of argon gas, 0.1MPa of pressure and 5 ℃/min of heating rate, heating the mixed gel to 1500 ℃ for reaction for 2 hours, naturally cooling to room temperature, standing for 2 hours, and finally heating in a 500 ℃ device for 3 hours to obtain silicon carbide aerogel;
(3) Adding 35g of silicon carbide aerogel into 450g of polypropylene, stirring for 1 hour, aging for 48 hours at room temperature, adding 1000g of absolute ethyl alcohol, aging for 5 hours at 65 ℃, adding 14g of polydimethylsiloxane, stirring for 6 hours at 95 ℃, and drying for 2 hours at 95 ℃ to obtain composite plastic resin;
(4) 460g of composite plastic resin and 15g of dibutyltin dilaurate are stirred for 30 minutes at room temperature, and a granulator is used for granulating to obtain the high-temperature-resistant silicon carbide aerogel master batch, wherein the particle size of the master batch is 3mm.
Test example 1
High temperature resistance weightlessness test
The silicon carbide aerogel master batch obtained by the preparation method of the examples 1-4 is used as a test sample, a TG209F1 thermogravimetric analyzer of German anti-relaxation company is used for testing the thermal decomposition temperature of the material, the gas atmosphere is a mixed gas of argon and oxygen in a ratio of 2:1, the test temperature range is 200 ℃, 220 ℃, 240 ℃, 260 ℃, 280 ℃, 300 ℃, the temperature rising rate is 20 ℃/min, and the residual mass ratio of the sample under different test temperatures in the temperature rising process is recorded. Four test groups, three parallel test groups were set, each group had an initial mass of 100mg, the test data were averaged, and the test results are shown in Table 1.
As can be seen from the comparison of test example 1, the unmodified silicon carbide aerogel of example 1 has the highest decomposition rate and the largest weight loss rate, and the residual mass of the masterbatch at 300 ℃ is lower than 50%; the residual mass of the master batch of the silicon carbide aerogel obtained in the examples 2-4 is still more than 60% at 300 ℃, and the difference is that the modifier is different; wherein the modification effect of the polydimethylsiloxane modifier used in the test of example 4 is best, the obtained silicon carbide aerogel master batch has best high temperature resistance and thermal stability, and the residual mass of the master batch is still more than 90 percent at 300 ℃.
Test example 2
Hydrophobicity test
The silicon carbide aerogel master batch obtained by the preparation method of examples 1-4 is used as a test sample, four groups of tests are performed, three groups of parallel tests are arranged in each group, and the test data are averaged.
During testing, 1g of silicon carbide aerogel master batch obtained by the preparation method of examples 1-4 is pressed by a simple tabletting machine and is placed on the surface of a glass sample with the length of 50mm and the width of 50mm and 2 mm; the glass samples of examples 1-4 were placed on a sample stage; a 5 μl volume of deionized water was dropped onto the surface of the glass samples of examples 1-4, and the magnification of the drops was adjusted to a size of about 2/3 of the visible range; measuring a static water drop contact angle of a coating surface taking silicon carbide aerogel master batch as a raw material by using a contact angle measuring instrument; finally, the water drop contact angle value of the surface of the sample sheet is obtained by the tan method through the software of the testing instrument. The hydrophobicity test results are shown in table 2.
The contact angle is calculated as follows:
wherein:
-contact angle in °;
h-water droplet height;
d-contact line length.
The hydrophilicity or the hydrophobicity of the surface can be judged by the wetting behavior of the surface and the liquid drop, and the contact angleThe wettability of a liquid on a solid surface can be quantitatively described when 0 ° < +.>A wet state of < 90 °;90 DEG </i>Less than 180 ° is non-wetting; />> 150 ° is a superhydrophobic surface; />=0° is fully wet; />=180° is incompletely wetted.
As can be seen from the comparison of test example 2, the unmodified silicon carbide aerogel master batch in example 1, too high a surface energy is detrimental to improving the hydrophobic properties of the material. Examples 2-4 all had good hydrophobicity, except for the modifier, which was the most excellent in the modification of the polydimethylsiloxane modifier tested in example 4, and the resulting silicon carbide aerogel master batch had the best hydrophobicity.
Claims (10)
1. The high-temperature-resistant silicon carbide aerogel master batch is characterized by comprising the following components: composite plastic resin and stabilizer.
2. The high temperature resistant silicon carbide aerogel masterbatch according to claim 1, characterized by comprising the following components in parts by weight: 40-60 parts of composite plastic resin and 0.5-2 parts of stabilizer.
3. The high temperature resistant silicon carbide aerogel master batch of claim 2, wherein the composite plastic resin is composed of the following components: silicon carbide aerogel, plastic resin, a modifier and absolute ethyl alcohol.
4. The high temperature resistant silicon carbide aerogel master batch of claim 3, wherein the silicon carbide aerogel is comprised of the following components: vinyl trimethoxy silane, base catalyst, aqueous ethanol solution.
5. The high temperature resistant silicon carbide aerogel master batch of claim 4, wherein the base catalyst is any one of potassium hydroxide, sodium hydroxide, and ammonia water.
6. The high temperature resistant silicon carbide aerogel master batch of claim 3, wherein the plastic resin is any one of polyethylene, polypropylene and polycarbonate.
7. The high temperature resistant silicon carbide aerogel master batch of claim 3, wherein the modifier is any one of trimethylchlorosilane, methyltrimethoxysilane, methyltriethoxysilane, n-octyltriethoxysilane, and polydimethylsiloxane.
8. The high temperature resistant silicon carbide aerogel masterbatch according to claim 1 wherein said stabilizer is dibutyltin dilaurate.
9. The method for preparing a high temperature resistant silicon carbide aerogel masterbatch according to any one of claims 1-8 comprising the steps of:
(1) Adding vinyl trimethoxy silane, trimethoxy silane and a base catalyst into an ethanol water solution, stirring, and drying at 90-100 ℃ to obtain mixed gel for later use;
(2) Heating the mixed gel to 1500-1600 ℃ for reaction under the conditions of inert gas, vacuum pressure and heating rate, naturally cooling to room temperature, placing, and finally heating in a device at 400-600 ℃ for 2-4 hours to obtain silicon carbide aerogel;
(3) Adding silicon carbide aerogel into plastic resin, stirring, ageing at room temperature, adding absolute ethyl alcohol, ageing at 60-80 ℃, adding modifier, stirring and drying to obtain composite plastic resin at room temperature;
(4) Stirring the composite plastic resin and the stabilizer at room temperature, and granulating by using a granulator to obtain the high-temperature-resistant silicon carbide aerogel master batch.
10. The method for preparing high temperature resistant silicon carbide aerogel master batch according to claim 9, wherein the heating rate in the step (2) is 5-10 ℃/min.
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