CN107033325A - A kind of siloxanes and the graphene heat filling particle of isocyanate-crosslinked modification and preparation method thereof - Google Patents
A kind of siloxanes and the graphene heat filling particle of isocyanate-crosslinked modification and preparation method thereof Download PDFInfo
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- CN107033325A CN107033325A CN201710277446.2A CN201710277446A CN107033325A CN 107033325 A CN107033325 A CN 107033325A CN 201710277446 A CN201710277446 A CN 201710277446A CN 107033325 A CN107033325 A CN 107033325A
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/61—Polysiloxanes
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/045—Polysiloxanes containing less than 25 silicon atoms
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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Abstract
A kind of siloxanes and the graphene heat filling particle of isocyanate-crosslinked modification, it is characterised in that eight vinyl polyhedral silsesquioxanes are obtained with vinyl trichlorosilane hydrolytic condensation first；The vinyl of eight vinyl polyhedral silsesquioxanes and the pi-allyl catalytic polymerization of allyl glycidyl ether, obtain epoxy radicals polyhedral silsesquioxane；Again with methyl diphenylene diisocyanate in graphene and the surface graft modification of carbon fiber；Finally with synthesized epoxy radicals polyhedral silsesquioxane and isocyanate groups cross-linking reaction coated graphite alkene and carbon fiber, siloxanes and the graphene heat filling particle of isocyanate-crosslinked modification are obtained.The present invention effectively further increases graphene and carbon fiber thermal performance and fire resistance, and heat filling particle of the present invention has excellent heat conductivility, can fill and prepare heat-conducting resin, thermal conductive adhesive and heat conducting coating etc..
Description
Technical field
The invention belongs to Material Field, and in particular to the graphene heat conduction of a kind of siloxanes and isocyanate-crosslinked modification is filled out
Expect particle and preparation method thereof.
Background technology
Polyhedral oligomeric silsesquioxane (polyhedral oligomeric silsesquioxane, POSS) is a class
Special silsesquioxane, molecule is (RSiO1.5)n, its structure is generally by the inorganic kernels of Si-O-Si of hexahedron cage type and top
8 organic substituent R compositions of point, wherein R can be one or more organo-functional groups, be a kind of molecule truly
Nano hybridization compound.This new hybrid material not only possesses that the toughness of high polymer material, cost be low and well processed
Property, while multiple advantages such as intensity is high, not oxidizable, high temperature resistant, mechanical property are good with inorganic material again.At present, utilize
POSS prepares the focus that novel organic-inorganic hybrid material has become research as nanostructures, and material can be improved by introducing POSS
The heat endurance of material, improves mechanical performance and other physical properties.
Author Tang Wei et al. exists《The synthesis of Epoxy-silsesquioxanes and sign》In one text, passed through with vinyl trichlorosilane
Hydrolytic condensation, first prepares eight vinyl polyhedral silsesquioxanes, is then made with Peracetic acid direct oxidation ethene functional group
Epoxy radicals polyhedral silsesquioxane.The epoxy radicals polyhedral silsesquioxane prepared is adopted this method, it is average each
Polyhedral silsesquioxane can only carry 3-4 epoxy radicals, and the relative position of epoxy radicals is not fixed, and what is obtained is with difference
The polyhedral silsesquioxane of number and diverse location epoxy radicals.And the epoxy radicals that such a method is obtained directly publishes in instalments polyhedron
On the skeleton Si of silsesquioxane, because steric hindrance is larger, reactivity is substantially reduced, and influences its performance.
The content of the invention
It is an object of the invention to provide a kind of siloxanes and the graphene heat filling particle of isocyanate-crosslinked modification
And preparation method thereof.
To achieve these goals, present invention employs following technical scheme：
A kind of siloxanes and the graphene heat filling particle of isocyanate-crosslinked modification, it is characterised in that first with vinyl
Trichlorosilane hydrolytic condensation obtains eight vinyl polyhedral silsesquioxanes；The vinyl of eight vinyl polyhedral silsesquioxanes
With the pi-allyl catalytic polymerization of allyl glycidyl ether, epoxy radicals polyhedral silsesquioxane is obtained；Again with diphenyl
Methane diisocyanate is in graphene and the surface graft modification of carbon fiber；Finally with synthesized epoxy polyhedral sesquialter silicon
Oxygen alkane and isocyanate groups cross-linking reaction coated graphite alkene and carbon fiber, obtain the stone of siloxanes and isocyanate-crosslinked modification
Black alkene heat filling particle.
Described siloxanes and the graphene heat filling particle of isocyanate-crosslinked modification, it is characterised in that it is by such as
Lower step is prepared from：
（1）It is 1 in mass ratio by vinyl trichlorosilane and acetone：10-12 ratio is added in reaction vessel, mechanical agitation
It is well mixed, the deionized water equivalent to acetone parts by weight 35-45%, 40- are slowly added dropwise with 30-40 drops/min speed
45 DEG C of constant-temperature condensations backflow 60-72h, suction filtration, acetone is washed 3-4 times, then uses tetrahydrofuran with methanol volume ratio for 1：2-3 matches somebody with somebody
The mixed solution recrystallization put, 60-65 DEG C of vacuum drying 20-24h, obtains eight vinyl polyhedral silsesquioxanes；
（2）By step（1）Product, allyl glycidyl ether and toluene in mass ratio 1：1.2-1.3：8-10, which adds reaction, to be held
In device, logical nitrogen 30-40min excludes oxygen and is mixed evenly, and adds catalyst 2,2 '-azodiisobutyronitrile and co-catalysis
Agent pentanedione acid chromium, continues to be mixed evenly, and is warming up to 60-70 DEG C, temperature constant magnetic stirring condensing reflux 12-15h, rotation
Turn to be concentrated by evaporation, 60-65 DEG C of vacuum drying obtains epoxy radicals polyhedral silsesquioxane；
（3）Using toluene as solvent, graphene, carbon fiber, methyl diphenylene diisocyanate and dibutyl tin laurate are added,
Temperature is raised after being mixed evenly to 70-80 DEG C, temperature constant magnetic stirring 12-15h；Filter after completion of the reaction, filter cake uses third
Ketone agitator treating 3-4 times, is centrifuged, 60-65 DEG C of vacuum drying 22-24h, obtains isocyanate-modified graphene；Wherein stone
Black alkene, carbon fiber, the mass ratio of methyl diphenylene diisocyanate and dibutyl tin laurate are 1：0.7-0.8：0.9-
1.1：0.05-0.06；
（4）By step（2）Product, step（3）Product with 1：0.8-1 mass ratio is added in toluene solvant, ultrasonic vibration
50-60min, makes its fully dispersed, adds equivalent to step（3）Products weight part 0.05-0.06 times benzoyl peroxide first
Acyl, rise temperature is to 70-80 DEG C, and temperature constant magnetic stirring reaction 22-24h, filtering, filter cake uses acetone agitator treating 3-4 times, from
The heart is separated, 60-65 DEG C of vacuum drying 22-24h, obtains siloxanes and the graphene heat filling of isocyanate-crosslinked modification
Grain.
3rd, according to claims 2 siloxanes and the graphene heat filling particle of isocyanate-crosslinked modification
Preparation method, it is characterised in that described step（3）With（4）In acetone agitator treating 50-60min every time.
Described siloxanes and the preparation method of the graphene heat filling particle of isocyanate-crosslinked modification, its feature exist
In described toluene solvant is the toluene solvant that processing has been pre-dried.
Using above-mentioned technical scheme, beneficial effects of the present invention are：
The present invention obtains eight vinyl polyhedral silsesquioxanes with vinyl trichlorosilane hydrolytic condensation；Eight ethene polyhedrals
The vinyl of silsesquioxane and the pi-allyl catalytic polymerization of allyl glycidyl ether, obtain epoxy polyhedral sesquialter
Siloxanes；Such a method obtains being whole epoxy radicals polyhedral silsesquioxanes, and epoxy radicals and polyhedral silsesquioxane
Skeleton Si between be connected by the flexible chain of certain length, steric hindrance is smaller, and the reactivity of epoxy radicals is higher.The present invention is with two
Methylenebis phenyl isocyanate is in graphene and the surface graft modification of carbon fiber；Again with synthesized epoxy polyhedral sesquialter
Siloxanes and isocyanate groups cross-linking reaction coated graphite alkene and carbon fiber, not only increase epoxy radicals polyhedral silsesquioxane
Grafting rate, and be introduced into huge in the larger Si-O keys of bond energy and Si-C keys and epoxy radicals polyhedral silsesquioxane molecule
Polyhedral structure, further improves the heat conductivility of graphene and carbon fiber.Heat filling particle of the present invention has excellent lead
Hot property, can fill and prepare heat-conducting resin, thermal conductive adhesive and heat conducting coating etc., and graphene film and carbon fiber guiding thermal process
In have obvious cooperative effect, can preferably improve the X, Y, Z-direction of heat-conducting resin, thermal conductive adhesive and heat conducting coating heat conduction
Property.
Embodiment
The siloxanes of the present embodiment and the graphene heat filling particle of isocyanate-crosslinked modification, it is by following steps system
It is standby to form：
（1）It is 1 in mass ratio by vinyl trichlorosilane and acetone：12 ratio is added in reaction vessel, and mechanical agitation makes
It is well mixed, and the deionized water equivalent to acetone parts by weight 35%, 45 DEG C of constant-temperature condensations is slowly added dropwise with 40 drops/min speed
Flowed back 72h, and suction filtration, acetone is washed 3 times, then uses tetrahydrofuran with methanol volume ratio for 1：The mixed solution recrystallization of 2 configurations,
65 DEG C of vacuum drying 20-24h, obtain eight vinyl polyhedral silsesquioxanes；
（2）By step（1）Product, allyl glycidyl ether and toluene in mass ratio 1：1.3：10 add in reaction vessel,
Logical nitrogen 40min excludes oxygen and is mixed evenly, and adds catalyst 2,2 '-azodiisobutyronitrile and co-catalyst acetyl group
Pyruvic acid chromium, continues to be mixed evenly, and is warming up to 70 DEG C, temperature constant magnetic stirring condensing reflux 15h, rotary evaporation concentration, 65
DEG C vacuum drying, obtain epoxy radicals polyhedral silsesquioxane；
（3）Using toluene as solvent, graphene, carbon fiber, methyl diphenylene diisocyanate and dibutyl tin laurate are added,
Temperature is raised after being mixed evenly to 80 DEG C, temperature constant magnetic stirring 15h；Filter after completion of the reaction, filter cake is stirred using acetone
Washing 4 times, is centrifuged, 65 DEG C of vacuum drying 24h, obtains isocyanate-modified graphene；Wherein graphene, carbon fiber, two
The mass ratio of methylenebis phenyl isocyanate and dibutyl tin laurate is 1：0.8：1.1：0.06；
（4）By step（2）Product, step（3）Product with 1：1 mass ratio is added in toluene solvant, ultrasonic vibration
60min, makes its fully dispersed, adds equivalent to step（3）Products weight part 0.06 times benzoyl peroxide, rise temperature
Degree is to 80 DEG C, and temperature constant magnetic stirring reaction 24h, filtering, filter cake uses acetone agitator treating 3 times, centrifuges, and 65 DEG C of vacuum are done
Dry 24h, obtains siloxanes and the graphene heat filling particle of isocyanate-crosslinked modification.
The step of the present embodiment（3）With（4）In acetone agitator treating 60min every time.
The toluene solvant of the present embodiment is the toluene solvant that processing has been pre-dried.
Claims (4)
1. a kind of siloxanes and the graphene heat filling particle of isocyanate-crosslinked modification, it is characterised in that first with ethene
Base trichlorosilane hydrolytic condensation obtains eight vinyl polyhedral silsesquioxanes；The ethene of eight vinyl polyhedral silsesquioxanes
The pi-allyl catalytic polymerization of base and allyl glycidyl ether, obtains epoxy radicals polyhedral silsesquioxane；Again with hexichol
Dicyclohexylmethane diisocyanate is in graphene and the surface graft modification of carbon fiber；Finally with synthesized epoxy polyhedral sesquialter
Siloxanes and isocyanate groups cross-linking reaction coated graphite alkene and carbon fiber, obtain siloxanes and isocyanate-crosslinked modification
Graphene heat filling particle.
2. the graphene heat filling particle of the siloxanes and isocyanate-crosslinked modification according to claims 1, it is special
Levy and be, it is prepared from by following steps：
（1）It is 1 in mass ratio by vinyl trichlorosilane and acetone：10-12 ratio is added in reaction vessel, mechanical agitation
It is well mixed, the deionized water equivalent to acetone parts by weight 35-45%, 40- are slowly added dropwise with 30-40 drops/min speed
45 DEG C of constant-temperature condensations backflow 60-72h, suction filtration, acetone is washed 3-4 times, then uses tetrahydrofuran with methanol volume ratio for 1：2-3 matches somebody with somebody
The mixed solution recrystallization put, 60-65 DEG C of vacuum drying 20-24h, obtains eight vinyl polyhedral silsesquioxanes；
（2）By step（1）Product, allyl glycidyl ether and toluene in mass ratio 1：1.2-1.3：8-10, which adds reaction, to be held
In device, logical nitrogen 30-40min excludes oxygen and is mixed evenly, and adds catalyst 2,2 '-azodiisobutyronitrile and co-catalysis
Agent pentanedione acid chromium, continues to be mixed evenly, and is warming up to 60-70 DEG C, temperature constant magnetic stirring condensing reflux 12-15h, rotation
Turn to be concentrated by evaporation, 60-65 DEG C of vacuum drying obtains epoxy radicals polyhedral silsesquioxane；
（3）Using toluene as solvent, graphene, carbon fiber, methyl diphenylene diisocyanate and dibutyl tin laurate are added,
Temperature is raised after being mixed evenly to 70-80 DEG C, temperature constant magnetic stirring 12-15h；Filter after completion of the reaction, filter cake uses third
Ketone agitator treating 3-4 times, is centrifuged, 60-65 DEG C of vacuum drying 22-24h, obtains isocyanate-modified graphene；Wherein stone
Black alkene, carbon fiber, the mass ratio of methyl diphenylene diisocyanate and dibutyl tin laurate are 1：0.7-0.8：0.9-
1.1：0.05-0.06；
（4）By step（2）Product, step（3）Product with 1：0.8-1 mass ratio is added in toluene solvant, ultrasonic vibration
50-60min, makes its fully dispersed, adds equivalent to step（3）Products weight part 0.05-0.06 times benzoyl peroxide first
Acyl, rise temperature is to 70-80 DEG C, and temperature constant magnetic stirring reaction 22-24h, filtering, filter cake uses acetone agitator treating 3-4 times, from
The heart is separated, 60-65 DEG C of vacuum drying 22-24h, obtains siloxanes and the graphene heat filling of isocyanate-crosslinked modification
Grain.
3. the preparation of the graphene heat filling particle of siloxanes and isocyanate-crosslinked modification according to claims 2
Method, it is characterised in that described step（3）With（4）In acetone agitator treating 50-60min every time.
4. the preparation of the graphene heat filling particle of siloxanes and isocyanate-crosslinked modification according to claims 2
Method, it is characterised in that described toluene solvant is the toluene solvant that processing has been pre-dried.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108948720A (en) * | 2018-06-25 | 2018-12-07 | 董小琳 | A kind of preparation method of TPU ventilated membrane |
| CN110330338A (en) * | 2019-05-17 | 2019-10-15 | 慈溪埃弗龙密封件有限公司 | A kind of long-life tooth plate enhancing high-strength graphite gasket and preparation method thereof |
| CN114426674A (en) * | 2021-12-10 | 2022-05-03 | 哈尔滨理工大学 | Preparation method and application of thermosetting resin-based toughened high-thermal-conductivity filler |
| CN114773861A (en) * | 2022-05-24 | 2022-07-22 | 昆山力普电子橡胶有限公司 | Silica gel protective sleeve for mobile storage hard disk and preparation method thereof |
| CN118240454A (en) * | 2024-05-06 | 2024-06-25 | 醴陵市精陶瓷业有限公司 | Special anti-corrosion coating for ceramics and preparation method thereof |
| CN118480287A (en) * | 2024-07-16 | 2024-08-13 | 成都虹润制漆有限公司 | Polyvinyl chloride fluorine-containing fluorescent primer and preparation method thereof |
Citations (1)
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| CN101503420A (en) * | 2009-03-20 | 2009-08-12 | 北京化工大学 | Octa-epoxy cage type sesquialter siloxane and preparation thereof |
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- 2017-04-25 CN CN201710277446.2A patent/CN107033325A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101503420A (en) * | 2009-03-20 | 2009-08-12 | 北京化工大学 | Octa-epoxy cage type sesquialter siloxane and preparation thereof |
Non-Patent Citations (1)
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| GUANGSHUN WU: "Internal properties and thermo-oxidative stability of carbon fiber reinforced methylphenylsilicone resin composites modified with polyhedral oligomeric silsesquioxanes in the interphase", 《RSC ADVANCES》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108948720A (en) * | 2018-06-25 | 2018-12-07 | 董小琳 | A kind of preparation method of TPU ventilated membrane |
| CN110330338A (en) * | 2019-05-17 | 2019-10-15 | 慈溪埃弗龙密封件有限公司 | A kind of long-life tooth plate enhancing high-strength graphite gasket and preparation method thereof |
| CN114426674A (en) * | 2021-12-10 | 2022-05-03 | 哈尔滨理工大学 | Preparation method and application of thermosetting resin-based toughened high-thermal-conductivity filler |
| CN114426674B (en) * | 2021-12-10 | 2023-02-24 | 哈尔滨理工大学 | Preparation method and application of thermosetting resin-based toughened high-thermal-conductivity filler |
| CN114773861A (en) * | 2022-05-24 | 2022-07-22 | 昆山力普电子橡胶有限公司 | Silica gel protective sleeve for mobile storage hard disk and preparation method thereof |
| CN114773861B (en) * | 2022-05-24 | 2022-12-27 | 昆山力普电子橡胶有限公司 | Silica gel protective sleeve for mobile storage hard disk and preparation method thereof |
| CN118240454A (en) * | 2024-05-06 | 2024-06-25 | 醴陵市精陶瓷业有限公司 | Special anti-corrosion coating for ceramics and preparation method thereof |
| CN118240454B (en) * | 2024-05-06 | 2024-09-20 | 醴陵市精陶瓷业有限公司 | Special anti-corrosion coating for ceramics and preparation method thereof |
| CN118480287A (en) * | 2024-07-16 | 2024-08-13 | 成都虹润制漆有限公司 | Polyvinyl chloride fluorine-containing fluorescent primer and preparation method thereof |
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