CN109486198A - A kind of high-density fire-proof silicone adhesive and its preparation process - Google Patents

A kind of high-density fire-proof silicone adhesive and its preparation process Download PDF

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Publication number
CN109486198A
CN109486198A CN201811444199.1A CN201811444199A CN109486198A CN 109486198 A CN109486198 A CN 109486198A CN 201811444199 A CN201811444199 A CN 201811444199A CN 109486198 A CN109486198 A CN 109486198A
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parts
powder
silicone adhesive
fire
density fire
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CN201811444199.1A
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王存富
王艳超
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Shenzhen Dongxin Silicon Material Co Ltd
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Shenzhen Dongxin Silicon Material Co Ltd
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Priority to CN201811444199.1A priority Critical patent/CN109486198A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions 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; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • C08K2003/2272Ferric oxide (Fe2O3)
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/006Additives being defined by their surface area
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of high-density fire-proof silicone adhesive and its preparation process, the raw material including following parts by weight: 95-108 parts of base rubber, 0-30 parts of plasticizer, 50-300 parts of flakey powder, 0-150 parts of non-reinforcement powder, 0-100 parts of reinforced filling, 0.01-20 parts of crosslinking agent, 0-5 parts of coupling agent and 0.0001-10 parts of catalyst.This product raw material sources are extensive, this product uses flakey powder, and flakey powder has high temperature resistant, acid and alkali-resistance, the low feature of moisture permeability, different mutual laminated arrangements can be formed after additive amount appropriate, and then high temperature or flame is prevented to penetrate, and reach fire-retardant purpose, under mating reaction by flakey powder and remaining raw material, also there is good radiation hardness, fire protecting performance, production cost is low, has wide prospect of the application in the case where without using fireproof powder and metal powder.

Description

A kind of high-density fire-proof silicone adhesive and its preparation process
Technical field
The present invention relates to rubber materials, specifically a kind of high-density fire-proof silicone adhesive.
Background technique
As people's lives are more and more intelligent, demand of the people to electricity is also more and more, and power plant is also more and more, Substation is more and more, and the accumulation regions apart from people are also increasingly closer.Electromagnetism ionising radiation is more and more, and people are to anti-spoke of preventing fires It is also higher and higher to penetrate requirement.
Fire-proof silicone rubber is a kind of people's commonly radiation proof material, it uses zinc borate, magnesium hydroxide, hydroxide Aluminium, nitrogen system, phosphorus system, the compound system of nitrogen phosphorus, halogen-containing flame retardant, Sb system fire retardant, rare earth oxide etc., independent or several fireproof powders Compound action, by fire retardant decompose generate aqueous vapor, two vaporized carbons, non-inflammable gas or powder can prevent further to fire It burns, or captures the burn free radical generated or several fire retardant cooperative flame retardants etc. and achieve the purpose that prevent burning.Fire prevention silicone rubber Glue is to improve radiation resistance by improving density, and in order to improve density, mostly uses metal powder such as, iron powder, zinc powder, aluminium Powder, lead powder, the specific gravity such as tungsten powder larger substances increase density.
Although existing fire-proof silicone rubber can reach fire protection requirement by fireproof powder, exist not environmentally, it is resistance to The disadvantages of warm nature is bad, and resistance to acid and alkali is bad, generates toxic gas or solid when decomposition, expensive;These metal powders are easy It is oxidized to bulk shape oxide and then influences silicone adhesive performance or be more toxic, expensive, this is all the use band of people Inconvenience is carried out.
Summary of the invention
The purpose of the present invention is to provide a kind of high-density fire-proof silicone adhesives, to solve mentioned above in the background art ask Topic.
To achieve the above object, the invention provides the following technical scheme:
A kind of high-density fire-proof silicone adhesive, the raw material including following parts by weight: 95-108 parts of base rubber, 0-30 parts of plasticizer, 50-300 parts of flakey powder, 0-150 parts of non-reinforcement powder, 0-100 parts of reinforced filling, 0.01-20 parts of crosslinking agent, coupling agent 0- 5 parts and catalyst 0.0001-10 parts.
As a further solution of the present invention: base rubber includes any one in 107 glue and vinylsiloxane rubber.
As a further solution of the present invention: plasticizer includes but is not limited to 201 silicone oil and aliphatic ester.
As a further solution of the present invention: reinforced filling includes gas-phase silica, precipitated silica and nanometer calcium carbonate In any one, flakey powder includes any one in micaceous iron oxide, sericite in powder and hexagonal boron nitride, non-reinforcement Powder includes any one in silica flour, coarse whiting and aluminium oxide.
As a further solution of the present invention: crosslinking agent includes containing hydrogen silicone oil, alkoxy silane, containing ketoximinosilanes and third Any one in ketone type silane.
As a further solution of the present invention: coupling agent includes aminopropyl triethoxysilane, glycidol ether oxygroup third Base trimethoxy silane, methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, three ethoxy of vinyl Base silane, mercapto propyl front three (second) oxysilane, N- β-(aminoethyl)-γ-aminopropyltriethoxy triethoxysilane and N- β-(ammonia Ethyl) any one in-γ-aminopropyltriethoxy dimethoxysilane.
As a further solution of the present invention: catalyst includes platinum catalyst, tin compound, titanium compound, zirconium chemical combination Any one in object, aluminium compound and peroxide.
The preparation process of the high-density fire-proof silicone adhesive, the specific steps are as follows:
Step 1 disperses base rubber, plasticizer, flakey powder, non-reinforcement powder and reinforced filling in blender Even, then between 100-160 degrees Celsius of temperature, the negative 0.1MPa of vacuum degree is 1-3 hours low to taking off between negative 0.05MPa, obtains First mixture;
After the first mixture is cooled to room temperature, then crosslinking agent, coupling agent and catalyst is added in step 2 thereto, The negative 0.1MPa of vacuum degree is packed after being filtered using metal screen to deaeration between negative 0.05MPa to get finished product is arrived.
Compared with prior art, the beneficial effects of the present invention are: this product raw material sources are extensive, by flakey powder with Under the mating reaction of remaining raw material, also there is good radiation hardness, fire protecting performance in the case where not using fireproof powder and metal powder, Production cost is low, has wide prospect of the application.
Specific embodiment
The technical solution of the patent is explained in further detail With reference to embodiment.
Embodiment 1
A kind of one-component condensed type silicone rubber with high-density fire-proof, the raw material including following parts by weight: 107 glue 100 parts, 5 parts of 201 silicone oil, 150 parts of micaceous iron oxide, 80 parts of silica flour, 5 parts of gas-phase silica, 10 parts of crosslinking agent, aminopropyl three 1.5 parts and 0.1 part of catalyst of Ethoxysilane.Crosslinking agent includes methyl tributanoximo silane and vinyl tributanoximo silicon The mass ratio of alkane, methyl tributanoximo silane and vinyl tributyl ketoximyl silane is 4:1.
The viscosity of 107 glue is 8000CS, and the weight fraction of hydroxyl is 0.06%, and the viscosity of 201 silicone oil is 500CS, mica The partial size of iron oxide is -1000 mesh of 10 mesh, and the partial size of silica flour is 10-10000 mesh, and the specific surface area of gas-phase silica is 150 Meters squared per gram.
107 glue, 201 silicone oil, micaceous iron oxide and silica flour are uniformly dispersed in blender, then taken the photograph in temperature 135 Between family name's degree, the negative 0.08MPa of vacuum degree takes off low 2 hours, obtains the first mixture, after the first mixture is cooled to room temperature, then Crosslinking agent, aminopropyl triethoxysilane and catalyst are added thereto and uses metal screen in the negative 0.1MPa deaeration of vacuum degree It is packed after filtering to get finished product is arrived.
Embodiment 2
A kind of one-component condensed type silicone rubber with high-density fire-proof, the raw material including following parts by weight: 107 glue 100 parts, 10 parts of 201 silicone oil, 120 parts of micaceous iron oxide, 50 parts of silica flour, 100 parts of nanometer calcium carbonate, methyltrimethylsilane 8 Part, 1.5 parts of glycidyl ester oxy propyl trimethoxysilane and 0.4 part of catalyst.
The viscosity of 107 glue is 8000CS, and the weight fraction of hydroxyl is 0.06%, and the viscosity of 201 silicone oil is 500CS, mica The partial size of iron oxide is -1000 mesh of 10 mesh, and the partial size of silica flour is 10-10000 mesh, and the partial size of nanometer calcium carbonate is that 40-60 is micro- Rice.
107 glue, 201 silicone oil, micaceous iron oxide, nanometer calcium carbonate and silica flour are uniformly dispersed in blender, then Between 150 degrees Celsius of temperature, the negative 0.05MPa of vacuum degree takes off low 3 hours, obtains the first mixture, and the first mixture is cooling To after room temperature, then methyltrimethylsilane, glycidyl ester oxy propyl trimethoxysilane and catalyst are added thereto, The negative 0.07MPa deaeration of vacuum degree is packed after being filtered using metal screen to get finished product is arrived.
Embodiment 3
A kind of two-component condensed type silicone rubber with high-density fire-proof, the raw material including following parts by weight: 107 glue 100 parts, 5 parts of 201 silicone oil, 100 parts of micaceous iron oxide, 80 parts of silica flour, 0.5 part of gas-phase silica, 30 parts of tetraethoxysilane, 20 parts and 0.1 part of catalyst of coupling agent.Coupling agent includes three second of glycidyl ester oxy propyl trimethoxysilane and aminopropyl The mass ratio of oxysilane, glycidyl ester oxy propyl trimethoxysilane and aminopropyl triethoxysilane is 1:1.
The viscosity of 107 glue is 750CS, and the weight fraction of hydroxyl is 0.2%, and the viscosity of 201 silicone oil is 350CS, mica oxygen The partial size for changing iron is -1000 mesh of 10 mesh, and the partial size of silica flour is 10-10000 mesh.
107 glue, 201 silicone oil, micaceous iron oxide, gas-phase silica and silica flour are uniformly dispersed in blender, then It is taken off low 2.6 hours in the negative 0.08MPa of vacuum degree, is cooled to room temperature, is packed after being filtered using metal screen, obtain component A;By four Ethoxysilane, coupling agent and catalyst are uniformly mixed and are filtered using metal screen, are packed, are obtained B component.
Application method: component A and B component are uniformly mixed with the ratio of weight ratio 20:1 or 10:1, that is, can be used.
Embodiment 4
A kind of dual composition addition type silicone rubber with high-density fire-proof, the raw material including following parts by weight: vinyl 100 parts of silicon rubber, 5 parts of 201 silicone oil, 100 parts of micaceous iron oxide, 100 parts of silica flour, 0.5 part of gas-phase silica, containing hydrogen silicone oil 30 Part and 0.1 part of catalyst.
The viscosity of vinylsiloxane rubber is 350CS, and the weight fraction of hydroxyl is 0.5%, and the viscosity of 201 silicone oil is 350CS, The partial size of micaceous iron oxide is -1000 mesh of 10 mesh, and the partial size of silica flour is 10-10000 mesh.
Vinylsiloxane rubber, 201 silicone oil, micaceous iron oxide, gas-phase silica and silica flour are dispersed in blender It is even, it is then taken off low 2.6 hours in the negative 0.08MPa of vacuum degree, is cooled to room temperature, be added 0.1 part of catalyst, use metal screen mistake It is packed after filter, obtains component A;
Vinylsiloxane rubber, 201 silicone oil, micaceous iron oxide, gas-phase silica and silica flour are uniformly dispersed in blender, Then it is taken off low 2.6 hours in the negative 0.08MPa of vacuum degree, is cooled to room temperature, containing hydrogen silicone oil is added and is uniformly mixed and uses metal Strainer filtering, packaging, obtains B component.
Application method: component A and B component are uniformly mixed with the ratio of weight ratio 1:1, that is, can be used.
Comparative example 1
Comparative example 1 and embodiment 1, which are distinguished, to be micaceous iron oxide to be changed into common black iron oxide, remaining is identical.
Comparative example 2
Comparative example 2 and embodiment 4, which are distinguished, to be micaceous iron oxide to be changed into common black iron oxide, remaining is identical.
The product of the product of embodiment 1-4 and comparative example 1-2 are subjected to flame retardant rating test and radiation protection test, test knot Fruit is shown in Table 1.
Table 1
Flame retardant rating Shielding property
Embodiment 1 V0 It is excellent
Embodiment 2 V0 It is excellent
Embodiment 3 V0 It is excellent
Embodiment 4 V0 It is excellent
Comparative example 1 V1 It is good
Comparative example 2 V1 It is good
From table 1 it follows that the product of embodiment 1-4 is better than comparative example 1- in flame retardant property and shielding property 2 product shows that product of the invention has good fire-retardant and shielding property.
Flakey powder is three-dimensional laminated structure, and such as sericite in powder, micaceous iron oxide etc. itself has high temperature resistant, acidproof Alkali, moisture permeability bottom feature can form different mutual laminated arrangements after additive amount appropriate, and then prevent high temperature water gas Through reaching fire-retardant purpose;Flakey powder also has in the case where making this product not use the above fireproof powder and metal powder Good radiation hardness, fire protecting performance, production cost are low.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art The other embodiments being understood that.

Claims (8)

1. a kind of high-density fire-proof silicone adhesive, which is characterized in that the raw material including following parts by weight: 95-108 parts of base rubber, plasticising 0-30 parts of agent, 50-300 parts of flakey powder, 0-150 parts of non-reinforcement powder, 0-100 parts of reinforced filling, crosslinking agent 0.01-20 Part, 0-5 parts of coupling agent and 0.0001-10 parts of catalyst.
2. high-density fire-proof silicone adhesive according to claim 1, which is characterized in that the base rubber includes 107 glue and ethylene Any one in base silicon rubber.
3. high-density fire-proof silicone adhesive according to claim 1, which is characterized in that the plasticizer includes but is not limited to 201 silicone oil and aliphatic ester.
4. high-density fire-proof silicone adhesive according to claim 1 or 3, which is characterized in that the reinforced filling includes gas phase Any one in white carbon black, precipitated silica and nanometer calcium carbonate, flakey powder include micaceous iron oxide, sericite in powder and Any one in hexagonal boron nitride, non-reinforcement powder includes any one in silica flour, coarse whiting and aluminium oxide.
5. high-density fire-proof silicone adhesive according to claim 1, which is characterized in that the crosslinking agent include containing hydrogen silicone oil, Alkoxy silane, containing any one in ketoximinosilanes and acetone type silane.
6. high-density fire-proof silicone adhesive according to claim 1 or 2, which is characterized in that the coupling agent includes aminopropyl Triethoxysilane, glycidyl ether oxypropyltrimethoxysilane, methacryloxypropyl trimethoxy silane, second Alkenyl triethoxysilane, vinyltriethoxysilane, mercapto propyl front three (second) oxysilane, N- β-(aminoethyl)-γ-ammonia Any one in hydroxypropyl methyl triethoxysilane, N- β-(aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane.
7. high-density fire-proof silicone adhesive according to claim 1, which is characterized in that the catalyst includes platinum catalysis Any one in agent, tin compound, titanium compound, zirconium compounds, aluminium compound and peroxide.
8. a kind of preparation process of the high-density fire-proof silicone adhesive as described in claim 1-7, which is characterized in that specific steps are such as Under:
Base rubber, plasticizer, flakey powder, non-reinforcement powder and reinforced filling are uniformly dispersed, so by step 1 in blender Afterwards between 100-160 degrees Celsius of temperature, the negative 0.1MPa of vacuum degree is 1-3 hours low to taking off between negative 0.05MPa, and it is mixed to obtain first Close object;
After the first mixture is cooled to room temperature, then crosslinking agent, coupling agent and catalyst is added, in vacuum in step 2 thereto Negative 0.1MPa is spent to deaeration between negative 0.05MPa, is packed after being filtered using metal screen to get finished product is arrived.
CN201811444199.1A 2018-11-29 2018-11-29 A kind of high-density fire-proof silicone adhesive and its preparation process Pending CN109486198A (en)

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CN113493673A (en) * 2020-03-19 2021-10-12 佛山市顺德区天采有机硅有限公司 Flame-retardant silicone sealant and preparation method thereof
CN114854204A (en) * 2022-06-29 2022-08-05 广东高士高科实业有限公司 Room-temperature vulcanized silicone rubber and preparation method and application thereof
CN116083042A (en) * 2023-02-09 2023-05-09 天合光能股份有限公司 Double-component organic silicon pouring sealant and application thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113493673A (en) * 2020-03-19 2021-10-12 佛山市顺德区天采有机硅有限公司 Flame-retardant silicone sealant and preparation method thereof
CN114854204A (en) * 2022-06-29 2022-08-05 广东高士高科实业有限公司 Room-temperature vulcanized silicone rubber and preparation method and application thereof
CN116083042A (en) * 2023-02-09 2023-05-09 天合光能股份有限公司 Double-component organic silicon pouring sealant and application thereof

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Application publication date: 20190319