CN106281205A - A kind of comprehensive silicon ketone seal gum of high-gas resistance performance and preparation method thereof - Google Patents
A kind of comprehensive silicon ketone seal gum of high-gas resistance performance and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to field of material technology, specifically disclose the comprehensive silicon ketone seal gum of a kind of high-gas resistance performance, including component A and B component;Described component A includes that mass fraction is: 100 parts of basic glue, 0.01 10 parts of nano material powder body, 40 100 parts of fillers, 5 10 parts of silane couplers;Described B component includes that mass fraction is: 10 20 parts of cross-linking agent, 10 30 parts of plasticizers, 0.1 2 parts of catalyst;Component A and B component weight ratio are 10~13:1;Described nano material powder body includes the one in graphene oxide, modified graphene or the modified white graphite alkene of 5 10 layers.The present invention adds that graphene oxide, modified graphene or the modified white graphite alkene of 5 10 layers can increase substantially the barrier property of silicone sealant and mechanical strength on a small quantity and other performances are unaffected;The silicone sealant of the present invention seals for two roads of double glazing, with together with to seal the butyl rubber compatibility used good, and there is good processing characteristics, environmentally friendly.
Description
Technical field
The present invention relates to field of material technology, be specifically related to comprehensive silicon ketone seal gum and the preparation thereof of a kind of high-gas resistance performance
Method.
Background technology
Along with country is to the attention of energy-saving material and the enhancing of people's environmental consciousness, double glazing is at building materials and ornaments, energy-conservation
The application of the aspect such as vehicle and refrigeration plant is increasingly extensive, and the requirement to its quality is more and more higher simultaneously.Double glazing has
Good air-tightness, watertightness and good heat-insulation and heat-preservation function, especially Low-E double glazing is by double glazing, Low emissivity
Silver-plated film, noble gas combine, and have the dual characteristics of Low-E glass and double glazing, possess good daylighting, with
Time there is no " light pollution ", very prominent effect is respectively provided with for heat insulation and anti-ultraviolet, is green truly, joint
Energy, environmental protection glass building material.
Hollow glass heat insulating, sound insulation, frost protection are to be realized by its internal one layer of sealing, dry hollow layer.Mesh
The subject matter of front China double glazing is that quality there is no guarantee that, the life-span is short, and after using 1 year or several years, knot occurs in double glazing
Dew or frosting, cause double glazing to lose efficacy.The double glazing of more than 90% lost efficacy and unsuccessfully caused by sealing, and seals and unsuccessfully leads
If owing to design of Sealing Structure is unreasonable, sealant sealing is the most thorough or aging causes.Therefore, sealing structure base is being determined
On plinth, the service life to extending double glazing that selects of fluid sealant has important effect.
Double glazing mainly uses double sealing method at present: seals to carry together and resists the closeest of vapor permeation
Envelope, currently mainly uses hot melt butyl sealant;Two road fluid sealants are possessing in good glassy bond performance basis, it is necessary to
Having good mechanical performance, main material has three kinds: TR sealant, silicone adhesive and polyurethane adhesive.Although TR sealant has preferably
Structural strength and high and low temperature resistance, and air-tightness is better than silicone adhesive, but its ultra-violet resistance can be poor, for a long time under sunlight irradiates
The most aging, affect service life.Polyurethane adhesive properties is the most moderate, but complicated construction technique, the humiture to construction
Require higher, therefore apply less at present in double glazing.Silicone sealant not only has good weatherability and structure is steady
Qualitative, and will not decompose under long-term ultraviolet irradiates, remain to keep under the repeated action of high temperature or low temperature and steam
Excellent caking property and intensity, and fabulous elastic restoration ratio.But the shortcoming of existing silicone sealant product is that gas oozes
Coefficient relatively big (about 10~15g/m thoroughly2D), such gas readily penetrates through sealant layer to the infiltration expansion of double glazing hollow layer
Dissipating, time one long there will be, condenses or frosting, thus affects the service life of double glazing.
Summary of the invention
In view of this, it is necessary to for above-mentioned problem, it is provided that a kind of simple and effective raising double glazing silicone adhesive
Comprehensive silicon ketone seal gum of gas barrier properties and preparation method thereof.
For achieving the above object, the present invention takes techniques below scheme:
The present invention uses the graphene oxide of 5-10 layer, surface-treated Graphene or white graphite alkenes two-dimensional layer to receive
Silicone sealant is modified by rice material so that it is barrier property and mechanical strength are greatly improved and other performances are unaffected.
The comprehensive silicon ketone seal gum of high-gas resistance performance of the present invention, including component A and B component;
Described component A includes that mass fraction is: 100 parts of basic glue, 0.01-10 part nano material powder body, 40-100 parts are filled out
Material, 5-10 part silane coupler;
Described B component includes that mass fraction is: 10-20 part cross-linking agent, 10-30 part plasticizer, 0.1-2 part catalyst;
Described component A and B component weight ratio are 10~13:1;
Described basic glue includes hydroxyl endblocked polydimethylsiloxane, hydroxyl-terminated polymethylphenyl sioxane, alcoxyl
In base end-blocking polydimethylsiloxane, ethenyl blocking polydimethylsiloxane, pi-allyl silica-based end-blocking polydimethylsiloxane
One;
Described nano material powder body includes in the graphene oxide of 5-10 layer, modified graphene or modified white graphite alkene
Kind.
Further, described basis glue is selected from the hydroxyl endblocked polydimethylsiloxane that viscosity is 50000~80000cP.
Further, described modified graphene or modified white graphite alkene, be by Graphene or white graphite alkene, dense in quality
Degree is the aqueous surfactant solution immersion 24h of 0.1%, and 50 DEG C of vacuum drying 48h prepare.
Further, described Graphene is modified use surfactant include dodecyl sodium sulfate, 12
In sodium alkyl benzene sulfonate, polyvinyl alcohol, sodium lignin sulfonate, cetyl trimethylammonium bromide, polyvinylpyrrolidone etc.
A kind of;The surfactant that dialogue Graphene is modified using is long-chain lewis base or long link Lewis acid.
Further, described long-chain lewis base is oleyl amine;Described long link Lewis acid is long-chain borine.
Further, described filler selected from gas-phase silica, silica flour, Pulvis Talci, ground calcium carbonate, precipitated calcium carbonate,
At least one in nm-class active calcium carbonate, montmorillonite, kieselguhr.
Further, described silane coupler is selected from γ-aminopropyl triethoxysilane, γ-(2,3-epoxy the third oxygen)
Propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-(β-aminoethyl)-γ-aminopropyl three
At least one in methoxy silane.
Further, described cross-linking agent is selected from MTMS, methyl three (dialkyl group dioxime) silane, vinyl
One in trimethoxy silane.
Further, described plasticizer is selected from 201 methyl-silicone oils that viscosity is 100~500cP.
Further, described catalyst is selected from dibutyl tin acetate, dibutyl tin dilaurate, Dibutyltin oxide
In one.
A kind of preparation method of the comprehensive silicon ketone seal gum of high-gas resistance performance, including:
Step 1) select the nano material powder body to be: the graphene oxide of 5-10 layer, process, through surfactant, changing of obtaining
Property Graphene or modified white graphite alkene in one;
Step 2) preparation of component A: by basis glue, nano material powder body, filler, silane coupler at kneader or planet
Stir in blender;
The preparation of B component: by cross-linking agent, plasticizer, catalyst add planetary mixer pressure be-0.06~-
Stir under the negative pressure of 0.099MPa;
At room temperature, by A, B two component mix to scale after i.e. obtain the silicone sealant of the present invention.
The invention have the benefit that
(1) modified graphene, graphene oxide or modified white graphite alkene have the performance of good separation gas and high strong
Degree, a small amount of interpolation can increase substantially the barrier property of silicone sealant and mechanical strength and other performances are unaffected;
(2) silicone sealant of the present invention is mainly used in two roads sealings of double glazing, seals with double glazing first
The butyl rubber compatibility used is good;
(3) present invention has good processing characteristics, environmentally friendly.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this
Bright technical scheme is made the most clearly and completely to describe.It should be noted that described embodiment is only the present invention one
Section Example rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not doing
Go out the every other embodiment obtained under creative work premise, broadly fall into the scope of protection of the invention.
Embodiment 1
Step 1) preparation of modified graphene: by the dodecyl sulphur that Graphene mass concentration is 0.1% of 5-10 layer
Acid sodium aqueous solution soaks 24h, 50 DEG C of vacuum drying 48h, obtains modified graphene.
Step 2) component A: by dialkyl polydimethylsiloxane that mass parts is 100 parts, step 1) in obtain 2 parts
Modified graphene, the gas-phase silica of 5 parts, the nm-class active calcium carbonate of 55 parts, the γ-aminopropyl triethoxysilane of 8 parts add
Enter and stir in kneader;
B component: by the MTMS that mass parts is 10 parts, 201 methyl-silicone oils of 20 parts, two fourths of 0.1 part
Base two tin acetate adds high speed planetary mixer, stirs under-0.08MPa negative pressure;
At room temperature, the silicone sealant of the present invention will i.e. be obtained after A, B two components mixing of 11:1 by weight.
Embodiment 2
Step 1) preparation of modified graphene: by the Graphene of the 5-10 layer polyvinylpyrrolidine of 0.1% mass concentration
Ketone aqueous solution soaking 24h, 50 DEG C of vacuum drying 48h, obtain modified graphene.
Step 2) component A: by dialkyl polydimethylsiloxane that mass parts is 100 parts, step 1) in obtain 5 parts
Modified graphene, the gas-phase silica of 5 parts, the nm-class active calcium carbonate of 75 parts, the γ-aminopropyl triethoxysilane of 10 parts
Join in kneader and stir;
B component: by the MTMS that mass parts is 12 parts, 201 methyl-silicone oils of 30 parts, two fourths of 0.2 part
Base two tin acetate adds planetary mixer, stirs under-0.08MPa negative pressure;
At room temperature, the silicone sealant of the present invention will i.e. be obtained after A, B two components mixing of 11:1 by weight.
Embodiment 3
Step 1) preparation of modified white graphite alkene: by the white graphite alkene of 5-10 layer with 0.1% the water-soluble immersion of long-chain borine
Bubble 24h, 50 DEG C of vacuum drying 48h, obtain modified white graphite alkene.
Step 2) component A: by dihydroxy PSI that mass fraction is 100 parts, step 1) in obtain 2
The modified white graphite alkene of part, 5 parts of silica flours, the precipitated calcium carbonate of 60 parts, γ-(2,3-epoxy the third oxygen) propyl group trimethoxy of 9 parts
Base silane joins in kneader and stirs;
B component: by methyl three (dialkyl group dioxime) silane that mass fraction is 10 parts, 201 methyl-silicone oils of 25 parts, 0.1
The dibutyl tin dilaurate of part adds planetary mixer and stirs under-0.09MPa negative pressure;
At room temperature, the silicone sealant of the present invention will i.e. be obtained after A, B two components mixing of 12:1 by weight.
Embodiment 4
Step 1) preparation of modified white graphite alkene: by the white graphite alkene of 5-10 layer with 0.1% oleyl amine aqueous solution soaking
24h, 50 DEG C of vacuum drying 48h, obtain modified white graphite alkene.
Step 2) component A: by dihydroxy PSI that mass fraction is 100 parts, step 1) in obtain 5
The modified white graphite alkene of part, 5 parts of silica flours, the precipitated calcium carbonate of 80 parts, γ-(2,3-epoxy the third oxygen) propyl group front three of 10 parts
TMOS is added in kneader and stirs;
B component: by methyl three (dialkyl group dioxime) silane that mass fraction is 13 parts, 201 methyl-silicone oils of 30 parts, 0.2
The dibutyl tin dilaurate of part adds planetary mixer and stirs under-0.09MPa negative pressure;
At room temperature, the silicone sealant of the present invention will i.e. be obtained after A, B two components mixing of 12:1 by weight.
Embodiment 5
Component A: by the alkoxy end-capped polydimethylsiloxane that mass parts is 100 parts, the graphene oxide of 2 parts, 70 parts
Nm-class active calcium carbonate, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane of 9 parts be added in kneader stirring all
Even;
B component: by vinyltrimethoxy silane that mass fraction is 10 parts, 201 methyl-silicone oils of 25 parts, 0.2 part
Dibutyltin oxide adds planetary mixer and stirs under-0.09MPa negative pressure;
At room temperature, the silicone sealant of the present invention will i.e. be obtained after A, B two components mixing of 12:1 by weight.
Embodiment 6
Component A: by the alkoxy end-capped polydimethylsiloxane that quality is 100 parts, the graphene oxide of 5 parts, 85 parts
Nm-class active calcium carbonate, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane of 10 parts add in kneader and stir;
B component: by vinyltrimethoxy silane that mass fraction is 14 parts, 201 methyl-silicone oils of 30 parts, 0.2 part
Dibutyltin oxide adds planetary mixer, stirs under-0.09MPa negative pressure;
At room temperature, the silicone sealant of the present invention will i.e. be obtained after A, B two components mixing of 12:1 by weight.
Comparative example 1
Component A: by the dialkyl polydimethylsiloxane that quality is 100 parts, the nm-class active calcium carbonate of 80 parts, 10 parts
N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane add in kneader and stir;
B component: by vinyltrimethoxy silane that mass fraction is 10 parts, 201 methyl-silicone oils of 30 parts, 0.2 part
Dibutyltin oxide adds planetary mixer, stirs under-0.09MPa negative pressure;
At room temperature, the silicone sealant of the present invention will i.e. be obtained after A, B two components mixing of 12:1 by weight.
For measuring the comprehensive silicon ketone seal gum ginseng of preparation-obtained high-gas resistance performance of the present invention in embodiment 1-6 in table 1
Number:
Table 1 embodiment 1-6 comprehensive silicon ketone seal gum data
Knowable to upper table 1, the preparation method of the present invention can increase substantially barrier property and the machinery of silicone sealant
Intensity.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (8)
1. the comprehensive silicon ketone seal gum of a high-gas resistance performance, it is characterised in that include component A and B component;
Described component A includes that mass fraction is: 100 parts of basic glue, 0.01-10 part nano material powder body, 40-100 part filler, 5-
10 parts of silane couplers;
Described B component includes that mass fraction is: 10-20 part cross-linking agent, 10-30 part plasticizer, 0.1-2 part catalyst;
Described component A and B component weight ratio are 10~13:1;
Described basic glue includes that hydroxyl endblocked polydimethylsiloxane, hydroxyl-terminated polymethylphenyl sioxane, alkoxyl seal
In end polydimethylsiloxane, ethenyl blocking polydimethylsiloxane, pi-allyl silica-based end-blocking polydimethylsiloxane one
Kind;
Described nano material powder body includes the one in the graphene oxide of 5-10 layer, modified graphene or modified white graphite alkene.
Comprehensive silicon ketone seal gum the most according to claim 1, it is characterised in that described basis glue is 50000 selected from viscosity
~the hydroxyl endblocked polydimethylsiloxane of 80000cP.
Comprehensive silicon ketone seal gum the most according to claim 1, it is characterised in that described modified graphene or modified white graphite
Alkene, is by Graphene or white graphite alkene, soaks 24h, 50 DEG C of vacuum at the aqueous surfactant solution that mass concentration is 0.1%
Dry 48h prepares.
Comprehensive silicon ketone seal gum the most according to claim 3, it is characterised in that described Graphene is modified use
Surfactant includes dodecyl sodium sulfate, dodecylbenzene sodium sulfonate, polyvinyl alcohol, sodium lignin sulfonate, cetyl
One in trimethylammonium bromide, polyvinylpyrrolidone etc.;The surfactant that dialogue Graphene is modified using is for long
One in chain lewis base, long link Lewis acid, quaternary ammonium compound, azochlorosulfonate acid compound, nonionic surfactant.
Comprehensive silicon ketone seal gum the most according to claim 4, it is characterised in that described long-chain lewis base is oleyl amine;Institute
State long link Lewis acid be long-chain lewis base described in long-chain borine be amine;Described long link Lewis acid is boranes;Described
Quaternary ammonium compound is the one in alkyl trimethyl quaternary ammonium salt, alkyldimethylbenzylammonium quaternary ammonium salt, dialkyl dimethyl quaternary ammonium salt;Institute
Stating azochlorosulfonate acid compound is the one in dodecylbenzene sodium sulfonate, dodecyl sodium sulfate, sodium lignin sulfonate, sodium glycocholate;Institute
Stating nonionic surfactant is the one in polyethers, polyester, polyvinyl alcohol, cellulose derivative.
Comprehensive silicon ketone seal gum the most according to claim 1, it is characterised in that described filler is selected from gas-phase silica, stone
At least one in Ying Fen, Pulvis Talci, ground calcium carbonate, precipitated calcium carbonate, nm-class active calcium carbonate, montmorillonite, kieselguhr;
Described silane coupler is selected from γ-aminopropyl triethoxysilane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicon
In alkane, γ-methacryloxypropyl trimethoxy silane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane
At least one.
Comprehensive silicon ketone seal gum the most according to claim 1, it is characterised in that described cross-linking agent is selected from methyl trimethoxy epoxide
One in silane, methyl three (dialkyl group dioxime) silane, vinyltrimethoxy silane;
Described plasticizer is selected from 201 methyl-silicone oils that viscosity is 100~500cP;
Described catalyst one in dibutyl tin acetate, dibutyl tin dilaurate, Dibutyltin oxide.
8. the preparation method of the comprehensive silicon ketone seal gum described in any one described in claim 1-7, it is characterised in that including:
Step 1) select the nano material powder body to be: the graphene oxide of 5-10 layer, process the modified stone obtained through surfactant
One in ink alkene or modified white graphite alkene;
Step 2) preparation of component A: by basis glue, nano material powder body, filler, silane coupler at kneader or planet stirring
Stir in machine;
The preparation of B component: cross-linking agent, plasticizer, catalyst are added planetary mixer is-0.06~-0.099MPa at pressure
Negative pressure under stir;
At room temperature, by A, B two component mix to scale after i.e. obtain the silicone sealant of the present invention.
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CN201610703675.1A CN106281205A (en) | 2016-08-22 | 2016-08-22 | A kind of comprehensive silicon ketone seal gum of high-gas resistance performance and preparation method thereof |
CN201710714421.4A CN107383752A (en) | 2016-08-22 | 2017-08-18 | A kind of modified compound ABS material of white graphite alkene and preparation method thereof |
CN201710713906.1A CN107446243A (en) | 2016-08-22 | 2017-08-18 | A kind of modified white graphite alkene composite polypropylene tubing and preparation method thereof |
CN201710713907.6A CN107383693A (en) | 2016-08-22 | 2017-08-18 | A kind of modified white graphite alkene composite ganoine polychloroethylene pipes and preparation method thereof |
CN201710713884.9A CN107383612B (en) | 2016-08-22 | 2017-08-18 | Modified white graphene composite polypropylene aluminum-plastic steady-state pipe and preparation method thereof |
CN201710714408.9A CN107541179A (en) | 2016-08-22 | 2017-08-18 | A kind of compound silicone sealant of high-gas resistance performance and preparation method thereof |
CN201710713133.7A CN107383545A (en) | 2016-08-22 | 2017-08-18 | A kind of modified white graphite alkene composite polyethylene pipe and preparation method thereof |
PCT/CN2017/098068 WO2018036427A1 (en) | 2016-08-22 | 2017-08-18 | Composite silicone sealant having high gas barrier property and preparation method therefor |
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CN201610703675.1A CN106281205A (en) | 2016-08-22 | 2016-08-22 | A kind of comprehensive silicon ketone seal gum of high-gas resistance performance and preparation method thereof |
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CN201610703675.1A Pending CN106281205A (en) | 2016-08-22 | 2016-08-22 | A kind of comprehensive silicon ketone seal gum of high-gas resistance performance and preparation method thereof |
CN201710714408.9A Pending CN107541179A (en) | 2016-08-22 | 2017-08-18 | A kind of compound silicone sealant of high-gas resistance performance and preparation method thereof |
CN201710713907.6A Pending CN107383693A (en) | 2016-08-22 | 2017-08-18 | A kind of modified white graphite alkene composite ganoine polychloroethylene pipes and preparation method thereof |
CN201710713133.7A Pending CN107383545A (en) | 2016-08-22 | 2017-08-18 | A kind of modified white graphite alkene composite polyethylene pipe and preparation method thereof |
CN201710713884.9A Active CN107383612B (en) | 2016-08-22 | 2017-08-18 | Modified white graphene composite polypropylene aluminum-plastic steady-state pipe and preparation method thereof |
CN201710714421.4A Pending CN107383752A (en) | 2016-08-22 | 2017-08-18 | A kind of modified compound ABS material of white graphite alkene and preparation method thereof |
CN201710713906.1A Pending CN107446243A (en) | 2016-08-22 | 2017-08-18 | A kind of modified white graphite alkene composite polypropylene tubing and preparation method thereof |
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CN201710714408.9A Pending CN107541179A (en) | 2016-08-22 | 2017-08-18 | A kind of compound silicone sealant of high-gas resistance performance and preparation method thereof |
CN201710713907.6A Pending CN107383693A (en) | 2016-08-22 | 2017-08-18 | A kind of modified white graphite alkene composite ganoine polychloroethylene pipes and preparation method thereof |
CN201710713133.7A Pending CN107383545A (en) | 2016-08-22 | 2017-08-18 | A kind of modified white graphite alkene composite polyethylene pipe and preparation method thereof |
CN201710713884.9A Active CN107383612B (en) | 2016-08-22 | 2017-08-18 | Modified white graphene composite polypropylene aluminum-plastic steady-state pipe and preparation method thereof |
CN201710714421.4A Pending CN107383752A (en) | 2016-08-22 | 2017-08-18 | A kind of modified compound ABS material of white graphite alkene and preparation method thereof |
CN201710713906.1A Pending CN107446243A (en) | 2016-08-22 | 2017-08-18 | A kind of modified white graphite alkene composite polypropylene tubing and preparation method thereof |
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2017
- 2017-08-18 CN CN201710714408.9A patent/CN107541179A/en active Pending
- 2017-08-18 CN CN201710713907.6A patent/CN107383693A/en active Pending
- 2017-08-18 CN CN201710713133.7A patent/CN107383545A/en active Pending
- 2017-08-18 CN CN201710713884.9A patent/CN107383612B/en active Active
- 2017-08-18 CN CN201710714421.4A patent/CN107383752A/en active Pending
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CN107383545A (en) | 2017-11-24 |
CN107446243A (en) | 2017-12-08 |
CN107383612B (en) | 2022-03-29 |
CN107383612A (en) | 2017-11-24 |
CN107541179A (en) | 2018-01-05 |
WO2018036427A1 (en) | 2018-03-01 |
CN107383752A (en) | 2017-11-24 |
CN107383693A (en) | 2017-11-24 |
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