CN109722216A - A kind of Silante terminated liquid polybutadiene modified organic silicon sealant and preparation method thereof - Google Patents
A kind of Silante terminated liquid polybutadiene modified organic silicon sealant and preparation method thereof Download PDFInfo
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- CN109722216A CN109722216A CN201811633173.1A CN201811633173A CN109722216A CN 109722216 A CN109722216 A CN 109722216A CN 201811633173 A CN201811633173 A CN 201811633173A CN 109722216 A CN109722216 A CN 109722216A
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Abstract
The invention discloses a kind of Silante terminated liquid polybutadiene modified organic silicon sealants, including following parts by weight component: α, 100 parts of alpha, omega-dihydroxy polydimethyl siloxane, 10~30 parts of silane-modified polybutadiene, 0.1~30 part of plasticizer, 10~500 parts of filler, take off 2~30 parts of diacetylmonoxime type organosilane cross-linking agent, 0.05~8 part of adhesive accelerant, 0.1~8 part of catalyst.The invention also discloses the preparation methods of Silante terminated liquid polybutadiene modified organic silicon sealant.Improved in the present invention using Silante terminated liquid polybutadiene modified organic silicon and solved thixotropic defect, can be eliminated on the basis of keeping certain adhesive property influence of the amino to system storage stability, can and bonding interface the generations bonding such as hydroxyl, metal ion, and polybutadiene main chain and polysiloxane network are entwined, to reach coupled action, promote bonding.
Description
Technical field
The present invention relates to a kind of organosilicon sealants and preparation method thereof, more particularly to a kind of Silante terminated poly- fourth of liquid
Diene modified organosilicon sealant and preparation method thereof.
Background technique
With social progress, industrial glue requires higher and higher, room temperature vulcanized silicone rubber requirement faster curing time, more
Simple curing process, higher storage stability requires and stronger service performance;Ketoxime removing type room temperature vulcanized sealant with
Its excellent strong adhesive property occupies the market share of the room temperature vulcanized silicone rubber overwhelming majority, but the height in its preparation process
Stability in viscosity, storing process and certain limitation is above received in application to the extensive adhesive property of various substrates.
Summary of the invention
In view of the above shortcomings of the prior art, the object of the present invention is to provide a kind of Silante terminated liquid polybutadiene is modified
Organosilicon sealant improves and solves thixotropic defect, and amino is eliminated on the basis of keeping certain adhesive property to system
The influence of storage stability.It is a further object to provide a kind of Silante terminated liquid polybutadiene modified organic silicon is close
The preparation method of sealing.
The technical scheme is that such: a kind of Silante terminated liquid polybutadiene modified organic silicon sealant, packet
Following parts by weight component: α is included, 100 parts of alpha, omega-dihydroxy polydimethyl siloxane, 10~30 parts of silane-modified polybutadiene increases
0.1~30 part of agent of modeling, takes off 2~30 parts of diacetylmonoxime type organosilane cross-linking agent, adhesive accelerant 0.05~8 by 10~500 parts of filler
Part, 0.1~8 part of catalyst.
Further, the silane-modified polybutadiene be methoxyl group modified polybutadiene, ethyoxyl modified polybutadiene,
One or more of methoxyl group/ethyoxyl mixing blocking modification polybutadiene mixture, the silane-modified polybutadiene knot
Structure formula is as follows:
Wherein R " is methyl, ethyl or propyl.
Further, the de- diacetylmonoxime type silane crosslinker is vinyl tributyl ketoximyl silane, three diacetylmonoxime of methyl
Base silane, four butanone oximino silanes and the one such or several mixture of phenyl tributanoximo silane.
Further, the α, kinematic viscosity of the alpha, omega-dihydroxy polydimethyl siloxane at 25 DEG C be 20000~
100000mPa·s。
Further, the filler includes reinforcement and functional filler, and the reinforced filling includes white carbon black, lightweight carbonic acid
Calcium or powdered whiting;The functional filler includes silver powder, graphite powder, silicon carbide, silicon powder, silicon nitride, aluminium oxide, hydrogen-oxygen
Change aluminium, magnesium hydroxide or di-iron trioxide;The filler is that the reinforced filling and functional filler are one such or several
Mixture.
Further, the plasticizer is one of dimethicone, alkoxy end-capped silicone oil, methoxyl group silicone oil or several
The mixture of kind.
Further, the adhesion promoters can be amino silicane coupling agent;The amino silicane coupling agent be mono amino,
The silane coupling agent of the bifunctionality of double amino or polyamino, three-functionality-degree or polyfunctionality, wherein amino contain primary amine groups,
One or more of combinations of secondary amine and tertiary amine groups.
Further, the catalyst is organotin catalysts, and the organotin catalysts include di lauric dibutyl
One of tin, two capric acid dioctyl tins, tin dilaurate dioctyl tin and two capric acid dibutyl tins.
A kind of preparation method of Silante terminated liquid polybutadiene modified organic silicon sealant, includes the following steps,
100 parts of α by weight, alpha, omega-dihydroxy polydimethyl siloxane, stirring heating are put into after step 1, mixing machine starting
To 50 DEG C or more investments 10~500 parts of fillers, 0.1~30 part of plasticizer, stirring is warming up to 135-150 DEG C, and 135 DEG C with
The upper continuous operation time is more than 3 hours, vacuum dehydration under -0.09MPa state, and detects output base when moisture value is lower than 100ppm
Material;
The base-material of output is cooled to room temperature by step 2, measures rate of extrusion in 7~15g15s-1;
Step 3 has base-material input in the high-speed mixer of vacuum condition, and it is≤60 that vacuum defoamation, which keeps state of temperature,
℃;
High-speed stirring under vacuum state is added in base-material in 10~30 parts by weight of silane-modified polybutadiene by step 4
Mix 0.5~1h;
Step 5, will 2~30 parts of de- diacetylmonoxime type organosilane cross-linking agents by weight, 0.05~8 part of adhesion promoters,
0.1~8 part of catalyst measures under normal temperature state prepares in addition system high speed dispersion under vacuum state;
Colloid after dispersion is inputted the condenser cooling temperature of 5~10 DEG C of ice water state of temperatures to 20~45 DEG C by step 6.
The beneficial effect of technical solution provided by the present invention is: silane-modified polybutadiene, which is added in base-material, significantly to be changed
The thixotropy of kind silicone sealant, greatly improves the elongation at break of silicone sealant, reduces its hardness and modulus, enhance it
Toughness.Group can generate bonding with amino silane in silane-modified polybutadiene, generate the adhesion promoters of macromolecular, can
Influence of the amino to system storage stability, while silane-modified polybutadiene are eliminated on the basis of keeping certain adhesive property
Interior group has very high reactivity, can be bonded with generations such as hydroxyl, the metal ions of bonding interface, and polybutadiene
Main chain and polysiloxane network are entwined, to reach coupled action, promote bonding.To obtain a kind of simple production process, viscous
Connect the organosilicon sealant that range is wide, storage performance is excellent.Silane-modified polybutadiene institute's performance characteristic such as Fig. 1 institute in the present invention
Show.
Detailed description of the invention
Fig. 1 is that silane-modified polybutadiene acts on schematic diagram.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but not as a limitation of the invention.
Embodiment 1
The α that 100 parts of viscosity of investment are 80000mPas after step 1, the starting of 5000L high-speed mixer, alpha, omega-dihydroxy are poly-
Dimethyl siloxane, the dimethyl-silicon that stirring is warming up to 50 DEG C of 350 parts of precipitated calcium carbonates of investment and 30 parts of viscosity are 350mPas
Oil, stirring is warming up to 145 DEG C, and 135 DEG C or more continuous operation times reach 3 hours, vacuum dehydration under -0.09MPa state,
Output base-material when moisture value is 80ppm is detected using moisture teller;
The base-material of step 1 output is cooled to room temperature by step 2, is surveyed with Hegman grind gage measurement fineness, with rate of extrusion machine
Rate of extrusion is determined in 10.2g15s-1;
Step 3 has the base-material input of test passes in the high-speed mixer of vacuum condition, and vacuum defoamation keeps temperature
State is 28 DEG C;
High-speed stirred 1h under vacuum state is added in base-material in 30 parts of methoxyl group modified polybutadienes by step 4, can significantly be changed
The thixotropy of kind silicone sealant, greatly improves the elongation at break of silicone sealant, reduces its hardness and modulus, enhance it
Toughness.
Step 5, by 25 parts of vinyl tributyl ketoximyl silanes, 8 parts of amino silane oligomer, 3 parts of di lauric dibutyls
Tin high speed dispersion under vacuum state in addition system under normal temperature state, in silane-modified polybutadiene group can and amino silicone
Alkane generates bonding, generates the adhesion promoters of macromolecular, amino can be eliminated on the basis of keeping certain adhesive property to body
It is the influence of storage stability, while group has very high reactivity in silane-modified polybutadiene, can and be bonded
The generations such as hydroxyl, the metal ion at interface bonding, and polybutadiene main chain and polysiloxane network are entwined, and are made to reach coupling
With promotion bonding;
Step 6, the finished product glue after step 5 reaction are in the condenser cooling temperature for inputting 8 DEG C of ice water state of temperatures to 27
DEG C, it is dispensed.
Embodiment 2
50 parts of viscosity of investment are that 50000mPas and 50 part of viscosity is after step 1, the starting of 5000L high-speed mixer
The α of 80000mPas, alpha, omega-dihydroxy polydimethyl siloxane, stirring are warming up to 50 DEG C of investment 110 parts of powdered whitings and 15
The dimethicone that part viscosity is 5000mPas, stirring is warming up to 150 DEG C, and 135 DEG C or more continuous operation times reach 3
Hour, vacuum dehydration under -0.09MPa state detects output base-material when moisture value is 50ppm using moisture teller;
The base-material of step 1 output is cooled to room temperature by step 2, is surveyed with Hegman grind gage measurement fineness, with rate of extrusion machine
Rate of extrusion is determined in 9.3g15s-1;
Step 3 has the base-material input of test passes in the high-speed mixer of vacuum condition, and vacuum defoamation keeps temperature
State is 30 DEG C;
Vacuum in base-material is added in 15 parts of methoxyl group modified polybutadienes and 10 parts of ethyoxyl modified polybutadienes by step 4
High-speed stirred 1h under state;
Step 5, by 15 part of four butanone oximino silane, 4 parts of N- (β-aminoethyl)-γ-aminopropyltrimethoxysilanes, 1 part
Two capric acid dibutyl tins high speed dispersion under vacuum state in addition system under normal temperature state;
Step 6, the finished product glue after step 5 reaction are in the condenser cooling temperature for inputting 8 DEG C of ice water state of temperatures to 20
DEG C, it is dispensed.
Embodiment 3
The α that 100 parts of viscosity of investment are 100000mPas after step 1, the starting of 5000L high-speed mixer, alpha, omega-dihydroxy are poly-
Dimethyl siloxane, the methoxyl group silicon that stirring is warming up to 50 DEG C of 10 parts of aluminium hydroxides of investment and 0.1 part of viscosity is 350mPas
Oil, stirring is warming up to 135 DEG C, and 135 DEG C or more continuous operation times reach 3.5 hours, and vacuum is de- under -0.09MPa state
Water detects output base-material when moisture value is 80ppm using moisture teller;
The base-material of step 1 output is cooled to room temperature by step 2, is surveyed with Hegman grind gage measurement fineness, with rate of extrusion machine
Rate of extrusion is determined in 7.3g15s-1;
Step 3 has the base-material input of test passes in the high-speed mixer of vacuum condition, and vacuum defoamation keeps temperature
State is 35 DEG C;
High speed under vacuum state is added in base-material in 20 parts of methoxyl groups/ethyoxyl mixing blocking modification polybutadiene by step 4
Stir 0.5h;
It is step 5,2 parts of phenyl tributanoximo silanes, 0.05 part of amino silane oligomer, 0.1 part of tin dilaurate two is pungent
Ji Xi high speed dispersion under vacuum state in addition system under normal temperature state;
Step 6, the finished product glue after step 5 reaction are in the condenser cooling temperature for inputting 10 DEG C of ice water state of temperatures to 45
DEG C, it is dispensed.
Embodiment 4
40 parts of viscosity of investment are that 20000mPas and 60 part of viscosity is after step 1, the starting of 5000L high-speed mixer
The α of 50000mPas, alpha, omega-dihydroxy polydimethyl siloxane, stirring are warming up to 50 DEG C of investment 500 parts of precipitated calcium carbonates and 10
The alkoxy end-capped silicone oil that part viscosity is 5000mPas, stirring are warming up to 148 DEG C, and 135 DEG C or more continuous operation times
Reach 3.5 hours, vacuum dehydration under -0.09MPa state, detects output base-material when moisture value is 50ppm using moisture teller;
The base-material of step 1 output is cooled to room temperature by step 2, is surveyed with Hegman grind gage measurement fineness, with rate of extrusion machine
Rate of extrusion is determined in 14.6g15s-1;
Step 3 has the base-material input of test passes in the high-speed mixer of vacuum condition, and vacuum defoamation keeps temperature
State is 45 DEG C;
High-speed stirred 1h under vacuum state is added in base-material in 10 parts of ethyoxyl modified polybutadienes by step 4;
Step 5, by 30 parts of methyl tributanoximo silanes, 8 parts of N- (β-aminoethyl)-γ-aminopropyltrimethoxysilanes,
3 parts of dibutyl tin dilaurates high speed dispersion under vacuum state in addition system under normal temperature state;
Step 6, the finished product glue after step 5 reaction are in the condenser cooling temperature for inputting 5 DEG C of ice water state of temperatures to 25
DEG C, it is dispensed.
Comparative example
The α that 100 parts of viscosity of investment are 80000mPas after step 1, the starting of 5000L high-speed mixer, alpha, omega-dihydroxy are poly-
Dimethyl siloxane, the dimethyl-silicon that stirring is warming up to 50 DEG C of 350 parts of precipitated calcium carbonates of investment and 30 parts of viscosity are 350mPas
Oil, stirring is warming up to 145 DEG C, and 135 DEG C or more continuous operation times reach 3 hours, vacuum dehydration under -0.09MPa state,
Output base-material when moisture value is 80ppm is detected using moisture teller;
The base-material of step 1 output is cooled to room temperature by step 2, is surveyed with Hegman grind gage measurement fineness, with rate of extrusion machine
Rate of extrusion is determined in 10.2g15s-1;
Step 3 has the base-material input of test passes in the high-speed mixer of vacuum condition, and vacuum defoamation keeps temperature
State is 28 DEG C;
Step 4, by 25 parts of vinyl tributyl ketoximyl silanes, 8 parts of amino silane oligomer, 3 parts of di lauric dibutyls
Tin high speed dispersion under vacuum state in addition system under normal temperature state;
Step 5, the finished product glue after step 4 reaction are in the condenser cooling temperature for inputting 8 DEG C of ice water state of temperatures to 27
DEG C, it is dispensed.
The testing result for the sealant performance that various embodiments of the present invention and comparative example are prepared is as follows:
Although the present invention is disclosed as above with preferred embodiment, they are not for limiting the present invention, guarantor of the invention
Shield range should be subject to the content that claims hereof protection scope defined.It is any to be familiar with the art person,
It does not depart from the spirit and scope of the present invention, made various change or equivalent replacement, protection model of the invention all should belong to
It encloses.
Claims (9)
1. a kind of Silante terminated liquid polybutadiene modified organic silicon sealant, it is characterised in that: including following parts by weight array
Point: α, 100 parts of alpha, omega-dihydroxy polydimethyl siloxane, 10~30 parts of silane-modified polybutadiene, is filled out by 0.1~30 part of plasticizer
10~500 parts of material, de- 2~30 parts of diacetylmonoxime type organosilane cross-linking agent, 0.05~8 part of adhesive accelerant, catalyst 0.1~8
Part.
2. Silante terminated liquid polybutadiene modified organic silicon sealant according to claim 1, it is characterised in that: described
Silane-modified polybutadiene is methoxyl group modified polybutadiene, ethyoxyl modified polybutadiene, methoxyl group/ethyoxyl mixing sealing end
One or more of modified polybutadiene mixture, the silane-modified polybutadiene configuration formula are as follows:
Wherein R " is methyl, ethyl or propyl.
3. Silante terminated liquid polybutadiene modified organic silicon sealant according to claim 1, it is characterised in that: described
De- diacetylmonoxime type silane crosslinker is vinyl tributyl ketoximyl silane, methyl tributanoximo silane, four butanone oximino silanes
One such or several mixture with phenyl tributanoximo silane.
4. Silante terminated liquid polybutadiene modified organic silicon sealant according to claim 1, it is characterised in that: described
α, kinematic viscosity of the alpha, omega-dihydroxy polydimethyl siloxane at 25 DEG C are 20000~100000mPas.
5. Silante terminated liquid polybutadiene modified organic silicon sealant according to claim 1, it is characterised in that: described
Filler includes reinforced filling and functional filler, and the reinforced filling includes white carbon black, precipitated calcium carbonate or powdered whiting;Institute
Stating functional filler includes silver powder, graphite powder, silicon carbide, silicon powder, silicon nitride, aluminium oxide, aluminium hydroxide, magnesium hydroxide or three
Aoxidize two iron;The filler is the reinforced filling and the one such or several mixture of functional filler.
6. Silante terminated liquid polybutadiene modified organic silicon sealant according to claim 1, it is characterised in that: described
Plasticizer is the mixture of one or more of dimethicone, alkoxy end-capped silicone oil, methoxyl group silicone oil.
7. Silante terminated liquid polybutadiene modified organic silicon sealant according to claim 1, it is characterised in that: described
Adhesion promoters can be amino silicane coupling agent;The amino silicane coupling agent is double officials of mono amino, double amino or polyamino
The silane coupling agent of energy degree, three-functionality-degree or polyfunctionality, wherein amino contains one kind of primary amine groups, secondary amine and tertiary amine groups
Or several combination.
8. Silante terminated liquid polybutadiene modified organic silicon sealant according to claim 1, it is characterised in that:, institute
Stating catalyst is organotin catalysts, and the organotin catalysts include dibutyl tin dilaurate, two capric acid dioctyl tins, two
One of dioctyltin laurate and two capric acid dibutyl tins.
9. a kind of preparation method of Silante terminated liquid polybutadiene modified organic silicon sealant, it is characterised in that: including following
Step,
100 parts of α by weight, alpha, omega-dihydroxy polydimethyl siloxane are put into after step 1, mixing machine starting, stirring is warming up to 50
DEG C or more investment 10~500 parts of fillers, 0.1~30 part of plasticizer, stirring be warming up to 135-150 DEG C, and held at 135 DEG C or more
The continuous activity duration is more than 3 hours, vacuum dehydration under -0.09MPa state, and detects output base-material when moisture value is lower than 100ppm;
The base-material of output is cooled to room temperature by step 2, measures rate of extrusion in 7~15g15s-1;
Step 3 has base-material input in the high-speed mixer of vacuum condition, and it is≤60 DEG C that vacuum defoamation, which keeps state of temperature,;
High-speed stirred 0.5 under vacuum state is added in base-material in 10~30 parts by weight of silane-modified polybutadiene by step 4
~1h;
Step 5, will 2~30 parts of de- diacetylmonoxime type organosilane cross-linking agents by weight, 0.05~8 part of adhesion promoters, 0.1~
8 parts of catalyst measure under normal temperature state prepares in addition system high speed dispersion under vacuum state;
Colloid after dispersion is inputted the condenser cooling temperature of 5~10 DEG C of ice water state of temperatures to 20~45 DEG C by step 6.
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CN116144315A (en) * | 2022-12-11 | 2023-05-23 | 湖北兴瑞硅材料有限公司 | Dealcoholized organosilicon sealant and preparation method thereof |
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CN116144315A (en) * | 2022-12-11 | 2023-05-23 | 湖北兴瑞硅材料有限公司 | Dealcoholized organosilicon sealant and preparation method thereof |
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