CN106833507A - Multicomponent silicone sealant and preparation method thereof - Google Patents
Multicomponent silicone sealant and preparation method thereof Download PDFInfo
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- CN106833507A CN106833507A CN201710121643.5A CN201710121643A CN106833507A CN 106833507 A CN106833507 A CN 106833507A CN 201710121643 A CN201710121643 A CN 201710121643A CN 106833507 A CN106833507 A CN 106833507A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of multicomponent silicone sealant for doors and windows sealing and preparation method thereof.Weight ratio of the multicomponent silicone sealant including component A, component B and component C, the component A and the component B is 7:1~15:1, the component A are 10 with the weight ratio of the component C:1~30:1；The component A is prepared from by organopolysiloxane polymer, inorganic filler and thixotropic agent, the component B is prepared from by organopolysiloxane polymer, inorganic filler, silane multiple crosslinking agent, silane coupler and organotin catalysts, and the component C is prepared from by organopolysiloxane polymer, organic silicon defoamer and toner.The multicomponent silicone sealant has advantages below：Curing rate is fast, and solidification can not be influenceed by ambient humidity, and can be adjusted within the specific limits, has good caking property to sash stuff, and toning is simple, the color needed for being conveniently deployed into user, good mechanical properties.
Description
Technical field
The present invention relates to fluid sealant field, more particularly to a kind of multicomponent silicone sealant and preparation method thereof.
Background technology
Silicone sealant has excellent ultraviolet aging resistance, weather-resistant performance and adhesive property, uses extensively at present
In joint seal, the door of the sealing of two roads, external wall and inside of the glass curtain wall structure bonding, double glazing of building trade
Window seam is sealing adhesive.
Fluid sealant for doors and windows sealing is needed according to section bar and user's request allotment shades of colour.Existing bi-component silicon
Ketone seal gum cannot meet toning and require, thus, bi-component silicone fluid sealant is little in the application of doors and windows sealing field.Existing door
Window seam silicone sealant is nearly all single-component silicone fluid sealant, because the advantage of single-component silicone fluid sealant is to construct
It is simple to operate, it is highly suitable for job site and uses.But single-component silicone fluid sealant needs absorption air in its solidification process
In moisture, solidification is relatively slow, and curing rate is non-adjustable, while being influenceed by environment temperature, humidity, and is difficult to consolidate under airtight condition
Change.The assembling processing of current door and window is most to be completed in processing factory workshop, need to often be supported in workshop using single-component silicone fluid sealant
Could be shipped after the shield a few days and dispatched from the factory, even longer curing time is needed when environment temperature, humidity are relatively low.Single-component silicone is close
The own characteristic of sealing can not meet the demand of existing door and window rapid processing.
The content of the invention
Based on this, the invention provides a kind of multicomponent silicone sealant.The curing rate of the multicomponent silicone sealant
Hurry up, and can realize simply being mixed colours according to demand, it is adaptable to doors and windows sealing field.
Concrete technical scheme is as follows：
A kind of multicomponent silicone sealant, including component A, component B and component C, the component A and the component B weight
Amount is than being 7:1~15:1, the component A are 10 with the weight ratio of the component C:1~30:1；
The component A is prepared from by the raw material of following weight portion：
100 parts of organopolysiloxane polymer
60~150 parts of inorganic filler
0~5 part of thixotropic agent；
The component B is prepared from by the raw material of following weight portion：
The component C is prepared from by the raw material of following weight portion：
4~20 parts of organopolysiloxane polymer
0.5~5 part of organic silicon defoamer
0.1~15 part of toner；
The organopolysiloxane polymer is selected from dimethyl silicone polymer, alkoxy end-capped poly- two of terminal hydroxy group end-blocking
At least one in methylsiloxane, alkyl-blocked dimethyl silicone polymer；
The silane multiple crosslinking agent is that mass ratio is 1:3-3:1 crosslinking agent A and the composition of crosslinking agent B；The friendship
Connection agent A is selected from methyl tributanoximo silane, vinyl tributyl ketoximyl silane, phenyl tributanoximo silane, four diacetylmonoximes
At least one in base silane, methyl tri acetylacetonate oximino silane；The crosslinking agent B is selected from the butanone oximido silicon of methyl ethylene two
Alkane, the butanone oximino silane of dimethyl two, the butanone oximino silane of aminomethyl phenyl two, the butanone oximino silane of diphenyl two, dimethyl two
(N- methylacetamidos) silane, dimethyl two (N- ethylacetamidos) silane, (the N- methyl vinyl ammonia of methyl ethylene two
Base) silane, methyl ethylene two (epsilon-caprolactams base) silane, aminomethyl phenyl two (N- methylacetamidos) silane, diphenyl
At least one in two (N- methylacetamidos) silane.
Wherein in some embodiments, the organopolysiloxane polymer is selected from α, alpha, omega-dihydroxy polydimethyl silica
At least one in alkane, dimethicone, trimethoxy end-blocking dimethyl silicone polymer.
Wherein in some embodiments, viscosity of the organopolysiloxane polymer at 25 DEG C be 100~
100000cp。
Wherein in some embodiments, viscosity of the organopolysiloxane polymer at 25 DEG C be 100~
20000cp。
Wherein in some embodiments, the inorganic filler be selected from nm-class active calcium carbonate, powdered whiting, silicon powder,
At least one in diatomite, kaolin, talcum powder, precipitated silica, fume colloidal silica；And/or the thixotropic agent choosing
At least one from polyamide wax, polyethers, silane-modified polyethers and organic bentonite.
Wherein in some embodiments, the inorganic filler is selected from nm-class active calcium carbonate, powdered whiting, silicon powder
At least one.
Wherein in some embodiments, the silane coupler is selected from r-chloropropyl trimethoxyl silane, the ethoxy of chloropropyl three
Base silane, γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, N- β-aminoethyl-γ-aminopropyl trimethoxy
Base silane, N- β-aminoethyl-gamma-aminopropyl-triethoxy-silane, N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane,
N- β-aminoethyl-γ-aminopropyltriethoxy diethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-shrink
Glycerin ether oxygen propyl-triethoxysilicane, γ-glycidyl ether oxygen propyl methyl dimethoxysilane, γ-glycidyl ether oxygen
Hydroxypropyl methyl diethoxy silane, epoxycyclohexyl trimethoxy silane, epoxycyclohexyl triethoxysilane, 3- mercaptos propyl group three
Methoxy silane, 3- mercaptopropyltriethoxysilanes, NCO propyl trimethoxy silicane, the second of NCO propyl group three
At least one in TMOS, 3- ureido-propyl trimethoxy silanes, 3- ureidopropyltriethoxysilanes.
Wherein in some embodiments, the silane coupler is selected from γ-aminopropyltrimethoxysilane, γ-aminopropyl
Triethoxysilane, N- β-aminoethyl-γ-aminopropyltrimethoxysilane, N- β-aminoethyl-gamma-aminopropyl-triethoxy silicon
Alkane, γ-glycidyl ether oxygen propyl trimethoxy silicane, epoxycyclohexyl trimethoxy silane, epoxycyclohexyl triethoxy
Two kinds in silane.
Wherein in some embodiments, the organotin catalysts are selected from dibutyltin diacetate, di lauric dibutyl
In tin, tin dilaurate dioctyl tin, stannous octoate, two neodecanoic acid stannous methides, dibutyl tin double (beta-diketo-esters) at least one
Kind.
Wherein in some embodiments, the organotin catalysts are selected from dibutyltin diacetate, di lauric dibutyl
At least one in tin, dibutyl tin double (beta-diketo-esters).
Wherein in some embodiments, the organic silicon defoamer is fluorosilicone.The fluorosilicone has Formulas I structure：
Wherein m is that 1~5, n is 10~1000.
Wherein in some embodiments, the toner be carbon black, titanium dioxide, zinc oxide, chrome yellow, cadmium yellow, iron oxide yellow,
At least one in iron oxide red, cadmium red, molybdate red, ultramarine, cobalt blue, barba hispanica, phthalocyanine blue, phthalocyanine green, cobalt green, chrome oxide green.
Wherein in some embodiments, the silane multiple crosslinking agent is that mass ratio is 0.8-2.8:1 crosslinking agent A and friendship
The composition of connection agent B；The crosslinking agent A is selected from vinyl tributyl ketoximyl silane, phenyl tributanoximo silane and four butanone
At least one in oximino silane；The crosslinking agent B is selected from the butanone oximino silane of methyl ethylene two, the butanone oximido of dimethyl two
At least one in silane and methyl ethylene two (N- methylacetamidos) silane.
Wherein in some embodiments, the component A is prepared from by the raw material of following weight portion：
100 parts of organopolysiloxane polymer
100~120 parts of inorganic filler
0~0.6 part of thixotropic agent；
The component B is prepared from by the raw material of following weight portion：
The component C is prepared from by the raw material of following weight portion：
6~10 parts of organopolysiloxane polymer
0.5~2 part of organic silicon defoamer
2~4 parts of toner.
Present invention also offers the preparation method of above-mentioned multicomponent silicone sealant.
Concrete technical scheme is as follows：
A kind of preparation method of above-mentioned multicomponent silicone sealant, comprises the following steps：
The preparation of component A：By the organopolysiloxane polymer in the preparing raw material of component A, inorganic filler and thixotropic agent
It is added in double screw extruder, the melt temperature of screw rod is 40~100 DEG C, and vacuum is 0.06~0.099MPa, and rotating speed is
250~600rpm, main frame electric current is 55~90A, by the mixture cooling after extrusion, obtains final product component A；
The preparation of component B：The silane multiple crosslinking agent, silane coupler and organotin catalysts are put into reactor
In, 70~140 DEG C are heated to, flow back 2~12h, discharging, and cooling obtains auxiliary agent B；By the organic poly- silicon in the preparing raw material of component B
Oxygen alkane polymer and inorganic filler are added in planetary mixer or high velocity dispersators, are sufficiently mixed, in 80~130 DEG C of temperature
Being vacuumized under degree carries out dehydration degassing, is subsequently cooled to less than 50 DEG C, adds the auxiliary agent B, in vacuum be 0.06~
0.099MPa, rotating speed obtain final product component B to be reacted 30~180 minutes under conditions of 10~800rpm；
The preparation of component C：By the organopolysiloxane polymer in the preparing raw material of component C, toner and organosilicon froth breaking
Agent is added in planetary mixer or high velocity dispersators, is sufficiently mixed, and is vacuumized at a temperature of 80~130 DEG C and is dehydrated
Degassing, is subsequently cooled to less than 50 DEG C, then the material that will be mixed is transferred to three-roll grinder and is ground, and obtains final product component C.
When above-mentioned multicomponent silicone sealant is used, component C, component A are added in component A：The part by weight of component C is
10~30:1, mixed in specific mixing plant；Component A is pressed again：The weight ratio of component B is 7~15:1 adds component B,
Be well mixed and deaeration in specific mixing plant, in room temperature or no more than 70 DEG C under conditions of solidify.
The multicomponent silicone sealant that the present invention is provided is bonded for doors and windows sealing, with advantages below：
1st, using multicomponent neutrality curing system, curing rate is fast, and solidification can not for multicomponent silicone sealant of the invention
Influenceed by ambient humidity, and there is good caking property to sash stuffs such as metal, glass, plastics, timber, and it is corrosion-free.
2nd, within the specific limits, curing rate can suitably be adjusted by the mixed proportion of appropriate adjustment each component, can be also led to
Cross appropriate heating and improve curing rate, can well meet door and window processing factory to the quick-setting demand of fluid sealant, can especially fit
Should be in the pipelining of door and window processing factory.
3rd, mix colours simple, the component C of the different toners of collocation addition, and the Different adding amount of component C is adjusted, can be conveniently
Shades of colour needed for being deployed into user.
4th, multicomponent silicone sealant of the invention caking property while possessing that curing rate is fast, toning facilitates is good, tool
There is good mechanical property, displacement capacity is up to 25 grades.
5th, application property is good, easily mixes, and is not likely to produce bubble during mixing；The adjustable extent of mixed proportion is larger, after mixing
Easily extrude.
Specific embodiment
Below in conjunction with specific embodiment to of the invention for the multicomponent silicone sealant of doors and windows sealing and its preparation side
Method is further described in detail.
Fluorosilicone antifoamant in following examples has Formulas I structure：
Wherein m is that 1~5, n is 10~1000.
Embodiment 1
The multicomponent silicone sealant of the present embodiment is made up of component A, component B and component C, the preparing raw material point of each component
Not following (in parts by weight)：
Component A：Viscosity for 12000mPa.s α, 90 parts of alpha, omega-dihydroxy polydimethyl siloxane, viscosity is 100mPa.s
10 parts of dimethicone, 100 parts of nm-class active calcium carbonate.
Component B：Viscosity for 1000mPa.s 4 parts of dimethicone, 2 parts of nm-class active calcium carbonate, 2 parts of powdered whiting,
Four 3 parts of butanone oximino silanes, 3 parts of two butanone oximino silane of dimethyl, 2 parts of gamma-aminopropyl-triethoxy-silane, γ-shrink is sweet
1 part of oily ether oxygen propyl trimethoxy silicane, 0.2 part of dibutyl tin laurate.
Component C：Viscosity is 6 parts of the dimethicone of 350mPa.s, 2 parts of carbon black, 2 parts of fluorosilicone antifoamant.
The preparation method of the multicomponent silicone sealant of the present embodiment is as follows：
The preparation of component A：By α, alpha, omega-dihydroxy polydimethyl siloxane, nm-class active calcium carbonate, dimethicone are through meter
It is added in double screw extruder after amount system accurate measurement, the melt temperature of screw rod is 70 DEG C, and vacuum is 0.095MPa, is turned
Speed is 400rpm, and main frame electric current is 75A, will be cooled down after the mixing after extrusion, obtains component A.
The preparation of component B：By four butanone oximino silanes, the butanone oximino silane of dimethyl two, gamma-aminopropyl-triethoxy silicon
Alkane, γ-glycidyl ether oxygen propyl trimethoxy silicane, dibutyl tin laurate are put into reactor by ormal weight, plus
To 110 DEG C, flow back heat 8h, discharging, cools down standby, prepared auxiliary agent B.
Dimethicone, nm-class active calcium carbonate, powdered whiting are added in high velocity dispersators by ormal weight,
It is sufficiently mixed, is cooled down after vacuumizing dehydration degassing 1h at 110 DEG C, when temperature of charge is cooled to less than 50 DEG C, adds above-mentioned helping
Agent B carries out chemical reaction 90 minutes under conditions of vacuum 0.09MPa, rotating speed 300rpm, and component B is obtained.
The preparation of component C：Dimethicone, carbon black, organic silicon defoamer are added to dispersion stirring at a high speed by ormal weight
In machine, it is sufficiently mixed, is cooled down after vacuumizing dehydration degassing 1h at 110 DEG C, then the material that will be mixed is transferred to three-roll grinder
Inside it is fully ground, prepares component C.
When using, component C, component A are added in component A：The weight ratio of component C is 10:1, in specific agitator
Mix；Component A is pressed again：The weight ratio of component B is 10:1 adds component B, is well mixed and deaeration in specific agitator,
Solidify under conditions of 23 DEG C.
Embodiment 2
The multicomponent silicone sealant of the present embodiment is made up of component A, component B and component C, the preparing raw material point of each component
Not following (in parts by weight)：
Component A：Viscosity is the α of 6000mPa.s, 100 parts of alpha, omega-dihydroxy polydimethyl siloxane, nm-class active calcium carbonate
80 parts, 40 parts of powdered whiting, 0.5 part of polyamide wax.
Component B：Viscosity is the α of 1500mPa.s, 12 parts of alpha, omega-dihydroxy polydimethyl siloxane, nm-class active calcium carbonate 8
Part, four 2 parts of butanone oximino silanes, 3 parts of vinyl tributyl ketoximyl silane, 3 parts of two butanone oximino silane of methyl ethylene, γ-
3 parts of aminopropyl trimethoxysilane, 1 part of epoxycyclohexyl triethoxysilane, 0.2 part of dibutyltin diacetate.
Component C：Viscosity is 8 parts of the dimethicone of 1000mPa.s, 3 parts of iron oxide red, 1 part of fluorosilicone antifoamant.
The preparation method of the multicomponent silicone sealant of the present embodiment is as follows：
The preparation of component A：It is alpha, omega-dihydroxy polydimethyl siloxane, nm-class active calcium carbonate, powdered whiting, poly- by α
Amide waxe is added in double screw extruder after metering system accurate measurement, and the temperature of screw melt is 60 DEG C, and vacuum is
0.090MPa, rotating speed is 500rpm, and main frame electric current is 60A, will be cooled down after the mixing after extrusion, obtains component A.
The preparation of component B：By four butanone oximino silanes, vinyl tributyl ketoximyl silane, the diacetylmonoxime of methyl ethylene two
Base silane, γ-aminopropyltrimethoxysilane, epoxycyclohexyl triethoxysilane, dibutyltin diacetate are thrown by ormal weight
Enter in reactor, be heated to 80 DEG C, flow back 8h, discharging, cool down standby, prepared auxiliary agent B.
α, alpha, omega-dihydroxy polydimethyl siloxane, nm-class active calcium carbonate are added in high velocity dispersators, fully
Mixing, 100 DEG C vacuumize dehydration degassing 1h after cool down, when temperature of charge is cooled to less than 50 DEG C, add above-mentioned auxiliary agent B in
Vacuum 0.09MPa, carries out chemical reaction 90 minutes under conditions of rotating speed 300rpm, component B is obtained.
The preparation of component C：Dimethicone, iron oxide red, organic silicon defoamer are added to dispersion at a high speed by ormal weight
In mixer, it is sufficiently mixed, is cooled down after vacuumizing dehydration degassing 2h at 90 DEG C, then the material that will be mixed is transferred to the grinding of three rollers
It is fully ground in machine, prepares component C.
When using, component C, component A are added in component A：The weight ratio of component C is 15:1, in specific agitator
Mix；Component A is pressed again：The weight ratio of component B is 14:1 adds component B, is well mixed and deaeration in specific agitator,
Solidify 30min under conditions of 50 DEG C, after under conditions of 23 DEG C solidify.
Embodiment 3
The multicomponent silicone sealant of the present embodiment is made up of component A, component B and component C, the preparing raw material point of each component
Not following (in parts by weight)：
Component A：Viscosity is trimethoxy 100 parts of the dimethyl silicone polymer of end-blocking of 20000mPa.s, nano active carbonic acid
70 parts of calcium, 50 parts of silicon powder, 0.6 part of polypropylene glycol.
Component B：Viscosity is 12 parts of the dimethicone of 12000mPa.s, 6 parts of nm-class active calcium carbonate, the diacetylmonoxime of phenyl three
4 parts of base silane, 3 parts of methyl ethylene two (N- methylacetamidos) silane, N- β-aminoethyl-gamma-aminopropyl-triethoxy silicon
3 parts of alkane, 1 part of epoxycyclohexyl triethoxysilane, 0.2 part of dibutyl tin double (beta-diketo-esters).
Component C：Viscosity is 10 parts of the dimethicone of 1000mPa.s, 2 parts of carbon black, orange 2 parts, fluorosilicone antifoamant 2
Part.
The preparation method of the multicomponent silicone sealant of embodiment is as follows：
The preparation of component A：Trimethoxy is blocked into dimethyl silicone polymer, nm-class active calcium carbonate, silicon powder, polyethers warp
It is added in double screw extruder after metering system accurate measurement, the melt temperature of screw rod is 60 DEG C, and vacuum is 0.085MPa,
Rotating speed is 350rpm, and main frame electric current is 70A, will be cooled down after the mixing after extrusion, obtains component A.
The preparation of component B：By phenyl tributanoximo silane, methyl ethylene two (N- methylacetamidos) silane, N-
β-aminoethyl-gamma-aminopropyl-triethoxy-silane, epoxycyclohexyl triethoxysilane, dibutyl tin double (beta-diketo-esters) are pressed
Ormal weight is put into reactor, is heated to 130 DEG C, and flow back 4h, discharging, cools down standby, prepared auxiliary agent B.
Dimethicone, nm-class active calcium carbonate are added in high velocity dispersators, are sufficiently mixed, taken out at 130 DEG C
Cooled down after vacuum dehydration degassing 1h, when temperature of charge is cooled to less than 50 DEG C, add above-mentioned auxiliary agent B in vacuum
0.095MPa, carries out chemical reaction 60 minutes under conditions of rotating speed 500rpm, component B is obtained.
The preparation of component C：Dimethicone, carbon black, orange, organic silicon defoamer are added to dispersion at a high speed by ormal weight
In mixer, it is sufficiently mixed, is cooled down after vacuumizing dehydration degassing 1h at 130 DEG C, then the material that will be mixed is transferred to three rollers and grinds
It is fully ground in grinding machine, prepares component C.
When using, component C, component A are added in component A：The weight ratio of component C is 20:1, in specific agitator
Mix；Component A is pressed again：The weight ratio of component B is 9:1 adds component B, is well mixed and deaeration in specific agitator,
Solidify 10min under conditions of 70 DEG C, after under conditions of 23 DEG C solidify.
Embodiment 4
The multicomponent silicone sealant of the present embodiment is made up of component A, component B and component C, the preparing raw material point of each component
Not following (in parts by weight)：
Component A：Viscosity is trimethoxy 100 parts of the dimethyl silicone polymer of end-blocking of 8000mPa.s, nm-class active calcium carbonate
110 parts, 0.2 part of organic bentonite.
Component B：Viscosity is trimethoxy 10 parts of the dimethyl silicone polymer of end-blocking of 4000mPa.s, nm-class active calcium carbonate 6
Part, four 4 parts of butanone oximino silanes, 1 part of vinyl tributyl ketoximyl silane, 2 parts of two butanone oximino silane of methyl ethylene, N- β-
3 parts of aminoethyl-γ-aminopropyltrimethoxysilane, 1 part of epoxycyclohexyl trimethoxy silane, the double (beta-diketons of dibutyl tin
Ester) 0.5 part.
Component C：Viscosity is 6 parts of the dimethicone of 4000mPa.s, 0.5 part of carbon black, 3 parts of ultramarine, fluorosilicone antifoamant
0.5 part.
The preparation method of the multicomponent silicone sealant of the present embodiment is as follows：
The preparation of component A：Trimethoxy is blocked into dimethyl silicone polymer, nm-class active calcium carbonate, organic bentonite warp
It is added in double screw extruder after metering system accurate measurement, the temperature of screw melt is 75 DEG C, and vacuum is 0.080MPa,
Rotating speed is 450rpm, and main frame electric current is 70A, will be cooled down after the mixing after extrusion, obtains component A.
The preparation of component B：By four butanone oximino silanes, vinyl tributyl ketoximyl silane, the butanone oximido silicon of dimethyl two
Double (the beta-diketons of alkane, N- β-aminoethyl-γ-aminopropyltrimethoxysilane, epoxycyclohexyl trimethoxy silane, dibutyl tin
Ester) put into reactor by ormal weight, 110 DEG C are heated to, flow back 4h, discharging, cools down standby, and auxiliary agent B is obtained.
Trimethoxy is blocked into dimethyl silicone polymer, nm-class active calcium carbonate and is added to dispersion stirring at a high speed by ormal weight
In machine, it is sufficiently mixed, is cooled down after vacuumizing dehydration degassing 2h at 110 DEG C, when temperature of charge is cooled to less than 50 DEG C, adds
State auxiliary agent B carries out chemical reaction 40 minutes under conditions of vacuum 0.090MPa, rotating speed 700rpm, and B component is obtained.
The preparation of component C：Dimethicone, carbon black, ultramarine, organic silicon defoamer are added to dispersion at a high speed by ormal weight
In mixer, it is sufficiently mixed, is cooled down after vacuumizing dehydration degassing 3h at 100 DEG C, then the material that will be mixed is transferred to three rollers and grinds
It is fully ground in grinding machine, prepares component C.
When using, component C, component A are added in component A：The weight ratio of component C is 10:1, in specific agitator
Mix；Component A is pressed again：The weight ratio of component B is 7:1 adds component B, is well mixed and deaeration in specific agitator,
Solidify under conditions of 15 DEG C.
The silicone sealant prepared to embodiment 1-4 is mixed in the ratio of each embodiment, by the solidification that each embodiment specifies
Condition is solidified, and hardness when hardness, solidification 24h, displacement level is tested after solidification 3d when testing surface drying time, solidification 3h respectively
Not, test result is as follows：
| Test index | Test foundation | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Surface drying time/min | GB/T 13477.5-2002 | 26 | 15 | 10 | 25 |
| Hardness during 3h | GB/T 531.1-2008 | 20 | 22 | 20 | 24 |
| Hardness during 24h | GB/T 531.1-2008 | 28 | 25 | 23 | 26 |
| Displacement rank | GB/T 14683-2003 | 25HM | 25HM | 25HM | 25HM |
From result in table, multicomponent silicone sealant surface drying speed of the invention consolidates speed quickly with just, 3 hours
Can be just solid, user can be met and move mobile hardness requirement.Rise on 3 hours only surfaces of existing single-component silicone fluid sealant
Skin, it is impossible to be cured to the hardness that can be moved, needs solidification to meet within 4-7 days requirement under the conditions of general environment, temperature is low or wet
Even the longer time is needed under the low condition of cure of degree.By contrast, multicomponent silicone sealant curing rate of the invention
With the obvious advantage, while having good mechanical property, displacement capacity is up to 25 grades.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously
Can not therefore be construed as limiting the scope of the patent.It should be pointed out that coming for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of multicomponent silicone sealant, it is characterised in that including component A, component B and component C, the component A with it is described
The weight ratio of component B is 7:1~15:1, the component A are 10 with the weight ratio of the component C:1~30:1；
The component A is prepared from by the raw material of following weight portion：
100 parts of organopolysiloxane polymer
60~150 parts of inorganic filler
0~5 part of thixotropic agent；
The component B is prepared from by the raw material of following weight portion：
The component C is prepared from by the raw material of following weight portion：
4~20 parts of organopolysiloxane polymer
0.5~5 part of organic silicon defoamer
0.1~15 part of toner；
The organopolysiloxane polymer is selected from dimethyl silicone polymer, the alkoxy end-capped poly dimethyl of terminal hydroxy group end-blocking
At least one in siloxanes, alkyl-blocked dimethyl silicone polymer；
The silane multiple crosslinking agent is that mass ratio is 1:3-3:1 crosslinking agent A and the composition of crosslinking agent B；The crosslinking agent A
Selected from methyl tributanoximo silane, vinyl tributyl ketoximyl silane, phenyl tributanoximo silane, four butanone oximido silicon
At least one in alkane, methyl tri acetylacetonate oximino silane；The crosslinking agent B is selected from the butanone oximino silane of methyl ethylene two, two
The butanone oximino silane of methyl two, the butanone oximino silane of aminomethyl phenyl two, the butanone oximino silane of diphenyl two, (the N- first of dimethyl two
Base acetylamino) silane, dimethyl two (N- ethylacetamidos) silane, methyl ethylene two (N- methylacetamidos) silicon
Alkane, methyl ethylene two (epsilon-caprolactams base) silane, aminomethyl phenyl two (N- methylacetamidos) silane, (N- of diphenyl two
Methylacetamido) at least one in silane.
2. multicomponent silicone sealant according to claim 1, it is characterised in that the organopolysiloxane polymer exists
Viscosity at 25 DEG C is 100~100000cp.
3. multicomponent silicone sealant according to claim 1, it is characterised in that the inorganic filler is selected from nano active
In calcium carbonate, powdered whiting, silicon powder, diatomite, kaolin, talcum powder, precipitated silica, fume colloidal silica extremely
Few one kind；And/or the thixotropic agent is selected from least in polyamide wax, polyethers, silane-modified polyethers and organic bentonite
Kind.
4. multicomponent silicone sealant according to claim 1, it is characterised in that the silane coupler is selected from chloropropyl
Trimethoxy silane, chloropropyl triethoxysilane, γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane,
N- β-aminoethyl-γ-aminopropyltrimethoxysilane, N- β-aminoethyl-gamma-aminopropyl-triethoxy-silane, N- β-aminoethyls-
γ-aminopropyltriethoxy dimethoxysilane, N- β-aminoethyl-γ-aminopropyltriethoxy diethoxy silane, γ-glycidol ether
Oxygen propyl trimethoxy silicane, γ-glycidoxypropyltrietandysilane andysilane, γ-glycidyl ether oxygen propyl methyl two
Methoxy silane, γ-glycidyl ether oxygen propyl methyldiethoxysilane, epoxycyclohexyl trimethoxy silane, epoxide ring
Hexyl triethoxysilane, 3- mercaptopropyl trimethoxysilanes, 3- mercaptopropyltriethoxysilanes, NCO propyl group front three
TMOS, NCO propyl-triethoxysilicane, 3- ureido-propyl trimethoxy silanes, 3- ureido-propyl triethoxies
At least one in silane.
5. multicomponent silicone sealant according to claim 1, it is characterised in that the organotin catalysts are selected from two vinegar
Sour dibutyl tin, dibutyl tin laurate, tin dilaurate dioctyl tin, stannous octoate, two neodecanoic acid stannous methides, dibutyl
At least one in tin double (beta-diketo-esters).
6. multicomponent silicone sealant according to claim 1, it is characterised in that the organic silicon defoamer is fluorine silica
Alkane.
7. multicomponent silicone sealant according to claim 1, it is characterised in that the toner be carbon black, titanium dioxide,
Zinc oxide, chrome yellow, cadmium yellow, iron oxide yellow, iron oxide red, cadmium red, molybdate red, ultramarine, cobalt blue, barba hispanica, phthalocyanine blue, phthalocyanine green,
At least one in cobalt green, chrome oxide green.
8. multicomponent silicone sealant according to claim 1, it is characterised in that the silane multiple crosslinking agent is quality
Than being 0.8-2.8:1 crosslinking agent A and the composition of crosslinking agent B；The crosslinking agent A be selected from vinyl tributyl ketoximyl silane,
At least one in phenyl tributanoximo silane and four butanone oximino silanes；The crosslinking agent B is selected from the fourth of methyl ethylene two
In ketoximinosilanes, the butanone oximino silane of dimethyl two and methyl ethylene two (N- methylacetamidos) silane at least one
Kind.
9. the multicomponent silicone sealant according to claim any one of 1-8, it is characterised in that the component A is by following
The raw material of weight portion is prepared from：
100 parts of organopolysiloxane polymer
100~120 parts of inorganic filler
0~0.6 part of thixotropic agent；
The component B is prepared from by the raw material of following weight portion：
The component C is prepared from by the raw material of following weight portion：
6~10 parts of organopolysiloxane polymer
0.5~2 part of organic silicon defoamer
2~4 parts of toner.
10. the preparation method of the multicomponent silicone sealant described in a kind of any one of claim 1-9, it is characterised in that including
Following steps：
The preparation of component A：Organopolysiloxane polymer in the preparing raw material of component A, inorganic filler and thixotropic agent are added
To in double screw extruder, the melt temperature of screw rod is 40~100 DEG C, and vacuum is 0.06~0.099MPa, rotating speed is 250~
600rpm, main frame electric current is 55~90A, by the mixture cooling after extrusion, obtains final product component A；
The preparation of component B：During the silane multiple crosslinking agent, silane coupler and organotin catalysts are put into reactor,
70~140 DEG C are heated to, flow back 2~12h, discharging, cooling obtains auxiliary agent B；By the organic poly- silica in the preparing raw material of component B
Alkane polymer and inorganic filler are added in planetary mixer or high velocity dispersators, are sufficiently mixed, in 80~130 DEG C of temperature
Under vacuumize and carry out dehydration degassing, be subsequently cooled to less than 50 DEG C, add the auxiliary agent B, in vacuum be 0.06~
0.099MPa, rotating speed obtain final product component B to be reacted 30~180 minutes under conditions of 10~800rpm；
The preparation of component C：Organopolysiloxane polymer in the preparing raw material of component C, toner and organic silicon defoamer are added
Enter in planetary mixer or high velocity dispersators, be sufficiently mixed, vacuumize that to carry out dehydration de- at a temperature of 80~130 DEG C
Gas, is subsequently cooled to less than 50 DEG C, then the material that will be mixed is transferred to three-roll grinder and is ground, and obtains final product component C.
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| CN108314990A (en) * | 2018-03-05 | 2018-07-24 | 广东阜和实业有限公司 | A kind of high-strength high temperature-resistant silicone sealant and preparation method thereof |
| CN108484803A (en) * | 2018-03-27 | 2018-09-04 | 浙江欧仁新材料有限公司 | A kind of silane-terminated polymer and moisture-curable adhesive compound prepared therefrom |
| CN108753198A (en) * | 2018-05-25 | 2018-11-06 | 株洲飞鹿高新材料技术股份有限公司 | A kind of silicone sealant adhesive accelerant and its preparation method and application is in the silicone sealant and preparation method thereof of non-fragment orbit |
| CN109722217A (en) * | 2019-01-24 | 2019-05-07 | 佛山市卡乐尔新材料有限公司 | A kind of preparation method of the color slurry of silicone adhesive |
| CN109777203A (en) * | 2019-01-24 | 2019-05-21 | 佛山市卡乐尔新材料有限公司 | A kind of preparation method of polyether modified silicone sealant mill base |
| CN110511596A (en) * | 2019-09-09 | 2019-11-29 | 青州宇信钙业股份有限公司 | A kind of silicone sealant high elongation rate composite Nano filler and preparation method thereof |
| CN110982272A (en) * | 2019-12-28 | 2020-04-10 | 深圳市旗盛科技有限公司 | A fill colloid for precious internal battery that charges is fixed |
| CN111057518A (en) * | 2019-12-31 | 2020-04-24 | 广州市白云化工实业有限公司 | Two-component silicone sealant for door and window seams and preparation method thereof |
| CN111218252A (en) * | 2020-01-15 | 2020-06-02 | 江苏明昊新材料科技股份有限公司 | Low-viscosity two-component sealant and preparation method thereof |
| CN114149767A (en) * | 2021-12-21 | 2022-03-08 | 宝美施化工(上海)有限公司 | Weather-resistant temperature-resistant inorganic silicone adhesive color paste and preparation method and application thereof |
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| CN108484803A (en) * | 2018-03-27 | 2018-09-04 | 浙江欧仁新材料有限公司 | A kind of silane-terminated polymer and moisture-curable adhesive compound prepared therefrom |
| CN108484803B (en) * | 2018-03-27 | 2020-07-31 | 浙江欧仁新材料有限公司 | Silane-terminated polymer and moisture-cured adhesive composition prepared from same |
| CN108753198A (en) * | 2018-05-25 | 2018-11-06 | 株洲飞鹿高新材料技术股份有限公司 | A kind of silicone sealant adhesive accelerant and its preparation method and application is in the silicone sealant and preparation method thereof of non-fragment orbit |
| CN109722217A (en) * | 2019-01-24 | 2019-05-07 | 佛山市卡乐尔新材料有限公司 | A kind of preparation method of the color slurry of silicone adhesive |
| CN109777203A (en) * | 2019-01-24 | 2019-05-21 | 佛山市卡乐尔新材料有限公司 | A kind of preparation method of polyether modified silicone sealant mill base |
| CN110511596A (en) * | 2019-09-09 | 2019-11-29 | 青州宇信钙业股份有限公司 | A kind of silicone sealant high elongation rate composite Nano filler and preparation method thereof |
| CN110982272A (en) * | 2019-12-28 | 2020-04-10 | 深圳市旗盛科技有限公司 | A fill colloid for precious internal battery that charges is fixed |
| CN111057518A (en) * | 2019-12-31 | 2020-04-24 | 广州市白云化工实业有限公司 | Two-component silicone sealant for door and window seams and preparation method thereof |
| CN111218252A (en) * | 2020-01-15 | 2020-06-02 | 江苏明昊新材料科技股份有限公司 | Low-viscosity two-component sealant and preparation method thereof |
| CN114149767A (en) * | 2021-12-21 | 2022-03-08 | 宝美施化工(上海)有限公司 | Weather-resistant temperature-resistant inorganic silicone adhesive color paste and preparation method and application thereof |
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