CN110003655A - A kind of preparation method of silicon rubber base aeroge composite insulation material - Google Patents
A kind of preparation method of silicon rubber base aeroge composite insulation material Download PDFInfo
- Publication number
- CN110003655A CN110003655A CN201910154099.3A CN201910154099A CN110003655A CN 110003655 A CN110003655 A CN 110003655A CN 201910154099 A CN201910154099 A CN 201910154099A CN 110003655 A CN110003655 A CN 110003655A
- Authority
- CN
- China
- Prior art keywords
- parts
- obtains
- silicon rubber
- insulation material
- room temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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
- C08L83/04—Polysiloxanes
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- 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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
-
- 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
-
- 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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of preparation methods of silicon rubber base aeroge composite insulation material, belong to new material technology field.The present invention uses ZrO_2 aerogel for raw material, prepare silicon rubber base aeroge composite insulation material, since the aperture of ZrO_2 aerogel is less than the mean free path of air molecule, porosity is high, volume ratio shared by solid is low, large specific surface area keeps the thermal conductivity of aeroge very low, can be improved the insulation effect of heat-insulating material.The present invention receives powder by adding nano silica, prepare silicon rubber base aeroge composite insulation material, nano grade silica particles purity is high, density is low, large specific surface area, good dispersion and nontoxic and pollution-free, due in nano grade silica particles pore-size be less than or close in air molecule mean free path, have the characteristics that no convective heat transfer and heat transfer are all very small, the thermal conductivity that material can be effectively reduced in nano grade silica particles is added in heat-insulating material, improves the heat insulation and preservation effect of heat-insulating material.
Description
Technical field
The present invention relates to a kind of preparation methods of silicon rubber base aeroge composite insulation material, belong to new material technology neck
Domain.
Background technique
All-glass paper is the widely used heat-insulating material in deep cooling Cryo Heat Insulation, is usually used as vacuum multi-layer
Interval insulant in insulation uses, and glass fibre sheathing paper plays vital work to the heat insulation of multiple layer heat insulation structure
With.With the continuous popularization of Cryo Heat Insulation technical application, more requirements also proposed to the performance of thermally insulated container；Especially as liquid
This kind of latent heat of vaporization of nitrogen, liquid hydrogen is small, the cryogenic liquid of low boiling point, requires the heat-insulating property of storage-transport vessel very high.In order to as far as possible
Cryogenic liquid is reduced in storage and the loss in transmission process, improves efficiency of storage, it is necessary to improve the thermal insulation of heat-barrier material
Energy.The multilayer heat insulation low temperature storage-transport vessel overwhelming majority of domestic production uses this material of glass fibre sheathing paper for spacer,
And demand is big, and the specific gravity for accounting for entire production is very big, high production cost.
At present cryogenic liquid storage-transport vessel and its substantially used with circuits ordinary packing insulation and vacuum insulation two major classes.
Vacuum insulation is divided into again: high-vacuum insulation, vacuum fiber (powder isolation), high vacuum multiple layer heat insulation, high vacuum multi shields insulation, more
Layer insulation etc., wherein vacuum fiber (powder isolation) is common, and vacuum fiber insulation is divided into organic fiber and inorfil again.Have
Machine fiber uses polyester fiber, and high temperature resistant is poor, easily shrinks, and around burning, area is big, and inorfil glass fabric, there is also cloth covers
Thickness > 0.1mm, fiber is thick and generates drawbacks, the powder isolation materials such as evaporative power under vacuum is big and there is the combustion of easily flowing and material
Inherent shortcoming is heated, application field is restricted, and service life is short.
According to document and related data, domestic more advanced common sheathing paper can only produce thickness > 0.06mm reluctantly
Ultra-fine fibre glass sheathing paper, and, base weight lower sheathing paper thinner for requiring, then be difficult to control, it is difficult to wind, paper rises
Wrinkle is serious, and the uniformity cannot ensure, tension intensity is even more to be unable to satisfy user's requirement.Due to low-temperature pressure container ectonexine gap
It is limited, and the installation requirement that insulating paper cannot be less than 50 layers is wound, to constrain the infiltration and development of low-temperature pressure container.Mesh
Preceding common thermal insulation material has polyurethane foam heat insulation material, polyvinyl chloride thermal insulation material and simple glass, heat-preservation cotton etc., still
The specific surface area of above-mentioned thermal insulation material is smaller, therefore thermal coefficient is big, and heat insulation effect is limited, cannot function as Cryogenic Thermal Insulating Materials
It uses.
Novel heat insulation material is researched and developed, bigger profit can be obtained to help enterprise to reduce cost；It can rise simultaneously
To effect that is energy saving, reducing environmental pollution.The development and popularization of the heat-insulating material of economical and efficient are steamed to cryogenic liquid is reduced
Hair, it is energy saving significant.
Summary of the invention
The technical problems to be solved by the invention: it is smaller for the specific surface area of existing thermal insulation material, therefore thermally conductive system
Number is big, and the limited problem of heat insulation effect provides a kind of preparation method of silicon rubber base aeroge composite insulation material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) by methyl silicone rubber, phenyl siloxane rubber, ZrO_2 aerogel, phenolic resin be placed in vacuum kneader premix 20 ~
30min obtains premix；
(2) nano silica, the short fibre of aramid fiber, zinc oxide, stearic acid, iron oxide are added in premix, in two-roll mill
On plasticate 30 ~ 40min, must plasticate mixture；
(3) vinyl triamine, sulphur addition are plasticated in mixture, the room temperature vulcanization 22 ~ for 24 hours on vulcanizing press obtains silicon rubber
Matrix aeroge composite insulation material.
The methyl silicone rubber, phenyl siloxane rubber, ZrO_2 aerogel, nano silica, phenolic resin, aramid fiber
Short fibre, zinc oxide, stearic acid, iron oxide, vinyl triamine, the parts by weight of sulphur are 50 ~ 70 parts of methyl silicone rubbers, 30 ~ 50 parts
Phenyl siloxane rubber, 20 ~ 30 parts of ZrO_2 aerogels, 15 ~ 20 parts of nano silicas, 10 ~ 15 parts of phenolic resin, 5 ~ 10 parts of virtues
The short fibre of synthetic fibre, 3 ~ 5 parts of zinc oxide, 1 ~ 3 part of stearic acid, 1 ~ 3 part of iron oxide, 3 ~ 5 parts of vinyl triamines, 2 ~ 4 parts of sulphur.
The molecular weight of methyl silicone rubber described in step (1) is 34000 ~ 36000, and the molecular weight of phenyl siloxane rubber is
43000~45000。
The length of the short fibre of aramid fiber described in step (2) be 2 ~ 4mm, 6 ~ 7 μm of diameter.
The specific preparation step of ZrO_2 aerogel described in step (1) are as follows:
(1) dehydrated alcohol is added in deionized water, 15 ~ 20min is stirred with 50 ~ 100r/min revolving speed under room temperature, it is molten to obtain ethyl alcohol
Liquid；
(2) zirconium chloride is added in ethanol solution, 40 ~ 50min is stirred with 150 ~ 200r/min revolving speed under room temperature, obtains four chlorinations
Zirconium ethanol solution；
(3) by ethylenediamine tetra-acetic acid be added zirconium chloride ethanol solution in, under room temperature with 100 ~ 150r/min revolving speed stirring 30 ~
40min obtains chelating liquid；
(4) first phthalein amine is added in chelating liquid, 30 ~ 40min is stirred with 150 ~ 200r/min revolving speed under room temperature, obtains mechanism liquid；
(5) propylene oxide is added in mechanism liquid, 15 ~ 20min is stirred with 150 ~ 200r/min revolving speed under room temperature, obtains reaction solution；
(6) reaction solution liquid is placed at 35 ~ 40 DEG C and is aged, obtain gel, gel is placed at 55 ~ 60 DEG C, repeatedly with dehydrated alcohol
Cleaning 3 ~ 5 times, obtains detergent gel；
(7) detergent gel is placed at 55 ~ 60 DEG C dry 6 ~ 8h, obtains ZrO_2 aerogel.
The zirconium chloride, dehydrated alcohol, deionized water, the parts by weight of ethylenediamine tetra-acetic acid, first phthalein amine, propylene oxide
For 20 ~ 30 parts of zirconium chlorides, 40 ~ 50 parts of dehydrated alcohols, 40 ~ 50 parts of deionized waters, 1 ~ 3 part of ethylenediamine tetra-acetic acid, 5 ~ 10 parts of first
Phthalein amine, 10 ~ 15 parts of propylene oxide.
The specific preparation step of nano silica described in step (2) are as follows:
(1) sodium metasilicate is added in deionized water, 20 ~ 30min is stirred with 80 ~ 100r/min revolving speed under room temperature, obtains sodium silicate salt
Solution；
(2) octyl phenol polyoxyethylene ether is added in n-amyl alcohol, 15 ~ 20min is stirred with 150 ~ 200r/min revolving speed under room temperature, is obtained
Mixed liquor；
(3) mixed liquor, hexamethylene are added in sodium silicate salt solution, 15 ~ 30min of supersonic oscillations under room temperature obtains microemulsion；
(4) microemulsion pH to 1 ~ 2 is adjusted, 1 ~ 1.5h is reacted under room temperature, obtains gel；
(5) gel is placed in dehydrated alcohol and is sufficiently washed 3 ~ 5 times, obtain washed product, by washed product through azeotropic distillation and very
After sky is dry, it is placed in 3 ~ 4h of calcination at 70 DEG C, obtains nano silica.
The sodium metasilicate, deionized water, octyl phenol polyoxyethylene ether, n-amyl alcohol, hexamethylene parts by weight be 20 ~ 30 parts
Sodium metasilicate, 120 ~ 130 parts of deionized waters, 1 ~ 3 part of octyl phenol polyoxyethylene ether, 5 ~ 10 parts of n-amyl alcohols, 3 ~ 5 parts of hexamethylenes.
PH described in step (4) adjusts the sulfuric acid using mass concentration 1%.
The partial size of nano silica described in step (5) is 40 ~ 50nm.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention prepares silicon rubber base aeroge composite insulation material using silicon rubber as raw material, and silicon rubber is one kind with silicon oxygen
Chain is main chain, can connect the linear polysiloxanes of the high molecular weight of organic side group such as methyl, phenyl on silicon atom, has both nothing
The macromolecular material of machine and organic nature, the bond energy of silicon oxygen bond is greater than the bond energy of carbon-carbon bond, so the heat of organosilicon product
Stability is high, and chemical bond is not easy to break in high temperature or the lower molecule of irradiation and decomposes, so that it is compound absolutely to improve silicon rubber base aeroge
The high temperature resistance and insulation capacity of hot material；
(2) present invention uses ZrO_2 aerogel for raw material, silicon rubber base aeroge composite insulation material is prepared, due to dioxy
The aperture for changing zirconium aeroge is less than the mean free path of air molecule, does not have cross-ventilation in aeroge, and porosity is high, Gu
Volume ratio shared by body is very low, large specific surface area, keeps the thermal conductivity of aeroge very low, so as to improve the insulation of heat-insulating material
The warm-up movement of effect, gas molecule can cause heat transfer, due to the inside overwhelming majority stomata ruler of ZrO_2 aerogel
The very little mean free path for being respectively less than gas molecule motion, this limits gas molecule just before carrying out collision transmitting energy
Activity will there is no can be with when hole diameter is less than 50nm, in stomata to efficiently control the conduction of heat of gas
The air molecule of free movement, but be attracted on gasification inner wall, a kind of state similar to vacuum is formed, in addition, receiving
Even if the gas molecule in internal nano-sized stomata is also due to lose certainly in metre hole when temperature and larger difference variation
Heat convection can not be participated in by flowing or the mutually ability collided, so the ZrO_2 aerogel of addition nano-pore grade can be with
Effectively improve the heat insulation of silicon rubber base aeroge composite insulation material；
(3) present invention receives powder by addition nano silica, prepares silicon rubber base aeroge composite insulation material, nanometer two
Silica powder purity is high, density is low, large specific surface area, good dispersion and nontoxic and pollution-free, due in nano grade silica particles
Pore-size be less than or close in air molecule mean free path, with no convective heat transfer and all very small spy of heat transfer
Point, since nano silica itself belongs to amorphous state, nano particle interior atoms are disorderly arranged, the transmitting need of energy
It to give the higher energy of atom thermal vibration by the external world just to realize, this just illustrates to be used as the solid phase material itself for preparing exhausted material
Has the very low capacity of heat transmission, on the other hand, unique nano-pore structure makes hot-fluid that can only transmit and receive along stomata inner wall
Rice grain is interrupted area and contact area very little, this makes the transmission path of hot-fluid is elongated to significantly reduce the heat transfer of solid
Ability, the thermal conductivity of material can be effectively reduced in addition nano silica in heat-insulating material, improve the heat-insulation and heat-preservation of heat-insulating material
Effect.
Specific embodiment
According to parts by weight, 20 ~ 30 parts of sodium metasilicate, 120 ~ 130 parts of deionized waters, 1 ~ 3 part of octyl phenol polyoxy are weighed respectively
Sodium metasilicate is added in deionized water for vinethene, 5 ~ 10 parts of n-amyl alcohols, 3 ~ 5 parts of hexamethylenes, is turned under room temperature with 80 ~ 100r/min
Speed 20 ~ 30min of stirring, obtains sodium silicate salt solution, octyl phenol polyoxyethylene ether is added in n-amyl alcohol, under room temperature with 150 ~
200r/min revolving speed stirs 15 ~ 20min, obtains mixed liquor, and mixed liquor, hexamethylene are added in sodium silicate salt solution, surpassed under room temperature
15 ~ 30min of sonication, obtains microemulsion, into microemulsion uniform speed slow instill mass fraction be 1% the concentrated sulfuric acid and with 10r/
The stirring of min revolving speed adjusts microemulsion pH to 1 ~ 2, reacts 1 ~ 1.5h under room temperature, obtain gel, gel is placed in dehydrated alcohol and is filled
Divide washing 3 ~ 5 times, obtain washed product, by washed product after azeotropic distillation and vacuum drying, is placed in 3 ~ 4h of calcination at 70 DEG C, obtains
Nano silica, then according to parts by weight, weigh respectively 20 ~ 30 parts of zirconium chlorides, 40 ~ 50 parts of dehydrated alcohols, 40 ~ 50 parts go
Ionized water, 1 ~ 3 part of ethylenediamine tetra-acetic acid, 5 ~ 10 parts of first phthalein amine, 10 ~ 15 parts of propylene oxide, are added deionized water for dehydrated alcohol
In, 15 ~ 20min is stirred with 50 ~ 100r/min revolving speed under room temperature, obtains ethanol solution, zirconium chloride is added in ethanol solution, often
40 ~ 50min is stirred with 150 ~ 200r/min revolving speed under temperature, zirconium chloride ethanol solution is obtained, tetrachloro is added in ethylenediamine tetra-acetic acid
Change in zirconium ethanol solution, 30 ~ 40min is stirred with 100 ~ 150r/min revolving speed under room temperature, obtains chelating liquid, first phthalein amine is added and is chelated
In liquid, 30 ~ 40min is stirred with 150 ~ 200r/min revolving speed under room temperature, obtains mechanism liquid, propylene oxide is added in mechanism liquid, often
15 ~ 20min is stirred with 150 ~ 200r/min revolving speed under temperature, reaction solution is obtained, reaction solution liquid is placed at 35 ~ 40 DEG C and is aged, obtain solidifying
Gel is placed at 55 ~ 60 DEG C by glue, is cleaned 3 ~ 5 times repeatedly with dehydrated alcohol, is obtained detergent gel, and detergent gel is placed in 55 ~ 60
Dry 6 ~ 8h, obtains ZrO_2 aerogel, then according to parts by weight at DEG C, weighs 50 ~ 70 parts of methyl silicone rubbers, 30 ~ 50 respectively
Part phenyl siloxane rubber, 20 ~ 30 parts of ZrO_2 aerogels, 15 ~ 20 parts of nano silicas, 10 ~ 15 parts of phenolic resin, 5 ~ 10 parts
The short fibre of aramid fiber, 3 ~ 5 parts of zinc oxide, 1 ~ 3 part of stearic acid, 1 ~ 3 part of iron oxide, 3 ~ 5 parts of vinyl triamines, 2 ~ 4 parts of sulphur, by methyl
Silicon rubber, phenyl siloxane rubber, ZrO_2 aerogel, phenolic resin are placed in 20 ~ 30min of premix in vacuum kneader, must premix
Nano silica, the short fibre of aramid fiber, zinc oxide, stearic acid, iron oxide are added in premix, mould on the double roll mill by material
30 ~ 40min is refined, must plasticate mixture, vinyl triamine, sulphur are added in mixture of plasticating, the room temperature on vulcanizing press
Vulcanization 22 ~ for 24 hours, obtain silicon rubber base aeroge composite insulation material.
According to parts by weight, 20 parts of sodium metasilicate, 120 parts of deionized waters, 1 part of octyl phenol polyoxyethylene ether, 5 parts are weighed respectively
Sodium metasilicate is added in deionized water for n-amyl alcohol, 3 parts of hexamethylenes, stirs 20min under room temperature with 80r/min revolving speed, obtains sodium metasilicate
Octyl phenol polyoxyethylene ether is added in n-amyl alcohol salting liquid, stirs 15min under room temperature with 150r/min revolving speed, obtains mixed liquor,
Mixed liquor, hexamethylene are added in sodium silicate salt solution, supersonic oscillations 15min under room temperature obtains microemulsion, even into microemulsion
Speed is slowly dropped into the concentrated sulfuric acid that mass fraction is 1% and with the stirring of 10r/min revolving speed, adjusts microemulsion pH to 1, reacts under room temperature
1h obtains gel, and gel is placed in dehydrated alcohol and is sufficiently washed 3 times, washed product is obtained, by washed product through azeotropic distillation and very
After sky is dry, is placed at 70 DEG C and is calcined 3h, obtain nano silica, then according to parts by weight, weigh respectively 20 parts of zirconium chlorides,
40 parts of dehydrated alcohols, 40 parts of deionized waters, 1 part of ethylenediamine tetra-acetic acid, 5 parts of first phthalein amine, 10 parts of propylene oxide, by dehydrated alcohol plus
Enter in deionized water, 15min is stirred with 50r/min revolving speed under room temperature, ethanol solution is obtained, ethanol solution is added in zirconium chloride
In, 40min is stirred with 150r/min revolving speed under room temperature, obtains zirconium chloride ethanol solution, four chlorinations are added in ethylenediamine tetra-acetic acid
In zirconium ethanol solution, 30min is stirred with 100r/min revolving speed under room temperature, obtains chelating liquid, first phthalein amine is added in chelating liquid, room temperature
Under with 150r/min revolving speed stir 30min, obtain mechanism liquid, by propylene oxide be added mechanism liquid in, under room temperature with 150r/min turn
Speed stirring 15min, obtains reaction solution, reaction solution liquid is placed at 35 DEG C and is aged, gel is obtained, gel is placed at 55 DEG C, use is anhydrous
Ethyl alcohol cleans 3 times repeatedly, obtains detergent gel, and detergent gel is placed at 55 DEG C dry 6h, obtains ZrO_2 aerogel, then by weight
Number meter is measured, weighs 50 parts of methyl silicone rubbers, 30 parts of phenyl siloxane rubbers, 20 parts of ZrO_2 aerogels, 15 parts of nanometers two respectively
The short fibre of silica, 10 parts of phenolic resin, 5 parts of aramid fibers, 3 parts of zinc oxide, 1 part of stearic acid, 1 part of iron oxide, 3 parts of vinyl triamines, 2
Part sulphur, methyl silicone rubber, phenyl siloxane rubber, ZrO_2 aerogel, phenolic resin are placed in vacuum kneader and are premixed
20min obtains premix, nano silica, the short fibre of aramid fiber, zinc oxide, stearic acid, iron oxide is added in premix, double
Plasticate 30min on roller open mill, and must plasticate mixture, vinyl triamine, sulphur is added in mixture of plasticating, in compression molding
Room temperature vulcanization 22h on machine obtains silicon rubber base aeroge composite insulation material.
According to parts by weight, 25 parts of sodium metasilicate, 125 parts of deionized waters, 2 parts of octyl phenol polyoxyethylene ether, 7 parts are weighed respectively
Sodium metasilicate is added in deionized water for n-amyl alcohol, 4 parts of hexamethylenes, stirs 25min under room temperature with 90r/min revolving speed, obtains sodium metasilicate
Octyl phenol polyoxyethylene ether is added in n-amyl alcohol salting liquid, stirs 17min under room temperature with 175r/min revolving speed, obtains mixed liquor,
Mixed liquor, hexamethylene are added in sodium silicate salt solution, supersonic oscillations 22min under room temperature obtains microemulsion, even into microemulsion
Speed is slowly dropped into the concentrated sulfuric acid that mass fraction is 1% and is stirred with 10r/min revolving speed, adjusting microemulsion pH to 1.5, anti-under room temperature
1.3h is answered, gel is obtained, gel is placed in dehydrated alcohol and is sufficiently washed 4 times, washed product is obtained, by washed product through azeotropic distillation
It after vacuum drying, is placed at 70 DEG C and is calcined 3.5h, obtain nano silica, then according to parts by weight, weigh 25 part four respectively
Zirconium chloride, 45 parts of dehydrated alcohols, 45 parts of deionized waters, 2 parts of ethylenediamine tetra-acetic acids, 7 parts of first phthalein amine, 13 parts of propylene oxide, by nothing
Water-ethanol is added in deionized water, stirs 17min under room temperature with 75r/min revolving speed, obtains ethanol solution, second is added in zirconium chloride
In alcoholic solution, 45min is stirred with 175r/min revolving speed under room temperature, zirconium chloride ethanol solution is obtained, ethylenediamine tetra-acetic acid is added
In zirconium chloride ethanol solution, 35min is stirred with 125r/min revolving speed under room temperature, obtains chelating liquid, chelating liquid is added in first phthalein amine
In, under room temperature with 175r/min revolving speed stir 35min, obtain mechanism liquid, by propylene oxide be added mechanism liquid in, under room temperature with
175r/min revolving speed stirs 17min, obtains reaction solution, reaction solution liquid is placed at 37 DEG C and is aged, gel is obtained, gel is placed in 57 DEG C
Under, it is cleaned repeatedly with dehydrated alcohol 4 times, obtains detergent gel, detergent gel is placed at 57 DEG C dry 7h, obtains zirconium dioxide airsetting
Glue, then according to parts by weight, 60 parts of methyl silicone rubbers, 40 parts of phenyl siloxane rubbers, 25 parts of ZrO_2 aerogels, 17 are weighed respectively
Part nano silica, 13 parts of phenolic resin, the short fibre of 7 parts of aramid fibers, 4 parts of zinc oxide, 2 parts of stearic acid, 2 parts of iron oxide, 4 parts of ethylene
Base triamine, 3 parts of sulphur, are placed in vacuum kneader for methyl silicone rubber, phenyl siloxane rubber, ZrO_2 aerogel, phenolic resin
Middle premix 25min, obtains premix, and premix is added in nano silica, the short fibre of aramid fiber, zinc oxide, stearic acid, iron oxide
In, plasticate 35min on the double roll mill, and must plasticate mixture, vinyl triamine, sulphur are added in mixture of plasticating,
Room temperature vulcanization 23h on vulcanizing press obtains silicon rubber base aeroge composite insulation material.
According to parts by weight, 30 parts of sodium metasilicate, 130 parts of deionized waters, 3 parts of octyl phenol polyoxyethylene ether, 10 are weighed respectively
Part n-amyl alcohol, 5 parts of hexamethylenes, sodium metasilicate is added in deionized water, is stirred 30min under room temperature with 100r/min revolving speed, is obtained silicon
Octyl phenol polyoxyethylene ether is added in n-amyl alcohol acid sodium-salt solution, stirs 20min under room temperature with 200r/min revolving speed, obtains mixed
Liquid is closed, mixed liquor, hexamethylene are added in sodium silicate salt solution, supersonic oscillations 30min under room temperature obtains microemulsion, to micro emulsion
In liquid uniform speed slow instill mass fraction be 1% the concentrated sulfuric acid and with 10r/min revolving speed stirring, adjust microemulsion pH to 2, room temperature
Lower reaction 1.5h, obtains gel, and gel is placed in dehydrated alcohol and is sufficiently washed 5 times, washed product is obtained, by washed product through azeotropic
It after distillation and vacuum drying, is placed at 70 DEG C and is calcined 4h, obtain nano silica, then according to parts by weight, weigh 30 parts respectively
Zirconium chloride, 50 parts of dehydrated alcohols, 50 parts of deionized waters, 3 parts of ethylenediamine tetra-acetic acids, 10 parts of first phthalein amine, 15 parts of propylene oxide, will
Dehydrated alcohol is added in deionized water, stirs 20min under room temperature with 100r/min revolving speed, obtains ethanol solution, by zirconium chloride plus
Enter in ethanol solution, 50min is stirred with 150 ~ 200r/min revolving speed under room temperature, zirconium chloride ethanol solution is obtained, by ethylenediamine tetraacetic
Acetic acid is added in zirconium chloride ethanol solution, stirs 40min under room temperature with 150r/min revolving speed, obtains chelating liquid, first phthalein amine is added
Enter to chelate in liquid, 40min is stirred with 200r/min revolving speed under room temperature, obtains mechanism liquid, propylene oxide is added in mechanism liquid, room temperature
Under with 200r/min revolving speed stir 20min, obtain reaction solution, reaction solution liquid be placed at 40 DEG C and is aged, gel is obtained, gel is placed in
It at 60 DEG C, is cleaned repeatedly with dehydrated alcohol 5 times, obtains detergent gel, detergent gel is placed at 60 DEG C dry 8h, obtains zirconium dioxide
Aeroge, then according to parts by weight, 70 parts of methyl silicone rubbers, 50 parts of phenyl siloxane rubbers, 30 parts of zirconium dioxide airsettings are weighed respectively
The short fibre of glue, 20 parts of nano silicas, 15 parts of phenolic resin, 10 parts of aramid fibers, 5 parts of zinc oxide, 3 parts of stearic acid, 3 parts of iron oxide, 5
Part vinyl triamine, 4 parts of sulphur, are placed in vacuum for methyl silicone rubber, phenyl siloxane rubber, ZrO_2 aerogel, phenolic resin
30min is premixed in kneader, obtains premix, nano silica, the short fibre of aramid fiber, zinc oxide, stearic acid, iron oxide is added pre-
In mixing, plasticate 40min on the double roll mill, and must plasticate mixture, and mixture of plasticating is added in vinyl triamine, sulphur
In, room temperature vulcanization for 24 hours, obtains silicon rubber base aeroge composite insulation material on vulcanizing press.
Silicon rubber base aeroge composite insulation material is prepared in above embodiments and passes through intelligent double plate heat conduction systems
Number analyzer measures thermal coefficient, and physical properties detect according to concerned countries standard " cryogenic vacuum reflective insulant
Standard schedule " method progress.
1 silicon rubber base aeroge composite insulation material performance characterization of table
Silicon rubber base aeroge composite insulation material prepared by the present invention as shown in Table 1, thermal coefficient is low, and high temperature resistant is good, and heat is steady
It is qualitative excellent, have a vast market value and application prospect.
Claims (10)
1. a kind of preparation method of silicon rubber base aeroge composite insulation material, which is characterized in that specific preparation step are as follows:
(1) methyl silicone rubber, phenyl siloxane rubber, ZrO_2 aerogel, phenolic resin are placed in vacuum kneader and premix 20
~ 30min, obtains premix；
(2) nano silica, the short fibre of aramid fiber, zinc oxide, stearic acid, iron oxide are added in premix, in two-roll mill
On plasticate 30 ~ 40min, must plasticate mixture；
(3) vinyl triamine, sulphur addition are plasticated in mixture, the room temperature vulcanization 22 ~ for 24 hours on vulcanizing press obtains silicon rubber
Matrix aeroge composite insulation material.
2. a kind of preparation method of silicon rubber base aeroge composite insulation material according to claim 1, which is characterized in that
The short fine, oxygen of the methyl silicone rubber, phenyl siloxane rubber, ZrO_2 aerogel, nano silica, phenolic resin, aramid fiber
Changing zinc, stearic acid, iron oxide, vinyl triamine, the parts by weight of sulphur is 50 ~ 70 parts of methyl silicone rubbers, 30 ~ 50 parts of phenyl silicon rubbers
The short fibre of glue, 20 ~ 30 parts of ZrO_2 aerogels, 15 ~ 20 parts of nano silicas, 10 ~ 15 parts of phenolic resin, 5 ~ 10 parts of aramid fibers, 3
~ 5 parts of zinc oxide, 1 ~ 3 part of stearic acid, 1 ~ 3 part of iron oxide, 3 ~ 5 parts of vinyl triamines, 2 ~ 4 parts of sulphur.
3. a kind of preparation method of silicon rubber base aeroge composite insulation material according to claim 1, which is characterized in that
The molecular weight of methyl silicone rubber described in step (1) is 34000 ~ 36000, and the molecular weight of phenyl siloxane rubber is 43000 ~ 45000.
4. a kind of preparation method of silicon rubber base aeroge composite insulation material according to claim 1, which is characterized in that
The length of the short fibre of aramid fiber described in step (2) be 2 ~ 4mm, 6 ~ 7 μm of diameter.
5. a kind of preparation method of silicon rubber base aeroge composite insulation material according to claim 1, which is characterized in that
The specific preparation step of ZrO_2 aerogel described in step (1) are as follows:
(1) dehydrated alcohol is added in deionized water, 15 ~ 20min is stirred with 50 ~ 100r/min revolving speed under room temperature, it is molten to obtain ethyl alcohol
Liquid；
(2) zirconium chloride is added in ethanol solution, 40 ~ 50min is stirred with 150 ~ 200r/min revolving speed under room temperature, obtains four chlorinations
Zirconium ethanol solution；
(3) by ethylenediamine tetra-acetic acid be added zirconium chloride ethanol solution in, under room temperature with 100 ~ 150r/min revolving speed stirring 30 ~
40min obtains chelating liquid；
(4) first phthalein amine is added in chelating liquid, 30 ~ 40min is stirred with 150 ~ 200r/min revolving speed under room temperature, obtains mechanism liquid；
(5) propylene oxide is added in mechanism liquid, 15 ~ 20min is stirred with 150 ~ 200r/min revolving speed under room temperature, obtains reaction solution；
(6) reaction solution liquid is placed at 35 ~ 40 DEG C and is aged, obtain gel, gel is placed at 55 ~ 60 DEG C, repeatedly with dehydrated alcohol
Cleaning 3 ~ 5 times, obtains detergent gel；
(7) detergent gel is placed at 55 ~ 60 DEG C dry 6 ~ 8h, obtains ZrO_2 aerogel.
6. a kind of preparation method of silicon rubber base aeroge composite insulation material according to claim 5, which is characterized in that
The zirconium chloride, dehydrated alcohol, deionized water, ethylenediamine tetra-acetic acid, first phthalein amine, propylene oxide parts by weight be 20 ~ 30
Part zirconium chloride, 40 ~ 50 parts of dehydrated alcohols, 40 ~ 50 parts of deionized waters, 1 ~ 3 part of ethylenediamine tetra-acetic acid, 5 ~ 10 parts of first phthalein amine, 10 ~
15 parts of propylene oxide.
7. a kind of preparation method of silicon rubber base aeroge composite insulation material according to claim 1, which is characterized in that
The specific preparation step of nano silica described in step (2) are as follows:
(1) sodium metasilicate is added in deionized water, 20 ~ 30min is stirred with 80 ~ 100r/min revolving speed under room temperature, obtains sodium silicate salt
Solution；
(2) octyl phenol polyoxyethylene ether is added in n-amyl alcohol, 15 ~ 20min is stirred with 150 ~ 200r/min revolving speed under room temperature, is obtained
Mixed liquor；
(3) mixed liquor, hexamethylene are added in sodium silicate salt solution, 15 ~ 30min of supersonic oscillations under room temperature obtains microemulsion；
(4) microemulsion pH to 1 ~ 2 is adjusted, 1 ~ 1.5h is reacted under room temperature, obtains gel；
(5) gel is placed in dehydrated alcohol and is sufficiently washed 3 ~ 5 times, obtain washed product, by washed product through azeotropic distillation and very
After sky is dry, 3 ~ 4 h of calcination at 70 DEG C are placed in, nano silica is obtained.
8. a kind of preparation method of silicon rubber base aeroge composite insulation material according to claim 7, which is characterized in that
The sodium metasilicate, deionized water, octyl phenol polyoxyethylene ether, n-amyl alcohol, hexamethylene parts by weight be 20 ~ 30 parts of sodium metasilicate,
120 ~ 130 parts of deionized waters, 1 ~ 3 part of octyl phenol polyoxyethylene ether, 5 ~ 10 parts of n-amyl alcohols, 3 ~ 5 parts of hexamethylenes.
9. a kind of preparation method of silicon rubber base aeroge composite insulation material according to claim 7, which is characterized in that
PH described in step (4) adjusts the sulfuric acid using mass concentration 1%.
10. a kind of preparation method of silicon rubber base aeroge composite insulation material according to claim 7, feature exist
In the partial size of nano silica described in step (5) is 40 ~ 50nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910154099.3A CN110003655A (en) | 2019-03-01 | 2019-03-01 | A kind of preparation method of silicon rubber base aeroge composite insulation material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910154099.3A CN110003655A (en) | 2019-03-01 | 2019-03-01 | A kind of preparation method of silicon rubber base aeroge composite insulation material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110003655A true CN110003655A (en) | 2019-07-12 |
Family
ID=67166154
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910154099.3A Withdrawn CN110003655A (en) | 2019-03-01 | 2019-03-01 | A kind of preparation method of silicon rubber base aeroge composite insulation material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110003655A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704458A (en) * | 2020-05-24 | 2020-09-25 | 福建华夏金刚科技股份有限公司 | Fine functional ceramic containing silicon dioxide nanocrystals and preparation method thereof |
| CN112555579A (en) * | 2020-12-24 | 2021-03-26 | 苏州市君悦新材料科技股份有限公司 | Heat insulating material and core material |
| WO2022183953A1 (en) * | 2021-03-03 | 2022-09-09 | 江苏时代新能源科技有限公司 | Thermal insulation pad and preparation method therefor, and battery pack and apparatus |
-
2019
- 2019-03-01 CN CN201910154099.3A patent/CN110003655A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704458A (en) * | 2020-05-24 | 2020-09-25 | 福建华夏金刚科技股份有限公司 | Fine functional ceramic containing silicon dioxide nanocrystals and preparation method thereof |
| CN111704458B (en) * | 2020-05-24 | 2022-05-27 | 福建华夏金刚科技股份有限公司 | Fine functional ceramic containing silicon dioxide nanocrystals and preparation method thereof |
| CN112555579A (en) * | 2020-12-24 | 2021-03-26 | 苏州市君悦新材料科技股份有限公司 | Heat insulating material and core material |
| WO2022183953A1 (en) * | 2021-03-03 | 2022-09-09 | 江苏时代新能源科技有限公司 | Thermal insulation pad and preparation method therefor, and battery pack and apparatus |
| EP4130156A4 (en) * | 2021-03-03 | 2023-11-29 | Jiangsu Contemporary Amperex Technology Limited | Thermal insulation pad and preparation method therefor, and battery pack and apparatus |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110003655A (en) | A kind of preparation method of silicon rubber base aeroge composite insulation material | |
| CN102633464B (en) | Method for preparing SiO2 aerogel heat insulating composite through adhesive slip casting | |
| CN108658576A (en) | A kind of preparation method of composite silicon dioxide aerogel blanket | |
| CN114031943B (en) | Inter-surface high-thermal-conductivity composite material and preparation method thereof | |
| CN101823897A (en) | Composite mesoporous material | |
| CN109439060A (en) | A kind of caesium tungsten bronze/graphene composite powder and the preparation method and application thereof | |
| CN108892471A (en) | A kind of preparation method of composite, insulating felt | |
| Zhao et al. | Sound absorption polyimide composite aerogels for ancient architectures’ protection | |
| CN109225079A (en) | A kind of high temperature resistant aeroge composite material and preparation method | |
| CN106898802B (en) | A kind of high-performing car hydrogen fuel cell composite nano-powder material and preparation method thereof | |
| CN101302091A (en) | Nano-hole silica composite heat insulation material and preparation thereof | |
| CN104476857A (en) | Nano silicon thermal insulation material and preparation method thereof | |
| CN108046664A (en) | A kind of ceramic beaverboard and preparation method thereof | |
| CN102107877A (en) | Method for preparing 0.85nm hydrated kaolinite by direct replacement intercalation | |
| CN106565198B (en) | A kind of method that constant pressure and dry prepares flexible aerosil | |
| CN114989588A (en) | Degradable material with heat insulation and energy storage performance and preparation method thereof | |
| Kang et al. | Thermal comfort and flame retardant performance of novel temperature-control coatings with modified phase change material microcapsules | |
| CN108659327A (en) | A kind of special heat-conducting insulation material of new energy car battery and preparation method thereof | |
| Zhang et al. | High thermal storage ability and photothermal conversion capacity phase change capsule with graphene oxide covalently grafted silica shell | |
| CN105968789A (en) | Lightweight organic-inorganic composite heat insulation foam material and preparation method thereof | |
| CN110216932A (en) | The preparation method and flexible nano heat-insulation and heat-preservation felt of flexible nano heat-insulation and heat-preservation felt | |
| Ji et al. | Electrostatic assembly of MOF-TiO2 frameworks and hollow structures for the preparation of ultra-thin thermally-insulated aerogels via electrospinning | |
| Yu et al. | Construction of AlN oriented skeletons using in-situ reaction strategy and their enhancement effect on the thermal conductivity of epoxy composites | |
| CN116715900A (en) | Modified hexagonal boron nitride and preparation method and application thereof | |
| CN107522961B (en) | Polystyrene-based high-heat-conductive composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190712 |
|
| WW01 | Invention patent application withdrawn after publication |