CN108034255A - High fire-retardance heat-conducting silica gel sheet and its manufacture method - Google Patents
High fire-retardance heat-conducting silica gel sheet and its manufacture method Download PDFInfo
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- CN108034255A CN108034255A CN201711053641.3A CN201711053641A CN108034255A CN 108034255 A CN108034255 A CN 108034255A CN 201711053641 A CN201711053641 A CN 201711053641A CN 108034255 A CN108034255 A CN 108034255A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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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
- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention discloses a kind of high fire-retardance heat-conducting silica gel sheet, include 320 370 parts of vinyl-terminated silicone fluid, 10 20 parts of containing hydrogen silicone oil, 4 7.5 parts of platinum catalyst according to mass parts, 0.2 0.3 parts of acetylenic alcohol inhibitor, 8 13 parts of coupling agent, 450 700 parts of fine grain aluminium hydroxide aluminium hydroxide, the fine grain aluminium hydroxide particle diameter are 0.5 15 microns, 680 1000 parts of coarse grain footpath aluminium hydroxide, the coarse grain footpath aluminium hydroxide particle diameter is 15 70 microns, 120 250 parts of bromide fire retardant, 15 20 parts of antimony oxide.The application add bromide fire retardant and and antimony oxide, compound the aluminium hydroxide of two kinds of particle diameters of thickness, flame retardant effect greatly enhances, and heat conductive silica gel plate sheet flame retardant rating can be made to reach UL94 V0 standards, therefore can operate with the heat conductive insulating electronic product of flame-retardancy requirements higher.
Description
Technical field
The present invention relates to thermal conductive silicon field, more particularly to high fire-retardance heat-conducting silica gel sheet and its manufacture method.
Background technology
Heat-conducting silica gel sheet is using silica gel as base material, and the various auxiliary materials such as addition metal oxide, are synthesized by special process
A kind of heat-conducting medium material, be exclusively for using gap transmit heat designing scheme produce, can blind, complete fever
The heat transfer of position and radiating part interdigit, while also act as insulation, damping, sealing etc. and act on, disclosure satisfy that device miniaturization and
The design requirement of ultrathin, is great craftsmanship and usability, and thickness is applied widely, a kind of splendid conductive filler material
Material.
It is all that through hole adds aluminium oxide as fire retardant is poor and cannot pass through UL94-V0 that traditional heat-conducting silica gel sheet is fire-retardant
Standard.The problem of above problem is this area urgent need to resolve.
The content of the invention
The technical problem to be solved by the present invention is to provide a kind of high fire-retardance heat-conducting silica gel sheet with good flame-retardance energy.
The technical solution adopted by the present invention to solve the technical problems is：A kind of high fire-retardance heat-conducting silica gel sheet, according to quality
Part includes 320-370 parts of vinyl-terminated silicone fluid, 10-20 parts of containing hydrogen silicone oil, 4-7.5 parts of platinum catalyst, acetylenic alcohol inhibitor 0.2-
0.3 part, 8-13 parts of coupling agent, 450-700 parts of fine grain aluminium hydroxide aluminium hydroxide, the fine grain aluminium hydroxide particle diameter is
0.5-15 microns, aluminium hydroxide 680-1000 parts of coarse grain footpath, the coarse grain footpath aluminium hydroxide particle diameter is 15-70 microns, the resistance of bromine system
Fire 120-250 parts of agent, 15-20 parts of antimony oxide.
The application add bromide fire retardant and and antimony oxide, compound two kinds of particle diameters of thickness aluminium hydroxide, it is fire-retardant
Effect greatly enhances, and heat conductive silica gel plate sheet flame retardant rating can be made to reach UL94-V0 standards, therefore can operate with flame-retardancy requirements more
In high heat conductive insulating electronic product.
It is further：The bromide fire retardant, is decabromodiphenylethane, its content is at 120-170 parts.
It is further：The fine grain aluminium hydroxide is 5 microns of 550-600 parts of aluminium hydroxides, coarse grain footpath hydrogen-oxygen
Change aluminium is 20 microns of 780-850 parts of aluminium hydroxides.
As a further improvement on the present invention, there is provided a kind of method for manufacturing high fire-retardance heat-conducting silica gel sheet, scheme are：One
The manufacture method of kind high fire-retardance heat-conducting silica gel sheet,
A, vinyl-terminated silicone fluid, containing hydrogen silicone oil, acetylenic alcohol inhibitor, platinum catalyst, coupling are added into stirred tank successively
Agent, starts to stir, mixing speed 45r/min stirrings 20min；
B, vacuumized after stirring a period of time and reduce rotating speed and be stirred 10-15min to 35r/min；
C, and then fine grain aluminium hydroxide is added, 2-3min is first stirred under the rotating speed of 20r/min, then improves rotating speed extremely
30r/min is simultaneously vacuumized, and stirs 15min under vacuum conditions；
D, add bromide fire retardant and antimony oxide first stirs 2-3min under the rotating speed of 20r/min, then improve and turn
Speed is to 30r/min and vacuumizes, and stirs 15min under vacuum conditions；
E, add coarse grain footpath aluminium hydroxide and mill base first stirs 2-3min under the rotating speed of 20r/min, then improve rotating speed
To 30r/min and vacuumize, stir 5-10min under vacuum conditions, then rotating speed is down to low speed 12-15r/min and then is kept
It is stirred under vacuum 25min；
F, discharging calendering；
G, sulfidization molding is carried out through 130 DEG C of ovens.
The beneficial effects of the invention are as follows：Application add bromide fire retardant and and antimony oxide, compound two kinds of grains of thickness
The aluminium hydroxide in footpath, flame retardant effect greatly enhance, and heat-conducting silica gel sheet flame retardant rating can be made to reach UL94-V0 standards, therefore can transport
For in the heat conductive insulating electronic product of flame-retardancy requirements higher.In addition stirring at low speed is first carried out during charging to disperse, then
Improve speed to be disperseed, vacuumize for removing high-speed stirred caused bubble later.The application flame retarding efficiency is high, processing
Technique is simple, has the excellent performances such as heat conduction, insulation, the small, high fire-retardance of proportion concurrently.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Embodiment
The present invention is further described with reference to the accompanying drawings and detailed description.
As shown in Figure 1, being the manufacturing process flow schematic diagram of the application, all numbers are mass parts in the application.
S1 adds 320-370 parts of vinyl-terminated silicone fluid, 10-20 parts of containing hydrogen silicone oil, acetylenic alcohol inhibitor into stirred tank successively
0.2-0.3 parts, 4-7.5 parts of platinum catalyst, 0.2-0.3 parts of coupling agent, starts to stir, since the material added at this time is liquid
Material, so mixing speed can be higher at this time, preferable mixing speed stirs 20min for 45r/min.
Then S2 is vacuumized and reduced rotating speed is stirred 10-15min to discharge first step high-speed stirred to 35r/min
Caused bubble.
S3 and then addition particle diameter are a kind of 450-700 parts in 0.5 micron to 15 microns of fine grain aluminium hydroxide, as
It is preferred that 5 microns of 550-600 parts of aluminium hydroxides are selected herein, since aluminium hydroxide is pulvis, so first under the rotating speed of 20r/min
Pre-dispersed, stirring 2-3min is carried out, rotating speed is then improved and to 30r/min and vacuumizes, accelerate scattered and discharge bubble, in vacuum
15min is stirred under state.
S4 adds 120-250 parts of bromide fire retardant, and 15-20 parts of antimony oxide first stirs under the rotating speed of 20r/min
2-3min, then improves rotating speed and to 30r/min and vacuumizes, stir 15min under vacuum conditions.Above-mentioned bromide fire retardant is preferred
Decabromodiphenylethane, 1.5 times or so can be reduced by dosage by selecting decabromodiphenylethane to make fire retardant, the addition of decabromodiphenylethane
Measure as 120-170 parts.
S5 adds a kind of 680-1000 parts and mill base 0.5-1.0 in the aluminium hydroxide that particle diameter is 15 microns to 20 microns
Part, 20 microns of 780-850 parts of aluminium hydroxides are selected as preferred the application, 2-3min are first stirred under the rotating speed of 20r/min, so
Rotating speed is improved afterwards to 30r/min and to vacuumize, and stirs 5-10min under vacuum conditions, then rotating speed is down to low speed 12-15r/
Min, at this time and then keeps being stirred under vacuum 25min, mill base is used to paint in this step.
S6 discharging calenderings, the product of any thickness of 0.3-3mm can be rolled into by calender,
For S7 by the product anti-corrosion oven by calendering, oven temperature is arranged on 130 DEG C of progress sulfidization moldings.
The effect of each component in this application：Vinyl-terminated silicone fluid is matrix resin；Containing hydrogen silicone oil is used for and matrix resin
Crosslinking curing acts on；Platinum catalyst is chemically reacted for being catalyzed silicone oil；Acetylenic alcohol inhibitor for delay chemically react into
OK, operability is increased；Coupling agent is used to increase the binding ability in formula between each component；Fine grain aluminium hydroxide assigns
Material thermal conductivity, insulating properties, and certain anti-flammability；Coarse grain footpath aluminium hydroxide assigns material thermal conductivity, insulating properties, Yi Jiyi
Fixed anti-flammability；Bromide fire retardant, flame retarding efficiency are high；Antimony oxide is synergistic flame retardant, arranges in pairs or groups and is lifted with bromide fire retardant
Flame retardant effect.
Obtained product is tested by UL94-V0 standards, equally takes 125mm long, the sample of 13mm wide, 0.3mm thickness
It is each 5 progress combustion testing, traditional heat-conducting silica gel sheet burning time for 10s to 30s between, and the product of the application burning when
Between be 1s to 5s, usually from fire i.e. go out.The application add bromide fire retardant and and antimony oxide, compound two kinds of particle diameters of thickness
Aluminium hydroxide, flame retardant effect greatly enhances, and heat conductive silica gel plate sheet flame retardant rating can be made to reach UL94-V0 standards, therefore can
Apply in the heat conductive insulating electronic product of flame-retardancy requirements higher.In addition stirring at low speed is first carried out during charging to disperse,
Disperseed improving speed, vacuumized for removing high-speed stirred caused bubble later.The application flame retarding efficiency is high, adds
Work technique is simple, has the excellent performances such as heat conduction, insulation, the small, high fire-retardance of proportion concurrently.
Some specific embodiments of some present invention presented below.
Embodiment 1
320 parts of vinyl-terminated silicone fluid, 10 parts of containing hydrogen silicone oil, 0.2 part of acetylenic alcohol inhibitor, platinum are added into stirred tank successively
4 parts of catalyst, 8 parts of coupling agent, starts to stir, and mixing speed stirs 20min for 45r/min.Vacuumized after stirring a period of time
And reduce rotating speed and be stirred 10min to 35r/min.Then 5 microns of 550 parts of aluminium hydroxides are added, are stirred under the rotating speed of 20r/min
2min is mixed, then rotating speed is improved to 30r/min and vacuumizes and stir 15min under vacuum conditions.Then decabrominated dipheny second is added
120 parts of alkane, and 15 parts of antimony oxide, stir 2min under the rotating speed of 20r/min, then improve rotating speed and to 30r/min and take out
Vacuum, stirs 15min under vacuum conditions.Then 0.5 part of 20 microns of addition, 780 parts of aluminium hydroxide and mill base, 20r/min's
2min is stirred under rotating speed, rotating speed is then improved and to 30r/min and vacuumizes, stir 5min under vacuum conditions, then rotating speed is dropped
To low speed 15r/min, at this time and then keep being stirred under vacuum 25min.
Discharging calendering.By the product anti-corrosion oven by calendering, oven temperature is arranged on 130 DEG C of progress sulfidization moldings.Most
Afterwards by product be put into guillotine cut into needed for specification finished product.
Embodiment 2
340 parts of vinyl-terminated silicone fluid, 15 parts of containing hydrogen silicone oil, 0.3 part of acetylenic alcohol inhibitor, platinum are added into stirred tank successively
6 parts of catalyst, 10 parts of coupling agent, starts to stir, and mixing speed stirs 20min for 45r/min.Vacuumized after stirring a period of time
And reduce rotating speed and be stirred 13min to 35r/min.Then 5 microns of 600 parts of aluminium hydroxides are added, are stirred under the rotating speed of 20r/min
2min is mixed, then rotating speed is improved to 30r/min and vacuumizes and stir 15min under vacuum conditions.Then decabrominated dipheny second is added
150 parts of alkane, and 17 parts of antimony oxide, stir 2min under the rotating speed of 20r/min, then improve rotating speed and to 30r/min and take out
Vacuum, stirs 15min under vacuum conditions.Then 0.7 part of 20 microns of addition, 800 parts of aluminium hydroxide and mill base, 20r/min's
2min is stirred under rotating speed, rotating speed is then improved and to 30r/min and vacuumizes, stir 7min under vacuum conditions, then rotating speed is dropped
To low speed 13r/min, at this time and then keep being stirred under vacuum 25min.
Discharging calendering.By the product anti-corrosion oven by calendering, oven temperature is arranged on 130 DEG C of progress sulfidization moldings.Most
Afterwards by product be put into guillotine cut into needed for specification finished product.
Embodiment 3
370 parts of vinyl-terminated silicone fluid, 20 parts of containing hydrogen silicone oil, 0.3 part of acetylenic alcohol inhibitor, platinum are added into stirred tank successively
7.5 parts of catalyst, 13 parts of coupling agent, starts to stir, and mixing speed stirs 20min for 45r/min.Taken out very after stirring a period of time
It is empty and reduce rotating speed and be stirred 15min to 35r/min.Then 5 microns of 650 parts of aluminium hydroxides are added, under the rotating speed of 20r/min
2min is stirred, then rotating speed is improved to 30r/min and vacuumizes and stir 15min under vacuum conditions.Then decabrominated dipheny is added
170 parts of ethane, and 20 parts of antimony oxide, stir 2min under the rotating speed of 20r/min, then improve rotating speed to 30r/min simultaneously
Vacuumize, stir 15min under vacuum conditions.Then 1 part of 20 microns of addition, 850 parts of aluminium hydroxide and mill base, 20r/min's
3min is stirred under rotating speed, rotating speed is then improved and to 30r/min and vacuumizes, stir 10min under vacuum conditions, then rotating speed is dropped
To low speed 12r/min, at this time and then keep being stirred under vacuum 25min.
Discharging calendering.By the product anti-corrosion oven by calendering, oven temperature is arranged on 130 DEG C of progress sulfidization moldings.Most
Afterwards by product be put into guillotine cut into needed for specification finished product.
Embodiment 4
370 parts of vinyl-terminated silicone fluid, 20 parts of containing hydrogen silicone oil, 0.3 part of acetylenic alcohol inhibitor, platinum are added into stirred tank successively
7.5 parts of catalyst, 13 parts of coupling agent, starts to stir, and mixing speed stirs 20min for 45r/min.Taken out very after stirring a period of time
It is empty and reduce rotating speed and be stirred 15min to 35r/min.Then 5 microns of 650 parts of aluminium hydroxides are added, under the rotating speed of 20r/min
2min is stirred, then rotating speed is improved to 30r/min and vacuumizes and stir 15min under vacuum conditions.Then brominated polyphenylene is added
250 parts of ethene, and 20 parts of antimony oxide, stir 2min under the rotating speed of 20r/min, then improve rotating speed to 30r/min simultaneously
Vacuumize, stir 15min under vacuum conditions.Then 1 part of 20 microns of addition, 850 parts of aluminium hydroxide and mill base, 20r/min's
3min is stirred under rotating speed, rotating speed is then improved and to 30r/min and vacuumizes, stir 10min under vacuum conditions, then rotating speed is dropped
To low speed 12r/min, at this time and then keep being stirred under vacuum 25min.
Discharging calendering.By the product anti-corrosion oven by calendering, oven temperature is arranged on 130 DEG C of progress sulfidization moldings.Most
Afterwards by product be put into guillotine cut into needed for specification finished product.
Embodiment 5
370 parts of vinyl-terminated silicone fluid, 20 parts of containing hydrogen silicone oil, 0.3 part of acetylenic alcohol inhibitor, platinum are added into stirred tank successively
7.5 parts of catalyst, 13 parts of coupling agent, starts to stir, and mixing speed stirs 20min for 45r/min.Taken out very after stirring a period of time
It is empty and reduce rotating speed and be stirred 15min to 35r/min.Then 0.5 micron of 700 parts of aluminium hydroxide, the rotating speed of 20r/min are added
Lower stirring 2min, then improves rotating speed to 30r/min and vacuumizes and stir 15min under vacuum conditions.Then bromination is added to gather
250 parts of styrene, and 20 parts of antimony oxide, stir 2min under the rotating speed of 20r/min, then improve rotating speed to 30r/min
And vacuumize, 15min is stirred under vacuum conditions.Then 1 part of 15 microns of addition, 1000 parts of aluminium hydroxide and mill base, in 20r/
3min is stirred under the rotating speed of min, rotating speed is then improved and to 30r/min and vacuumizes, stirs 10min under vacuum conditions, then will
Rotating speed is down to low speed 12r/min, at this time and then keeps being stirred under vacuum 25min.
Discharging calendering.By the product anti-corrosion oven by calendering, oven temperature is arranged on 130 DEG C of progress sulfidization moldings.Most
Afterwards by product be put into guillotine cut into needed for specification finished product.
Embodiment 6
370 parts of vinyl-terminated silicone fluid, 20 parts of containing hydrogen silicone oil, 0.3 part of acetylenic alcohol inhibitor, platinum are added into stirred tank successively
7.5 parts of catalyst, 13 parts of coupling agent, starts to stir, and mixing speed stirs 20min for 45r/min.Taken out very after stirring a period of time
It is empty and reduce rotating speed and be stirred 15min to 35r/min.Then 15 microns of 450 parts of aluminium hydroxides, the rotating speed of 20r/min are added
Lower stirring 2min, then improves rotating speed to 30r/min and vacuumizes and stir 15min under vacuum conditions.Then bromination is added to gather
250 parts of styrene, and 20 parts of antimony oxide, stir 2min under the rotating speed of 20r/min, then improve rotating speed to 30r/min
And vacuumize, 15min is stirred under vacuum conditions.Then 1 part of 70 microns of addition, 680 parts of aluminium hydroxide and mill base, in 20r/min
Rotating speed under stir 3min, then improve rotating speed and to 30r/min and vacuumize, stir 10min under vacuum conditions, then by rotating speed
Low speed 12r/min is down to, at this time and then keeps being stirred under vacuum 25min.
Discharging calendering.By the product anti-corrosion oven by calendering, oven temperature is arranged on 130 DEG C of progress sulfidization moldings.Most
Afterwards by product be put into guillotine cut into needed for specification finished product.
Particular embodiments described above, has carried out the purpose of the present invention, technical solution and beneficial effect further in detail
Describe in detail it is bright, it should be understood that the foregoing is merely the present invention specific embodiment, be not intended to limit the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done, should be included in the guarantor of the present invention
Within the scope of shield.
Claims (4)
1. a kind of high fire-retardance heat-conducting silica gel sheet, it is characterised in that include by mass parts：320-370 parts of vinyl-terminated silicone fluid, it is hydrogeneous
10-20 parts of silicone oil, 4-7.5 parts of platinum catalyst, 0.2-0.3 parts of acetylenic alcohol inhibitor, 8-13 parts of titanate coupling agent, fine grain hydrogen
450-700 parts of aluminium oxide aluminium hydroxide, the fine grain aluminium hydroxide particle diameter are 0.5-15 microns, coarse grain footpath aluminium hydroxide 680-
1000 parts, the coarse grain footpath aluminium hydroxide particle diameter is 15-70 microns, 120-250 parts of bromide fire retardant, antimony oxide 15-20
Part.
2. high fire-retardance heat-conducting silica gel sheet as claimed in claim 1, it is characterised in that：The bromide fire retardant is decabrominated dipheny second
Alkane, its content is at 120-170 parts.
3. high fire-retardance heat-conducting silica gel sheet as claimed in claim 1, it is characterised in that：The fine grain aluminium hydroxide is 5 microns
550-600 parts of aluminium hydroxide, coarse grain footpath aluminium hydroxide are 20 microns of 780-850 parts of aluminium hydroxides.
A kind of 4. manufacture method of high fire-retardance heat-conducting silica gel sheet as claimed in claim 1, it is characterised in that：
A, vinyl-terminated silicone fluid is added into stirred tank successively, containing hydrogen silicone oil, acetylenic alcohol inhibitor, platinum catalyst, coupling agent, is opened
Begin to stir, mixing speed 45r/min stirrings 20min；
B, and then vacuumize and reduce rotating speed to 35r/min, be stirred 10-15min；
C, and then fine grain aluminium hydroxide is added, 2-3min is first then stirred under the rotating speed of 20r/min, then improve rotating speed extremely
30r/min is simultaneously vacuumized, and stirs 15min under vacuum conditions；
D, bromide fire retardant and antimony oxide are added, 2-3min is first stirred under the rotating speed of 20r/min, then improves rotating speed extremely
30r/min is simultaneously vacuumized, and stirs 15min under vacuum conditions；
E, coarse grain footpath aluminium hydroxide and mill base are added, 2-3min is first stirred under the rotating speed of 20r/min, then improves rotating speed extremely
30r/min is simultaneously vacuumized, and stirs 5-10min under vacuum conditions, then rotating speed is down to low speed 12-15r/min, then keeps true
Sky stirring 25min；
F, discharging calendering；
G, sulfidization molding is carried out through 130 DEG C of ovens.
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| CN109777118A (en) * | 2018-12-28 | 2019-05-21 | 东莞市汉品电子有限公司 | A kind of High-Voltage Insulation heat-conducting silica gel sheet and preparation method thereof |
| CN110317581A (en) * | 2019-06-06 | 2019-10-11 | 东莞市盛元新材料科技有限公司 | A kind of pureed thermostable heat-conductive composite material and preparation method |
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Application publication date: 20180515 |