CN105441019B - A kind of low-density ketoxime removing type silicone sealant and preparation method thereof - Google Patents
A kind of low-density ketoxime removing type silicone sealant and preparation method thereof Download PDFInfo
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/32—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof from compositions containing microballoons, e.g. syntactic foams
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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
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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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
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
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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
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Abstract
The invention discloses a kind of low-density ketoxime removing type silicone sealant, the fluid sealant is grouped as by the group of following parts by weight：100 parts of α, ω dialkyl polydimethylsiloxane, 1~40 part of dimethicone, 0.1~4 part of thermal expansivity microcapsules, 1~25 part of crosslinking agent, 20~180 parts of reinforced filling, 0.01~5 part of coupling agent, 0.005~1 part of catalyst.The invention also discloses a kind of preparation methods of low-density ketoxime removing type silicone sealant.There is product of the present invention good mechanical property and adhesive property, product density to significantly reduce, and foaming effect is good, and stability is high.Preparation method of the present invention is simple for process, and equipment is conventional, implementation easy to operation, is conducive to industrial amplification production.
Description
Technical field
The present invention relates to a kind of low-density ketoxime removing type silicone sealants and preparation method thereof, belong to organosilicon downstream product
Synthesis field.
Background technology
Silicone sealant is a kind of organic silicon product, using hydroxy-end capped polysiloxanes as primary raw material, is aided with crosslinking
Agent, filler, plasticizer, coupling agent, catalyst mix under vacuum conditions.Silicone sealant at room temperature by with air
In water generation should be formed by curing elastic silicone rubber.Silicone sealant is easy to use, and cured glue body cubical contraction is small, sealing
Property it is good, bonding force is strong, and tensile strength is big, and with good resistance to ag(e)ing, resistant of high or low temperature, resistance to electrical insulating property, resistance to flexion
Property, weatherability etc., are widely used in the new high-tech industries such as building, automobile, machinery, electronics, weaving field.
According to the difference of crosslinking agent used, silicone sealant can be divided into depickling type, ketoxime removing type, dealcoholized type, de- amine type,
Multiple and different kinds such as de amide type, de- ketone type.Wherein, ketoxime removing type silicone sealant is due to nontoxic, odorless, adhesive property
Well, surface drying time is short, curingprocess rate is fast, comprehensive performance is strong, and corrosivity is less than depickling type and de- amine type, and storage stability is better than de-
Alcohol type is developing progressively as the maximum ketone seal gum product of current dosage, and people pay close attention to it and study also more and more.
Chinese patent CN101586018A discloses a kind of expanded silicone fireproof seal gum and its manufacturing method, the sealing
The starting material formula of glue is by weight：A, 30~60 parts of alpha, omega-dihydroxy polysiloxanes, 1~10 part of coupling agent, filler 30~
90 parts, 1~10 part of thixotropic agent, 10~50 parts of fire retardant, 1~10 part of crosslinking agent, 1~10 part of tackifier, catalytic curing agent 0.1~
5 parts, 1~10 part of foaming agent.The invention fluid sealant fire retardant performance is good, adhesive property disclosure satisfy that requirement, to base material
Corrosivity is small, excellent combination property, has foam performance, can play the role of better seal.In that patent, using foaming
In ammonium polyphosphate, intumescent phosphate monoammonium, intumescent phosphate diamines, the foam performance of these foaming agents is slightly worse for agent, system
Fluid sealant density is big, heavy, be not easy to very much store and transport, production and transport is of high cost.
Chinese patent CN102766420A discloses a kind of environmental protection type sealing adhesive, and it is micro- to contain hollow glass in the fluid sealant
The grain size of pearl, the hollow glass micropearl is 0.01~500 μm, and density is 0.1~1.2g/cm3, wall thickness be its diameter 6~
12%.The invention environmental protection type sealing adhesive proportion is compared with light, fillibility is good, dispersibility is excellent, VOC is low, particularly suitable for building, vapour
Vehicle, field of electronics.The hollow glass micropearl that the invention uses have density is low, size is small, self-lubricating, non-ignitable, heat-insulated, nothing
The advantages that malicious, can play the role of reducing density and even bubble in fluid sealant.But hollow glass micro-ball is a kind of inorganic crystalline substance
Body, its own weight is slightly larger, and reducing degree for the density of fluid sealant has certain limitations；And hollow glass micro-ball brittleness is big, warp
It crosses and stirs or be easy to happen rupture after rolling, the cullet after rupture, which just cannot achieve, to be improved mechanical property, reduce density and again
The effect of amount, stability are poor.
Therefore, it is close how to research and develop the ketoxime removing type silicone that a kind of foaming effect is good, fluid sealant density is low, Simultaneous Stabilization is high
Sealing is those skilled in the art's urgent problem to be solved.
Invention content
To solve the above problem of the existing technology, the purpose of the present invention is to provide a kind of low-density ketoxime removing type silicon
Ketone seal gum, the fluid sealant have lower density and weight, and foaming effect is good, and stability is high, easy to process.
To achieve the above object, the technical solution adopted in the present invention is：
A kind of low-density ketoxime removing type silicone sealant, is grouped as by the group of following parts by weight：
| α, alpha, omega-dihydroxy polydimethyl siloxane | 100 parts |
| Dimethicone | 1~40 part |
| Thermal expansivity microcapsules | 0.1~4 part |
| Crosslinking agent | 1~25 part |
| Reinforced filling | 20~180 parts |
| Coupling agent | 0.01~5 part |
| Catalyst | 0.005~1 part |
It is preferred that being grouped as by the group of following parts by weight：
| α, alpha, omega-dihydroxy polydimethyl siloxane | 100 parts |
| Dimethicone | 1~30 part |
| Thermal expansivity microcapsules | 0.1~2 part |
| Crosslinking agent | 2~20 parts |
| Reinforced filling | 50~150 parts |
| Coupling agent | 0.05~3 part |
| Catalyst | 0.01~0.5 part |
The viscosity of the α, alpha, omega-dihydroxy polydimethyl siloxane are 10~50mpas；The dimethicone 350~
500pa·s；The reinforced filling is that stearic acid modified calcium carbonate is passed through on surface.
The thermal expansivity microcapsules are that loose this microsphere F series low-temperature expansion types or loose this microsphere F series medium temperatures are swollen
Swollen type.This microsphere of pine F series low-temperature expansion types are selected from F-20, F-30, F-36LV, F-36, F-48；Described this microballoon of pine
Body F series medium temperature intumescents are selected from F-50, F-78K, F-79, F-80S, F-82.
The crosslinking agent is methyl tributanoximo silane, vinyl tributyl ketoximyl silane, phenyl tributanoximo silicon
The mixture of one or both of alkane, four butanone oximino silanes；
The coupling agent is γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-methacryl
Oxygroup propyl trimethoxy silicane, γ-(2,3- glycidyl) propyl trimethoxy silicane, isocyanate group propyl triethoxy
One or both of silane mixes；
The catalyst dibutyltin dilaurylate, dibutyltin diacetate, tin dilaurate dioctyl tin and two acetic acid two
The mixture of one or both of normal-butyl tin.
A kind of preparation method of low-density ketoxime removing type silicone sealant, includes the following steps：
A：By α, alpha, omega-dihydroxy polydimethyl siloxane, dimethicone, thermal expansivity microcapsules, reinforced filling press than
It puts into planet stirring kettle and is stirred after example mixing, in 120~150 DEG C of temperature, vacuum degree -0.09~-0.1MPa conditions
2~4h of lower mixing；It is to be mixed uniformly after be passed through N2, vacuum is released, base-material is obtained；
B：Crosslinking agent is added into base-material according to the ratio, is mixed in the case where vacuum degree -0.09~-0.1MPa, temperature are less than 70 DEG C
20~40min it is to be mixed uniformly after be passed through N2, release vacuum；
C：Coupling agent and catalyst are added into step B resulting materials according to the ratio, in vacuum degree -0.09~-0.1MPa, temperature
Degree, which is less than at 70 DEG C, mixes 20~40min, is passed through N2, vacuum is released to get low-density ketoxime removing type silicone sealant product, is pressed
Package encapsulation is carried out according to packing specification.
The beneficial effects of the invention are as follows：
The present invention provides a kind of low-density ketoxime removing type silicone sealants to be prepared by being adjusted to amounts of components
Obtain low-density fluid sealant.The present invention is added thermal expansivity microcapsules and is used as foaming agent, and thermal expansivity microcapsules are a kind of
Nucleocapsid, shell are thermoplastic acrylic resin Type of Collective object, and kernel is the hollow ball-shape microparticle of alkanes gas composition,
Microsphere volume after foaming temperature range heating, which can expand rapidly, increases to itself 8~10 times, the stability of dilation dimension
By force, foaming effect is very good.After thermal expansivity microcapsule expansion, larger volume is occupied, the interior alkanes gas filled
Weight very little, to significantly reduce the density of fluid sealant.Thermal expansivity microcapsules expand but not during preparing fluid sealant
Rupture, do not discharge kernel gas, in the case that the shell for stirring or rolling microcapsules have good toughness and ductility, one
As rupture will not occur cause to lose its effect, simplify processing technology, stability is high.Thermal expansivity microcapsules are light-weight, swollen
Swollen volume is big, therefore only needs that slight amount is added, you can and it obtains good foam performance and reduces the effect of fluid sealant density, at
This is cheap, economical and practical.The diameter of thermal expansivity microcapsules is between 5~50 μm, density and other recipe ingredients of fluid sealant
The similar density of mixture, thus it is more uniform when being mixed, it is not susceptible to settle；The shell of thermal expansivity microcapsules is
Crylic acid resin polymer is significantly higher than hollow glass microbead and fluid sealant component with the compatibility of other components in fluid sealant
Compatibility, the adhesive property of silicone sealant is ensured while reducing density.
To raw material α, the viscosity of alpha, omega-dihydroxy polydimethyl siloxane and dimethicone has all carried out further the present invention
It limits.The viscosity of both raw materials all has an impact the property of reaction preparation process and fluid sealant finished product.With α, ω-
The increase of dialkyl polydimethylsiloxane viscosity can make strand elongated, and terminal hydroxy group is reduced, crosslinking points are reduced, fluid sealant
Intensity and elongation increase；But viscosity, which crosses conference, reduces its mobile performance.The viscosity of dimethicone is less than normal to be easy to happen migration,
Moving to surface layer influences caking property, and viscosity is bigger than normal not to have plasticization.But silicone sealant is an entirety, Suo Youyuan
Material is reacted under given conditions, and the product of function admirable is finally just made；In the reaction system, exist between various raw materials
It interacts and affects one another and restrict, not individualism.In the fluid sealant system of the present invention, work as α, alpha, omega-dihydroxy poly- two
The optimum viscosity of methylsiloxane is 10~50mpas, the optimum viscosity of dimethicone is 350~500pas, uses this
Silicone sealant performance prepared by the raw material of sample viscosity is very good.
It is simple for process the present invention also provides a kind of preparation method of low-density ketoxime removing type silicone sealant, if
Standby conventional, implementation easy to operation is conducive to industrial amplification production.
Specific implementation mode
Below by specific embodiment, invention is further described in detail, but embodiment is not the scope of the present invention
Limitation.
In the examples below that, used thermal expansivity microcapsule product F-48, F-50, F-78K are purchased from this loose oil
Fat Pharmaceutical Co., Ltd, remaining raw material are commercial product.
Embodiment 1
A kind of low-density ketoxime removing type silicone sealant, is grouped as by the group of following parts by weight：
| α, alpha, omega-dihydroxy polydimethyl siloxane | 100g |
| Dimethicone | 25g |
| Thermal expansivity microcapsules F-48 | 0.3g |
| Vinyl tributyl ketoximyl silane (crosslinking agent) | 2g |
| Methyl tributanoximo silane (crosslinking agent) | 15g |
| Modified CaCO3(reinforced filling) | 80g |
| Gamma-aminopropyl-triethoxy-silane (coupling agent) | 2g |
| Dibutyl tin laurate (catalyst) | 0.2g |
The preparation method of the low-density ketoxime removing type silicone sealant is：
A, by the α that 100g viscosity is 30mpas, alpha, omega-dihydroxy polydimethyl siloxane, 25g viscosity are 400pas's
Dimethicone, 0.3g thermal expansivity microcapsules F-48,80g are modified CaCO3It puts into planet stirring kettle and is stirred after mixing
It mixes, mixes 3h under the conditions of 120 DEG C of temperature of control, vacuum degree -0.1MPa, then pass to N2, vacuum is released, base-material is obtained；
B, 2g vinyl tributyl ketoximyl silanes, 15g methyl tributanoximo silanes are added into base-material, vacuumizes, very
Vacuum mixes 30min under the conditions of reciprocal of duty cycle -0.1MPa, 65 DEG C of temperature；Then pass to N2, release vacuum；
C, 2g gamma-aminopropyl-triethoxy-silanes and 0.2g dibutyl tin laurates are added into step B resulting materials,
It vacuumizes, 30min is mixed under the conditions of vacuum degree -0.095MPa, 65 DEG C of temperature；Then pass to N2, vacuum is released, it will be obtained low
Density fluid sealant carries out package encapsulation according to packing specification.
Embodiment 2
A kind of low-density ketoxime removing type silicone sealant, is made of following component：
| A, alpha, omega-dihydroxy polydimethyl siloxane | 100g |
| Dimethicone | 10g |
| Thermal expansivity microcapsules F-50 | 0.5g |
| Methyl tributanoximo silane (crosslinking agent) | 12g |
| Modified CaCO3(reinforced filling) | 100g |
| γ-(2,3- glycidyl) propyl trimethoxy silicane (coupling agent) | 1.6g |
| Dibutyl tin laurate (catalyst) | 0.3g |
The preparation method of the low-density ketoxime removing type silicone sealant is：
A, by the α that 100g viscosity is 40mpas, alpha, omega-dihydroxy polydimethyl siloxane, 10g viscosity are 500pas's
Dimethicone, 0.5g thermal expansivity microcapsules F-50,100g are modified CaCO3It puts into planet stirring kettle and is stirred after mixing
It mixes, mixes 3h under the conditions of 130 DEG C of temperature of control, vacuum degree -0.098MPa, then pass to N2, vacuum is released, base-material is obtained；
B, 12g methyl tributanoximo silanes are added into base-material, vacuumize, in vacuum degree -0.098MPa, temperature 60 C
Under the conditions of vacuum mix 40min；Then pass to N2, release vacuum；
C, 1.6g γ-(2,3- glycidyl) propyl trimethoxy silicane and 0.3g bis- are added into step B resulting materials
Dibutyl tin laurate vacuumizes, and mixes 30min under the conditions of vacuum degree -0.098MPa, temperature 60 C, is passed through N2, release true
Low-density fluid sealant obtained is carried out package encapsulation by sky according to packing specification.
Embodiment 3
A kind of low-density ketoxime removing type silicone sealant, is made of following component：
| A, alpha, omega-dihydroxy polydimethyl siloxane | 100g |
| Dimethicone | 20g |
| Thermal expansivity microcapsules F-78K | 0.4g |
| Vinyl tributyl ketoximyl silane (crosslinking agent) | 2g |
| Methyl tributanoximo silane (crosslinking agent) | 8g |
| Modified CaCO3(reinforced filling) | 120g |
| Gamma-aminopropyl-triethoxy-silane (coupling agent) | 2.4g |
| Tin dilaurate dioctyl tin (catalyst) | 0.4g |
The preparation method of the low-density ketoxime removing type silicone sealant is：
A, by the α that 100 parts of viscosity are 20mpas, alpha, omega-dihydroxy polydimethyl siloxane, 20g viscosity are 450pas
Dimethicone, 0.4g thermal expansivity microcapsules F-78K, 120g be modified CaCO3Put into after mixing in planet stirring kettle into
Row stirs, and mixes 3h under the conditions of 140 DEG C of temperature of control, vacuum degree -0.099MPa, then passes to N2, vacuum is released, base-material is obtained；
B, 2g vinyl tributyl ketoximyl silanes, 8g methyl tributanoximo silanes are added into base-material, vacuumizes, vacuum
30min is mixed under the conditions of degree -0.099MPa, 55 DEG C of temperature, then passes to N2, release vacuum；
C, 2.4g gamma-aminopropyl-triethoxy-silanes and 0.4g tin dilaurate dioctyls are added into step B resulting materials
Tin mixes 30min under the conditions of vacuum degree -0.099MPa, 55 DEG C of temperature, is passed through N2, vacuum is released, low-density obtained is close
Sealing carries out package encapsulation according to packing specification.
Embodiment 4
The present embodiment is comparative example 1, does not add thermal expansivity microcapsule foamer；It is made of following component：
Specifically preparation process is：
A, by the α that 100g viscosity is 20mpas, alpha, omega-dihydroxy polydimethyl siloxane, 20g viscosity are 400pas's
Dimethicone, 120gCaCO3It puts into planet stirring kettle and is stirred after mixing in proportion, control 140 DEG C of temperature, vacuum
3h is mixed under the conditions of degree -0.099MPa, mixture is passed through N after mixing2, vacuum is released, base-material is obtained；
B：Then tetra- butanone oximino silanes of 3g, 8g methyl tributanoximo silanes are added according to the ratio, vacuumizes mixing 30min
It is passed through N again afterwards2, vacuum is released, base-material is obtained；
C：Continue to add silane 0.7g γ-bis- bay of methacryloxypropyl trimethoxy silane and 0.3g according to the ratio
Sour dioctyl tin mixes 30min under the conditions of vacuum degree -0.099MPa, is passed through N2, vacuum is released, low-density obtained is sealed
Glue carries out package encapsulation according to packing specification.
Embodiment 5
The present embodiment is comparative example 2, and hollow glass microbead is added as foaming agent.
The raw material, raw material dosage and preparation method of the present embodiment are essentially identical with comparative example 1, difference lies in：It uses
Grain size is the hollow glass microbead of 80~100um as foaming agent, addition 15g.
Ketoxime removing type fluid sealant prepared by 1~embodiment of above-described embodiment 5 is respectively labeled as S-1~S-3, D-1, D-
2.The said goods are taken to measure its hardening time, tensile strength, elongation at break, hardening time and density respectively, wherein stretching strong
Degree and elongation at break are measured by GB/T528-2009, and density uses density bottle method, are measured by GJB77B-2005.
Test result is shown in Table 1.
1 silicone sealant performance test data of table
Can be seen that the D-1 products that foaming agent is not added by above-mentioned data, tensile strength and elongation at break all with
The product of the present embodiment S-1~S-3 is not much different, but its density is significantly higher；The averag density of S-1~S-3 products is only
0.84g/cm3, and the density of D-1 products is up to 1.4g/cm3, the density re-duction rate of product of the present invention reaches 35.7% or more, effect
Fruit is very notable.D-2 products using hollow glass microbead as foaming agent, density close to S-1~S-3 products, but its
Stretching is slight, these mechanical properties of elongation at break are poor, and the tensile strength of D-2 is only the 58.4% of S-3 tensile strengths, breaks
Split elongation is only S-2 products 80.6%.Compared with D-1, D-2 product, product of the present invention ensure product mechanical property and
On the basis of adhesive property, product density is significantly reduced, improves foaming effect, maintains good stability, usability
It can be excellent.
Above-described embodiment is used for illustrating the present invention, rather than limits the invention, in the claims in the present invention
Protection domain in, to any modifications and changes for making of the present invention, both fall within protection scope of the present invention.
Claims (5)
1. a kind of low-density ketoxime removing type silicone sealant, it is characterised in that be grouped as by the group of following parts by weight：
The thermal expansivity microcapsules are loose this microsphere F series low-temperature expansion types or loose this microsphere F series medium temperature intumescents；
This microsphere of pine F series low-temperature expansion types are selected from F-20, F-30, F-36LV, F-36, F-48；Pine this microsphere F systems
Row medium temperature intumescent is selected from F-78K, F-79, F-80S, F-82.
2. a kind of low-density ketoxime removing type silicone sealant as described in claim 1, it is characterised in that by following parts by weight
Group is grouped as：
3. such as a kind of low-density ketoxime removing type silicone sealant of claims 1 or 2 any one of them, it is characterised in that：It is described
The viscosity of α, alpha, omega-dihydroxy polydimethyl siloxane are 10~50MPas；The viscosity of the dimethicone be 350~
500Pa·s；The reinforced filling is that stearic acid modified calcium carbonate is passed through on surface.
4. such as a kind of low-density ketoxime removing type silicone sealant of claims 1 or 2 any one of them, it is characterised in that：It is described
Crosslinking agent is methyl tributanoximo silane, vinyl tributyl ketoximyl silane, phenyl tributanoximo silane, four butanone oximidos
The mixture of one or both of silane；
The coupling agent is γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-methacryloxy
Propyl trimethoxy silicane, γ-(2,3- glycidyl) propyl trimethoxy silicane, isocyanate group propyl-triethoxysilicane
One or both of mixing；The catalyst dibutyltin dilaurylate, dibutyltin diacetate, tin dilaurate dioctyl tin
One or both of mixture.
5. a kind of preparation method of such as claims 1 or 2 any one of them low-density ketoxime removing type silicone sealant, feature
It is to include the following steps：
A：By α, alpha, omega-dihydroxy polydimethyl siloxane, dimethicone, thermal expansivity microcapsules, reinforced filling mix in proportion
It puts into planet stirring kettle and is stirred after conjunction, under the conditions of 120~150 DEG C of temperature of control, vacuum degree -0.09~-0.1MPa
Mix 2~4h；It is to be mixed uniformly after be passed through N2, release vacuum, obtain base-material；
B：Crosslinking agent is added into base-material according to the ratio, vacuum degree -0.09~-0.1MPa, temperature be less than 70 DEG C at mixing 20~
40min it is to be mixed uniformly after be passed through N2, release vacuum；
C：Coupling agent and catalyst are added into step B resulting materials according to the ratio, it is small in vacuum degree -0.09~-0.1MPa, temperature
20~40min is mixed at 70 DEG C, is passed through N2, releases vacuum to get low-density ketoxime removing type silicone sealant product, according to packet
It fills specification and carries out package encapsulation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511025884.7A CN105441019B (en) | 2015-12-30 | 2015-12-30 | A kind of low-density ketoxime removing type silicone sealant and preparation method thereof |
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| JP6699743B2 (en) * | 2016-09-21 | 2020-05-27 | 信越化学工業株式会社 | Organopolysiloxane composition for resin adhesive oil seal and oil seal for automobile |
| CN106520060A (en) * | 2016-10-28 | 2017-03-22 | 广东长鹿精细化工有限公司 | Neutral oxime-type silicone sealant and preparation method thereof |
| CN106633908A (en) * | 2016-12-26 | 2017-05-10 | 广州市高士实业有限公司 | Novel environment-friendly double component heat insulation silicone rubber and preparation method thereof |
| CN107201170B (en) * | 2017-05-23 | 2019-07-09 | 广东阜和实业有限公司 | A kind of silicone sealant and preparation method thereof containing microcapsules |
| CN107652942A (en) * | 2017-10-24 | 2018-02-02 | 山东永安胶业有限公司 | High extrudability silicone sealant of low-density and preparation method thereof |
| CN108084955B (en) * | 2017-12-20 | 2021-05-28 | 中天东方氟硅材料有限公司 | Single-component self-leveling silicone sealant composition for concrete joint, sealant and preparation method of sealant |
| CN110117477A (en) * | 2018-02-06 | 2019-08-13 | 上杭鑫昌龙实业有限公司 | Silicone sealant and preparation method thereof |
| CN109401725A (en) * | 2018-11-28 | 2019-03-01 | 东莞兆舜有机硅科技股份有限公司 | A kind of new-energy automobile high thermal conductivity encapsulating silicon rubber |
| CN110079267A (en) * | 2019-04-29 | 2019-08-02 | 山东飞度胶业科技股份有限公司 | It is a kind of can porcelainization insulation two-component silicone foam glue and preparation method thereof |
| CN111286300B (en) * | 2020-04-01 | 2022-03-25 | 运研材料科技（上海）有限公司 | Room temperature vulcanized silicone rubber and preparation method and application thereof |
| CN111574950B (en) * | 2020-06-08 | 2022-02-01 | 韦尔通(厦门)科技股份有限公司 | Ultra-soft silane modified polyether adhesive with buffering performance and preparation method thereof |
| CN111892905A (en) * | 2020-08-06 | 2020-11-06 | 广州汇纳新材料科技有限公司 | Anti-settling high-hardness single-component room temperature vulcanized silicone rubber for encapsulation and preparation method thereof |
| CN111944476B (en) * | 2020-08-25 | 2022-05-17 | 广州市白云化工实业有限公司 | Low-modulus two-component ketoxime-removing type organosilicon sealant and preparation method thereof |
| CN114058325A (en) * | 2021-11-17 | 2022-02-18 | 湖北兴发凌志新材料有限公司 | Low-specific-gravity high-strength silicone sealant |
| CN114907814B (en) * | 2022-06-10 | 2024-05-17 | 浙江中天东方氟硅材料股份有限公司 | Foaming ceramic heat-insulating fireproof silicone sealant and preparation method thereof |
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| CN103305140A (en) * | 2012-03-13 | 2013-09-18 | 日东电工株式会社 | Heat-resistance pressure-sensitive adhesive tape for semiconductor device production and method for producing semiconductor device by using heat-resistance pressure-sensitive adhesive tape |
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| FR2770220B1 (en) * | 1997-10-29 | 2003-01-31 | Rhodia Chimie Sa | CROSSLINKABLE SILICONE COMPOSITION IN ADHESIVE GEL AND SHOCK ABSORBER WITH MICROSPHERES |
| JP6378501B2 (en) * | 2014-03-05 | 2018-08-22 | 日東電工株式会社 | Adhesive sheet |
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| CN103305140A (en) * | 2012-03-13 | 2013-09-18 | 日东电工株式会社 | Heat-resistance pressure-sensitive adhesive tape for semiconductor device production and method for producing semiconductor device by using heat-resistance pressure-sensitive adhesive tape |
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Address after: 324000 No. 20 Huayin North Road, Quzhou City, Zhejiang Province, China Patentee after: Zhongtian Oriental Fluorosilicone Material Co., Ltd. Address before: 324000 incubator building of Quzhou High-tech Industrial Park, Zhejiang Province Patentee before: Zhejiang Zhongtian Fluorine Silicon Materials Co., Ltd. |
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Address after: 324000 No. 20 Huayin North Road, Quzhou City, Zhejiang Province, China Patentee after: Zhejiang Zhongtian Dongfang fluorosilicone Material Co.,Ltd. Address before: 324000 No. 20 Huayin North Road, Quzhou City, Zhejiang Province, China Patentee before: ZHONGTIAN DONGFANG FLUORINE SILICON MATERIAL Co.,Ltd. |