CN106633908A - Novel environment-friendly double component heat insulation silicone rubber and preparation method thereof - Google Patents
Novel environment-friendly double component heat insulation silicone rubber and preparation method thereof Download PDFInfo
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- CN106633908A CN106633908A CN201611217761.8A CN201611217761A CN106633908A CN 106633908 A CN106633908 A CN 106633908A CN 201611217761 A CN201611217761 A CN 201611217761A CN 106633908 A CN106633908 A CN 106633908A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/28—Glass
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- 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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
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Abstract
The invention provides a novel environment-friendly double component heat insulation silicone rubber and a preparation method thereof. The rubber is prepared from a component A and a component B. The component A comprises, by mass, 100 parts of hydroxy-terminated poly-dimethylsiloxane with the viscosity of 200cps-150000cps, 5-30 parts of hollow glass microspheres with the size of 10<=D50<=100, 1-40 parts of silica aerogel with the specific surface of larger than or equal to 300m2/g, and smaller than or equal to 1000me/g, 50-150 parts of incremental fillers and 1-10 parts of reinforcing fillers with the specific surface of smaller than or equal to 150m2/g. The component B comprises, by mass, 10-50 parts of crosslinking agent, 0.005-10 parts of catalyst, 5-100 parts of solvent and 0.1-50 parts of coupling agent. The novel environment-friendly double component heat insulation silicone rubber is not only environment-friendly, but also good in weatherproof property and thermal insulation property.
Description
Technical field
The present invention relates to silicone rubber art, more particularly to a kind of double-component adiabatic heat-insulation silicon rubber and preparation method thereof.
Background technology
According to equipment and pipeline heat-insulating technology general rule, heat-insulating material to be referred to and be equal to or less than 623K (350 in mean temperature
DEG C) when thermal conductivity less than 0.14W/ (mK) material.It is generally used to prevent heat power equipment and pipeline heat to scatter and disappear, or cold
Freeze and use under low temperature, thus be also called insulation or cold insulation material.Heat-insulating material species is various, and according to material inorganic material can be divided into
Material, high-molecular organic material and metal material.The fields such as building, metallurgy, chemical industry, oil, building materials, machinery are widely used in, in state
Occupy very important status in people's economy.
Zhengzhou University Yang Jiujun professors are more than 44 μm with the particle diameter of the separation and Extraction from flyash, and apparent density is more than
1.0g/m3Thick-wall hollow microballon be primary raw material, add appropriate alumina cement and polymeric aluminum as binding agent, produce not
Fly ash micro-sphere insulating brick is burnt, with low thermal conductivity, the features such as permanent Linear change rate is low, anti-seismic performance is good is heated.
University of Science ＆ Technology, Beijing Yang Hailong is taught with tetraethyl orthosilicate as silicon source, is combined using two step sol-gal processes overcritical
Dry technology prepares block flawless aerosil, and its bulk density is 50-300kg/m3, calorifics test surfaces,
Normal temperature and pressure lower volume density is 100kg/m3Sample thermal conductivity factor be 0.02W/ (mK).
Jia Mengqiu etc. adds hollow glass micropearl and hollow microsphere based on epoxy resin, be prepared for heat-proof quality and
Impervious excellent insulating moulding coating.Raouf etc. adds micron order fullerene thin film in heat insulating coatings, because it has absolutely
The characteristic of hot and high emissivity.Therefore, the coating has efficient heat-insulation and heat-preservation.U.S.'s shield (Thermo-shield)
Energy-saving coatings, contain many superfine ceramic bubbles in the coating, there is very high reflectivity to sunshine, and ceramic bubbles are tight after being dried
Arrangement form insulating.Shinkareva etc., as heat-insulated aggregate, will be prepared for good after hollow glass micro-ball nickel plating
Good heat-proof quality, the thermal insulation coatings of low resistivity.Nahar etc. has made intensive studies to the cooling technology of sunshine, as a result
It was found that the indoor temperature for measuring coating reflective coating is more much lower than the indoor temperature for being not coated with reflective coating.
However, existing heat-insulating material also has many deficiencies, for example, still lack that weatherability is excellent and more ring
The matrix material of guarantor, such as based on the use epoxy resin having, and the easy xanthochromia of epoxy resin, it is fragile under low temperature to split；Some uses
Acrylic emulsions do matrix, and acrylic-based products chemical toxicity is big, not environmentally, has injury to human body.
The content of the invention
The present invention is to make up the deficiencies in the prior art, there is provided a kind of novel environment friendly double-component adiabatic heat-insulation silicon rubber
Glue, not only environmental protection, and also weatherability is good, and insulation capacity is excellent.
The present invention is to reach its purpose, and the technical scheme of employing is as follows：
A kind of environmentally friendly double-component adiabatic heat-insulation silicon rubber, its formula includes component A and B component, wherein, the component A bag
Include the raw material of following mass parts：Viscosity is 100 parts of the hydroxyl-terminated injecting two methyl siloxane (PDMS) of 200cps-150000cps；10
Hollow glass micropearl (HG) 5-30 parts of≤D50≤100 micron；300m2/ g≤specific surface area≤1000m2/ g silica airsettings
Glue 1-40 parts；Extending fillers 50-150 parts；Specific surface area >=150m2Reinforced filling 1-10 parts of/g；The B component includes as follows
The raw material of mass parts：Crosslinking agent 10-50 parts；Catalyst 0.005-10 parts；Solvent 5-100 parts；Coupling agent 0.1-50 parts.
Environmental protection double-component adiabatic heat-insulation silicon rubber of the invention, preferred viscosities are the terminal hydroxy group poly- two of 200cps-150000cps
Methylsiloxane, if viscosity is less than 200cps, can cause crosslink density excessive and embrittlement occurs；Viscosity is higher than 150000cps, then
The coating that glue can be made is deteriorated.It is preferred that the hollow glass micropearl (HG) of 10 microns≤D50≤100 micron, if particle diameter is too little, can make
Adhesiveness increases, and loading is reduced；Particle diameter is too big, then the lustrous surface that can make glue is deteriorated.It is preferred that 300m2/ g≤specific surface area≤
1000m2The aerosil of/g, if specific surface area is too small, organic silica aerogel can not play its effect of heat insulation, specific surface
Product is excessive, then be difficult to be distributed in glue.It is preferred that specific surface area >=150m2The reinforced filling of/g, if specific surface area is too small can cause
Sedimentation, layering.The present invention can prepare a kind of not only environmental protection by such scheme, and weatherability is good, and insulation capacity is excellent
Novel environment friendly double-component adiabatic heat-insulation silicon rubber.
Preferably, the mass ratio of component A and B component is 8～12:1.
Preferably, the extending fillers are selected from least in kaolin, silicon powder, talcum powder, diatomite, Firebrake ZB
Kind；The particle diameter of the extending fillers is preferably 400-5000 mesh, more preferably kaolin, and preferable particle size is the height of 400-5000 mesh
Ridge soil can ensure that the loading of filler is larger, while will not settle.
Preferably, the crosslinking agent is selected from positive silicic acid propyl ester, tetraethyl orthosilicate, SI-40, SI-28, methyl trimethoxy epoxide silicon
At least one in alkane, MTES, vinyltrimethoxy silane, VTES.
Preferably, the catalyst selected from dibutyl tin laurate, dibutyltin diacetate, stannous octoate, two (12
Alkyl sulfide) dibutyl tin, titanium propanolate, butyl titanate or above-mentioned catalyst chelate at least one.
Preferably, the solvent is selected from least in dimethyldiethoxysilane, terminal methyl dimethyl silicone polymer
Kind.
Used as a kind of specific embodiment, the coupling agent is selected from gamma-aminopropyl-triethoxy-silane, γ-glycidol
Ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, N- (β-aminoethyl)-γ-aminopropyl
At least one in trimethoxy silane.
Used as a kind of specific embodiment, the reinforced filling is selected from aerosil, methyl MQ resins, vinyl MQ
At least one in resin, precipitated silica.
Used as a kind of preferred version, using silicon dioxide aerogel powder, its porosity is more than 90%, and aperture is in 30-
80nm, surface hydrophobicity.
Second aspect present invention provides a kind of preparation method of environmentally friendly double-component adiabatic heat-insulation silicon rubber mentioned above, bag
Include following steps：
1) each raw material of component A is added in mixer, is heated to 100 DEG C, vacuumized, keep vacuum be -0.07～-
0.12MPa, stirs 1-4 hours, is cooled to room temperature；
2) B component is added in mixer, is vacuumized, holding vacuum is -0.07～-0.12MPa, stirring 20-50 divides
Clock；
3) component A and B component are well mixed, vacuum defoamation.
The technical scheme that the present invention is provided, has the advantages that：
1st, the present invention is compounded according to a certain percentage using hollow glass micropearl and aerosil, can be effectively improved
The heat insulation effect of silicon rubber.
2nd, based on hydroxyl-terminated injecting two methyl siloxane of the present invention with viscosity as 200cps-150000cps material guarantor
Adiabator, not only environmental protection, and weather resistance is excellent, in a specific embodiment, can using 400cps, 500cps,
Resin based on the isoviscous hydroxyl-terminated injecting two methyl siloxane of 1000cps, 10000cps.
3rd, in optimization formula system of the invention, add the kaolin of specified particle diameter, good increment, hardening can be reached
Purpose.
4th, not only weatherability is good for environmentally friendly double-component adiabatic heat-insulation silicon rubber of the invention, and good heat insulating, its heat conduction
Coefficient is at 0.01-0.12W/ (mK)；And, the silicon rubber environmental protection of the present invention will not be damaged to human body.
Specific embodiment
Technical scheme is described further with reference to specific embodiment：
Embodiment 1
Component A：1000g 20000cps PDMS, 100g HG, 10g specific surface areas are added in double planetary mixer
400m2The aerosil of/g, 500g kaolin, 20g specific surface areas >=150m2The aerosil of/g.It is heated to
100 DEG C, vacuumize afterwards, keep vacuum -0.09MPa, revolve round the sun 45HZ, rotation 45HZ.Stir 2 hours in the above conditions,
Room temperature is cooled to afterwards, both.Aerosil used is provided for Guizhou Aerospace Wujiang Electro-Mechanical Equipment Co., Ltd.
Aerogel powder, porosity is greater than 90%, and aperture is in 30-80nm, surface hydrophobicity.
B component：Positive silicic acid propyl ester 200g is added in double planetary mixer；Dibutyl tin laurate 10g；Dimethyl two
Ethoxysilane 200g；20 parts of γ-aminopropyl triethoxysilane.Vacuumize, keep vacuum -0.09MPa, revolve round the sun 30HZ,
Rotation 10HZ, stirs 30 minutes and discharges, both.
Solidification：By component A and B component according to mass ratio 10:1 ratio is well mixed, and needs are coated on after vacuum defoamation
The material surface of insulation, primary solidification is complete after 24 hours.
In the present embodiment, the D50 of hollow glass micropearl material (HG) is 60 microns.The reference area of organic silica aerogel is
700m2/ g or so.Kaolinic particle diameter is 1000 mesh.
After testing, the thermal conductivity factor after solidification is：0.07W/(m·K).
Embodiment 2
Component A：1000g 20000cps PDMS, 200g HG, 10g specific surface areas are added in double planetary mixer
300m2The aerosil of/g, 500g kaolin, 20g specific surface areas >=150m2The aerosil of/g.It is heated to
100 DEG C, vacuumize afterwards, keep vacuum -0.09MPa, revolve round the sun 45HZ, rotation 45HZ.Stir 2 hours in the above conditions,
Room temperature is cooled to afterwards, both.Aerosil used is provided for Guizhou Aerospace Wujiang Electro-Mechanical Equipment Co., Ltd.
Aerogel powder, porosity is greater than 90%, and aperture is in 30-80nm, surface hydrophobicity.
B component：Positive silicic acid propyl ester 200g is added in double planetary mixer；Dibutyl tin laurate 10g；Dimethyl two
Ethoxysilane 200g；20 parts of gamma-aminopropyl-triethoxy-silane.Vacuumize, keep vacuum -0.09MPa, revolve round the sun 30HZ,
Rotation 10HZ, stirs 30 minutes and discharges, both.
Solidification：By component A and B component according to mass ratio 10:1 ratio is well mixed, and needs are coated on after vacuum defoamation
The material surface of insulation, primary solidification is complete after 24 hours.
In the present embodiment, the D50 of hollow glass micropearl material (HG) is 45 microns.The reference area of organic silica aerogel is
500m2/ g or so.Kaolinic particle diameter is 600 mesh.
After testing, the thermal conductivity factor after solidification is：0.05W/(m·K).
Embodiment 3
Component A：1000g 20000cps PDMS, 200g HG, 100g specific surface areas are added in double planetary mixer
350m2The aerosil of/g, 500g kaolin, 20g specific surface areas >=150m2The aerosil of/g.It is heated to
100 DEG C, vacuumize afterwards, keep vacuum -0.09MPa, revolve round the sun 45HZ, rotation 45HZ.Stir 2 hours in the above conditions,
Room temperature is cooled to afterwards, both.Aerosil used is provided for Guizhou Aerospace Wujiang Electro-Mechanical Equipment Co., Ltd.
Aerogel powder, porosity is greater than 90%, and aperture is in 30-80nm, surface hydrophobicity.
B component：Positive silicic acid propyl ester 200g is added in double planetary mixer；Dibutyl tin laurate 10g；Dimethyl two
Ethoxysilane 200g；20 parts of γ-aminopropyl triethoxysilane.Vacuumize, keep vacuum -0.09MPa, revolve round the sun 30HZ,
Rotation 10HZ, stirs 30 minutes and discharges, both.
Solidification：By component A and B component according to mass ratio 10:1 ratio is well mixed, and needs are coated on after vacuum defoamation
The material surface of insulation, primary solidification is complete after 24 hours.
In the present embodiment, the D50 of hollow glass micropearl material (HG) is 20 microns.The reference area of organic silica aerogel is
900m2/ g or so.Kaolinic particle diameter is 2000 mesh.
After testing, the thermal conductivity factor after solidification is：0.01W/(m·K).
Comparative example 1
Component A：1000g 20000cps PDMS, 710g kaolin, 20g specific surface areas are added in double planetary mixer
150m2The aerosil of/g.100 DEG C are heated to, are vacuumized afterwards, keep vacuum -0.09MPa, revolve round the sun 45HZ, rotation
45HZ.Stir 2 hours in the above conditions, room temperature is cooled to afterwards, both.
B component：Positive silicic acid propyl ester 200g is added in double planetary mixer；Dibutyl tin laurate 10g；Dimethyl two
Ethoxysilane 200g；20 parts of γ-aminopropyl triethoxysilane.Vacuumize, keep vacuum -0.09MPa, revolve round the sun 30HZ,
Rotation 10HZ, stirs 30 minutes and discharges, both.
Solidification：By component A and B component according to mass ratio 10:1 ratio is well mixed, and needs are coated on after vacuum defoamation
The material surface of insulation, primary solidification is complete after 24 hours.
Thermal conductivity factor after solidification：0.21W/(m·K).
Comparative example 2
Component A：1000g 20000cps PDMS, 710g silicon powders, 20g specific surface areas are added in double planetary mixer
150m2/ g aerosils.100 DEG C are heated to, are vacuumized afterwards, keep vacuum -0.09MPa, revolve round the sun 45HZ, rotation
45HZ.Stir 2 hours in the above conditions, room temperature is cooled to afterwards, both.
B component：Positive silicic acid propyl ester 200g is added in double planetary mixer；Dibutyl tin laurate 10g；Dimethyl two
Ethoxysilane 200g；20 parts of γ-aminopropyl triethoxysilane.Vacuumize, keep vacuum -0.09MPa, revolve round the sun 30HZ,
Rotation 10HZ, stirs 30 minutes and discharges, both.
Solidification：By component A and B component according to mass ratio 10:1 ratio is well mixed, and needs are coated on after vacuum defoamation
The material surface of insulation, primary solidification is complete after 24 hours.
Thermal conductivity factor after solidification：0.33W/(m·K).
From above-mentioned experiment, the silicon rubber insulation capacity that the present invention is provided is excellent, and its weatherability is good.Jing is examined
Survey, under the product normal temperature environment after hardening of the present invention, possess the weather resistance of at least 20 years.
The above, is only presently preferred embodiments of the present invention, and any pro forma restriction is not done to the present invention, therefore
All contents without departing from technical solution of the present invention, any simply repair according to the technical spirit of the present invention to made for any of the above embodiments
Change, equivalent variations and modification, still fall within the range of technical solution of the present invention.
Claims (10)
1. a kind of novel environment friendly double-component adiabatic heat-insulation silicon rubber, it is characterised in that its formula includes component A and B component,
Wherein, the component A includes the raw material of following mass parts：Viscosity is the terminal hydroxy group poly dimethyl of 200cps-150000cps
100 parts of siloxanes；Hollow glass micropearl 5-30 parts of 10≤D50≤100 micron；300m2/ g≤specific surface area≤1000m2/ g's
Aerosil 1-40 parts；Extending fillers 50-150 parts；Specific surface area >=150m2Reinforced filling 1-10 parts of/g；
The B component includes the raw material of following mass parts：Crosslinking agent 10-50 parts；Catalyst 0.005-10 parts；Solvent 5-100 parts；
Coupling agent 0.1-50 parts.
2. novel environment friendly double-component adiabatic heat-insulation silicon rubber according to claim 1, it is characterised in that component A and B component
Mass ratio be 8-12:1.
3. environmentally friendly double-component adiabatic heat-insulation silicon rubber according to claim 1, it is characterised in that the extending fillers are selected from
At least one in kaolin, silicon powder, talcum powder, diatomite, Firebrake ZB；The particle diameter of the extending fillers is preferably 400-
5000 mesh.
4. novel environment friendly double-component adiabatic heat-insulation silicon rubber according to claim 1, it is characterised in that the crosslinking agent choosing
From positive silicic acid propyl ester, tetraethyl orthosilicate, SI-40, SI-28, MTMS, MTES, vinyl
At least one in trimethoxy silane, VTES.
5. novel environment friendly double-component adiabatic heat-insulation silicon rubber according to claim 1, it is characterised in that the catalyst choosing
From dibutyl tin laurate, dibutyltin diacetate, stannous octoate, two (dodecyl sulphur) dibutyl tins, titanium propanolate, titanium
At least one in the chelate of acid butyl ester or above-mentioned catalyst.
6. novel environment friendly double-component adiabatic heat-insulation silicon rubber according to claim 1, it is characterised in that the solvent is selected from
At least one in dimethyldiethoxysilane, terminal methyl dimethyl silicone polymer.
7. novel environment friendly double-component adiabatic heat-insulation silicon rubber according to claim 1, it is characterised in that the coupling agent choosing
From gamma-aminopropyl-triethoxy-silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl group
At least one in trimethoxy silane, N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane.
8. novel environment friendly double-component adiabatic heat-insulation silicon rubber according to claim 1, it is characterised in that the reinforced filling
At least one in aerosil, methyl MQ resins, vinyl MQ resin, precipitated silica.
9. novel environment friendly double-component adiabatic heat-insulation silicon rubber according to claim 1, it is characterised in that the silica
Aeroge is powder, and porosity is more than 90%, and aperture is in 30-80nm, surface hydrophobicity.
10. the preparation method of the novel environment friendly double-component adiabatic heat-insulation silicon rubber described in any one of claim 1-9, its feature exists
In comprising the steps：
1) each raw material of component A is added in mixer, is heated to 95-105 DEG C, vacuumized, keep vacuum be -0.07～-
0.1MPa, stirs 1-4 hours, is cooled to room temperature；
2) B component is added in mixer, is vacuumized, holding vacuum is -0.07～-0.1MPa, stirs 20-50 minutes；
3) component A and B component are well mixed, vacuum defoamation.
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| CN107141531A (en) * | 2017-05-27 | 2017-09-08 | 徐文忠 | A kind of aeroge composite adiabatic rubber and plastic and preparation method thereof |
| CN107236450A (en) * | 2017-05-18 | 2017-10-10 | 广州城建职业学院 | Environmentally friendly silastic material of a kind of insulating energy-saving and preparation method thereof |
| CN109266212A (en) * | 2018-09-07 | 2019-01-25 | 西安宙通新材料科技有限公司 | A kind of low density and high performance thermal protective coating |
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| CN115895436A (en) * | 2022-11-14 | 2023-04-04 | 湖南航天三丰科工有限公司 | Insulating coating material and preparation method thereof |
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| CN107141531A (en) * | 2017-05-27 | 2017-09-08 | 徐文忠 | A kind of aeroge composite adiabatic rubber and plastic and preparation method thereof |
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Application publication date: 20170510 |