CN108727824A - Height rebound closed pore flame-proof silicon rubber foamed material and preparation method thereof - Google Patents
Height rebound closed pore flame-proof silicon rubber foamed material and preparation method thereof Download PDFInfo
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- CN108727824A CN108727824A CN201810534903.6A CN201810534903A CN108727824A CN 108727824 A CN108727824 A CN 108727824A CN 201810534903 A CN201810534903 A CN 201810534903A CN 108727824 A CN108727824 A CN 108727824A
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- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
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Abstract
The invention discloses a kind of high rebound closed pore flame-retardant foam silastic materials, it includes:Silicon rubber 40-60%, auxiliary agent 30-50%, foaming agent 0.5 ~ 2%, crosslinking agent 1 ~ 3%, catalyst 0.5 ~ 2%, inhibitor 0.5 ~ 2%, colorant 0.5-1.5%.
Description
Technical field
The present invention relates to a kind of silicon rubber foam material and preparation method thereof more particularly to a kind of fire-retardant silicon of high rebound closed pore
Rubbery foam and preparation method thereof.
Background technology
Under the overall background such as energy restriction, environmental pollution, each automobile production enterprise is also using new-energy automobile as seizing not
Come the grand strategy direction of automobile industry commanding elevation.Core of the battery as entire new-energy automobile, environment sealing and
Damping part is also particularly important, and high resilience closed pore flame-proof silicon rubber foam can not only reduce the external shake that battery is subjected to
It is dynamic, it is ensured that battery dilation safe under cold cycling plays performance, additionally it is possible to avoid electricity to a certain extent steadily in the long term
Pond temperature is excessively high or unexpected fire occurring due to shock and explosion.However foam silicone rubber product passes through note mostly at present
The gas that enters, the chemical substance thermally decomposed in advance and chemical reaction generate gas to realize the foam structure of silica gel, main to use
Room temperature vulcanization is foamed or high temperature vulcanized foaming both methods.The former can be realized at room temperature, and formula is simple, is produced
The product come is more single, and is cured to product using the production technology for pouring molding or rubber, it is difficult to the company of realization
Continuous metaplasia production, thus product poor processability, application range also more narrow and minorityization.Such as Chinese patent CN104559190A
A kind of preparation method of two-component foamed silica gel composite material is disclosed, this method encapsulates isobutyl using shell Corvic
The microcapsules of alkane can carry out crosslinked foaming reaction as foaming agent, at room temperature mixing A, B component, which can effectively solve
Certainly existing foamed silica gel shock resistance and the poor problem of barrier propterty, but sample poor processability, it is difficult to realize serialization
Production.Although the method for high temperature vulcanized foaming can realize continuous production, crosslinking and the speed to foam matching difficult to realize,
Surface layer and internal crosslinking degree are inconsistent, thus easily lead to that abscess-size is uneven, influence sample resilience and
Other performances far can not reach the demand in market for field of shock absorption.Chinese patent CN105331117A using air,
The mixed gas of oxygen and carbon dioxide is used as foaming agent, although prepared silicon rubber foam abscess is more uniform, bubble
Hole is larger, and resilience performance is bad, and moulding process is single, therefore may be only available for industrial injection molding art.
In addition to this, the anti-flammability of silicon rubber foam is realized by adding a large amount of fire retardant, fire retardant
A large amount of additions can further influence the uniformity of abscess, cause abscess to become larger even holes, greatly reduce silicon rubber bubble
The damping performance of foam.
Invention content
Technical problem to be solved by the invention is to provide a kind of high rebound closed pore flame-proof silicon rubber foamed materials, it is adopted
Technical solution is:A kind of high rebound closed pore flame-proof silicon rubber foamed material, it is characterised in that include by weight percentage:Silicon
Rubber 40-60%, auxiliary agent 30-50%, foaming agent 0.5 ~ 2%, crosslinking agent 1 ~ 3%, catalyst 0.5 ~ 2%, inhibitor 0.5 ~ 2%, coloring
Agent 0.5-1.5%.
The further technical characteristic of the present invention is:
The silicon rubber is 107 silicon rubber(α, alpha, omega-dihydroxy methylsiloxane), end-vinyl methyl silicone rubber, ethylene methacrylic
One or more of base phenyl siloxane rubber, more vinylsiloxane rubbers;
The silicon rubber viscosity is 2000 ~ 50000 mPa.s;
The foaming agent is at least one in hydroxy silicon oil, hollow microsphere, normal heptane, sodium bicarbonate, azodicarbonamide, urea
Kind;
The auxiliary agent includes following component by weight percentage:Blowing promotor 2.5 ~ 4%, reinforcing agent 41 ~ 62%, fire retardant 30 ~
45%, intercalator 2.5 ~ 10%.The wherein described blowing promotor is four acicular type zinc oxide crystal whisker,;Reinforcing agent is gas-phase silica, precipitation
At least two in white carbon, silicon powder, diatomite, calcium carbonate, titanium dioxide;Fire retardant is aluminium hydroxide, magnesium hydroxide, three
Aoxidize at least one of two antimony;Intercalator is by long chain alkane quaternary ammonium salt treated organo montmorillonite, organo montmorillonite
Interlamellar spacing be 1.3 ~ 3.9 nm;
The crosslinking agent is at least one in containing hydrogen silicone oil, ethyl orthosilicate, cumyl peroxide, dibenzoyl peroxide
Kind;
The inhibitor be ethynylcyclohexanol, silanization alkynol, ethyl maleate, in more vinyl polysiloxanes at least
It is a kind of;
The catalyst is tin dilaurate dioctyl tin, dibutyl tin laurate, more alkoxy titanates, chloroplatinic acid, platinum-second
At least one of alkenyl siloxane complex compound;
The present invention also provides a kind of preparation methods of high rebound closed pore flame-retardant foam silastic material, it includes the following steps:
Step 1: by weight percentage by silicon rubber 40-60%, auxiliary agent 30-50%, foaming agent 0.5 ~ 2%, catalyst 0.5 ~ 2%, suppression
Preparation 0.5 ~ 2%, colorant 0.5-1.5% are added in planetary stirrer, are vacuumized at 110 DEG C -160 DEG C and 30-40 is mixed
Min stands object to be mixed and restores to room temperature;
Step 2: adding crosslinking agent 1 ~ 3% in mixture into planetary stirrer, SAPMAC method system is opened, control temperature exists
5 DEG C -10 DEG C, 10-20 min are quickly mixed and obtain spare sizing material to uniformly mixed;
Step 3: the spare sizing material obtained to step 2 respectively covers a polyester film layer and rolls through twin pressure roller calender up and down, later
Enter high temperature oven by conveyer belt, normal pressure foaming vulcanization 5-15 min is carried out at 60-120 DEG C, to molding continuous foamed
Silica gel plate is wound, and high rebound closed pore flame-retardant foam silastic material coiled material is obtained.
The wherein described auxiliary agent includes following component by weight percentage:Blowing promotor 2.5 ~ 4%, it is reinforcing agent 41 ~ 62%, fire-retardant
Agent 30 ~ 45%, intercalator 2.5 ~ 10%;The wherein described blowing promotor be four acicular type zinc oxide crystal whisker, reinforcing agent be gas-phase silica,
At least two in precipitated silica, silicon powder, diatomite, calcium carbonate, titanium dioxide;Fire retardant is aluminium hydroxide, hydroxide
At least one of magnesium, antimony oxide;Intercalator is by long chain alkane quaternary ammonium salt treated organo montmorillonite, You Jimeng
The interlamellar spacing for taking off soil is 1.3 ~ 3.9 nm.
The beneficial effects of the invention are as follows:
Intercalator in the present invention in auxiliary agent be by long chain alkane quaternary ammonium salt treated organo montmorillonite, organo montmorillonite
Interlamellar spacing is 1.3 ~ 3.9 nm;It is easily achieved stripping dispersion under high velocity agitation, silicon rubber is easy to form intercalation configuration, removes
Lamella form isolation in silicon rubber system, regular prevents from being formed and being steeped when foaming, it is thus possible to it is straight to greatly reduce abscess
Diameter promotes rate of closed hole, enhances resilience;Another aspect montmorillonite also has flame retardant property, is cooperateed with fire retardant and with can reduce
The additive amount of fire retardant, avoid a large amount of additions due to fire retardant and the phenomenon that reduce silicon rubber foam damping performance.Auxiliary agent
In blowing promotor be four acicular type zinc oxide crystal whisker, can reduce abscess-size, optimize distribution of cells;
In addition, passing through twin pressure roller calender pressure in a kind of preparation method of high rebound closed pore flame-retardant foam silastic material of the present invention
Prolong, and then accurately control the thickness of molding product, the foam silicone rubber material of different-thickness can be produced, the later stage carries out coiled material
It processes very convenient.
Specific implementation mode
Present invention firstly provides a kind of high rebound closed pore flame-proof silicon rubber foamed materials, it includes by weight percentage:Silicon
Rubber 40-60%, auxiliary agent 30-50%, foaming agent 0.5 ~ 2%, crosslinking agent 1 ~ 3%, catalyst 0.5 ~ 2%, inhibitor 0.5 ~ 2%, coloring
Agent 0.5-1.5%.
The wherein described silicon rubber is 107 silicon rubber(α, alpha, omega-dihydroxy methylsiloxane), end-vinyl methyl silicone rubber,
One or more of methyl vinyl phenyl silicon rubber, more vinylsiloxane rubbers;
The silicon rubber viscosity is 2000 ~ 50000 mPa.s;
The foaming agent is at least one in hydroxy silicon oil, hollow microsphere, normal heptane, sodium bicarbonate, azodicarbonamide, urea
Kind;
The auxiliary agent includes following component by weight percentage:Blowing promotor 2.5 ~ 4%, reinforcing agent 41 ~ 62%, fire retardant 30 ~
45%, intercalator 2.5 ~ 10%.
The blowing promotor is four acicular type zinc oxide crystal whisker;Reinforcing agent be gas-phase silica, precipitated silica, silicon powder,
At least two in diatomite, calcium carbonate, titanium dioxide;Fire retardant is aluminium hydroxide, magnesium hydroxide, in antimony oxide extremely
Few one kind;Intercalator is by long chain alkane quaternary ammonium salt treated organo montmorillonite, the interlamellar spacing of organo montmorillonite is 1.3 ~
3.9 nm;
The crosslinking agent is at least one in containing hydrogen silicone oil, ethyl orthosilicate, cumyl peroxide, dibenzoyl peroxide
Kind;
The inhibitor be ethynylcyclohexanol, silanization alkynol, ethyl maleate, in more vinyl polysiloxanes at least
It is a kind of;
The catalyst is tin dilaurate dioctyl tin, dibutyl tin laurate, more alkoxy titanates, chloroplatinic acid, platinum-second
At least one of alkenyl siloxane complex compound;
The present invention also provides a kind of preparation methods of high rebound closed pore flame-retardant foam silastic material, it includes the following steps:
Step 1: by weight percentage by silicon rubber 40-60%, auxiliary agent 30-50%, foaming agent 0.5 ~ 2%, catalyst 0.5 ~ 2%, suppression
Preparation 0.5 ~ 2%, colorant 0.5-1.5% are added in planetary stirrer, are vacuumized at 110 DEG C -160 DEG C and 30-40 is mixed
Min stands object to be mixed and restores to room temperature;
Step 2: adding crosslinking agent 1 ~ 3% in mixture into planetary stirrer, SAPMAC method system is opened, control temperature exists
5 DEG C -10 DEG C, 10-20 min are quickly mixed and obtain spare sizing material to uniformly mixed;
Step 3: the spare sizing material obtained to step 2 respectively covers a polyester film layer and rolls through twin pressure roller calender up and down, later
Enter high temperature oven by conveyer belt, normal pressure foaming vulcanization 5-15 min is carried out at 60-120 DEG C, to molding continuous foamed
Silica gel plate is wound, and high rebound closed pore flame-retardant foam silastic material coiled material is obtained.
The wherein described auxiliary agent includes following component by weight percentage:Blowing promotor 2.5 ~ 4%, it is reinforcing agent 41 ~ 62%, fire-retardant
Agent 30 ~ 45%, intercalator 2.5 ~ 10%;The wherein described blowing promotor be four acicular type zinc oxide crystal whisker, reinforcing agent be gas-phase silica,
At least two in precipitated silica, silicon powder, diatomite, calcium carbonate, titanium dioxide;Fire retardant is aluminium hydroxide, hydroxide
At least one of magnesium, antimony oxide;Intercalator is by long chain alkane quaternary ammonium salt treated organo montmorillonite, You Jimeng
The interlamellar spacing for taking off soil is 1.3 ~ 3.9 nm.
With reference to embodiment to the present invention it is a kind of it is high rebound closed pore flame-retardant foam silastic material preparation method do into
One step is described in detail.
Embodiment 1
Step 1: by weight percentage by silicon rubber 40%, auxiliary agent 50%, foaming agent 2%, catalyst 2%, inhibitor 2%, colorant
1% is added in planetary stirrer, is vacuumized at 110 DEG C and 40 min are mixed, stood object to be mixed and restore to room temperature;
Step 2: adding crosslinking agent 3% in mixture into planetary stirrer, SAPMAC method system is opened, control temperature is 5
DEG C, 20 min are quickly mixed and obtain spare sizing material to uniformly mixed;
Step 3: the spare sizing material obtained to step 2 respectively covers a polyester film layer and rolls through twin pressure roller calender up and down, later
Enter high temperature oven by conveyer belt, normal pressure foaming 15 min of vulcanization is carried out at 60 DEG C, to molding continuous foamed silica gel plate
It is wound, obtains high rebound closed pore flame-retardant foam silastic material coiled material.
Embodiment 2
Step 1: by weight percentage by silicon rubber 60%, auxiliary agent 30%, foaming agent 2%, catalyst 2%, inhibitor 2%, colorant
1% is added in planetary stirrer, is vacuumized at 160 DEG C and 30 min are mixed, stood object to be mixed and restore to room temperature;
Step 2: adding crosslinking agent 3% in mixture into planetary stirrer, SAPMAC method system is opened, control temperature is 10
DEG C, 10 min are quickly mixed and obtain spare sizing material to uniformly mixed;
Step 3: the spare sizing material obtained to step 2 respectively covers a polyester film layer and rolls through twin pressure roller calender up and down, later
Enter high temperature oven by conveyer belt, normal pressure foaming 5 min of vulcanization is carried out at 120 DEG C, to molding continuous foamed silica gel plate
It is wound, obtains high rebound closed pore flame-retardant foam silastic material coiled material.
Embodiment 3
Step 1: by weight percentage by silicon rubber 55%, auxiliary agent 40%, foaming agent 0.5%, catalyst 1%, inhibitor 1%, coloring
Agent 0.5% is added in planetary stirrer, is vacuumized at 140 DEG C and 35 min are mixed, stood object to be mixed and restore to room temperature;
Step 2: adding crosslinking agent 2% in mixture into planetary stirrer, SAPMAC method system is opened, control temperature is 7
DEG C, 15 min are quickly mixed and obtain spare sizing material to uniformly mixed;
Step 3: the spare sizing material obtained to step 2 respectively covers a polyester film layer and rolls through twin pressure roller calender up and down, later
Enter high temperature oven by conveyer belt, normal pressure foaming 10 min of vulcanization is carried out at 100 DEG C, to molding continuous foamed silica gel plate
It is wound, obtains high rebound closed pore flame-retardant foam silastic material coiled material.
Embodiment 4
Step 1: by weight percentage by silicon rubber 50%, auxiliary agent 45%, foaming agent 1.5%, catalyst 0.5%, inhibitor 0.5%,
Colorant 1.5% is added in planetary stirrer, is vacuumized at 150 DEG C and 33 min are mixed, stood object to be mixed and restore to room
Temperature;
Step 2: adding crosslinking agent 1% in mixture into planetary stirrer, SAPMAC method system is opened, control temperature is 8
DEG C, 12 min are quickly mixed and obtain spare sizing material to uniformly mixed;
Step 3: the spare sizing material obtained to step 2 respectively covers a polyester film layer and rolls through twin pressure roller calender up and down, later
Enter high temperature oven by conveyer belt, normal pressure foaming 12 min of vulcanization is carried out at 90 DEG C, to molding continuous foamed silica gel plate
It is wound, obtains high rebound closed pore flame-retardant foam silastic material coiled material.
In above-mentioned all embodiments, the silicon rubber is 107 silicon rubber(α, alpha, omega-dihydroxy methylsiloxane), end ethylene
One or more of ylmethyl silicon rubber, methyl vinyl phenyl silicon rubber, more vinylsiloxane rubbers;The silicon rubber viscosity
For 2000 ~ 50000 mPa.s.
The foaming agent be hydroxy silicon oil, hollow microsphere, normal heptane, sodium bicarbonate, azodicarbonamide, in urea extremely
Few one kind;
The auxiliary agent includes following component by weight percentage:Blowing promotor 2.5 ~ 4%, reinforcing agent 41 ~ 62%, fire retardant 30 ~
45%, intercalator 2.5 ~ 10%.The wherein described blowing promotor is four acicular type zinc oxide crystal whisker;Reinforcing agent is gas-phase silica, precipitation
At least two in white carbon, silicon powder, diatomite, calcium carbonate, titanium dioxide;Fire retardant is aluminium hydroxide, magnesium hydroxide, three
Aoxidize at least one of two antimony;Intercalator is by long chain alkane quaternary ammonium salt treated organo montmorillonite, organo montmorillonite
Interlamellar spacing be 1.3 ~ 3.9 nm.
The crosslinking agent be containing hydrogen silicone oil, ethyl orthosilicate, cumyl peroxide, in dibenzoyl peroxide at least
It is a kind of.
The inhibitor is in ethynylcyclohexanol, silanization alkynol, ethyl maleate, more vinyl polysiloxanes
It is at least one.
The catalyst be tin dilaurate dioctyl tin, dibutyl tin laurate, more alkoxy titanates, chloroplatinic acid,
At least one of platinum-vinyl siloxane complex compound.
Intercalator in the present invention in auxiliary agent is used by long chain alkane quaternary ammonium salt treated organo montmorillonite, You Jimeng
The interlamellar spacing for taking off soil is 1.3 ~ 3.9 nm;It is easily achieved stripping dispersion under high velocity agitation, silicon rubber is easy to form intercalation knot
The lamella of structure, stripping forms isolation in silicon rubber system, and regular prevents from being formed and being steeped when foaming, it is thus possible to greatly reduce
Cell diameter promotes rate of closed hole, enhances resilience;Another aspect montmorillonite also has flame retardant property, cooperates with and is used in combination with fire retardant
The additive amount that fire retardant can be reduced avoids due to a large amount of additions of fire retardant and reduces showing for silicon rubber foam damping performance
As.Blowing promotor in auxiliary agent is four acicular type zinc oxide crystal whisker, can reduce abscess-size, optimizes distribution of cells.
In addition, being rolled by twin pressure roller in a kind of preparation method of high rebound closed pore flame-retardant foam silastic material of the present invention
Machine rolls, and then accurately controls the thickness of molding product, can produce the foam silicone rubber material of different-thickness, the later stage is to coiled material
It is processed very convenient.
Above example is merely to illustrate the present invention and not limits, and the present invention is also not limited only to above-mentioned example, all
Technical solution and its improvement for not departing from the spirit and scope of the present invention, should be included in scope of the presently claimed invention.
Claims (10)
1. a kind of high rebound closed pore flame-retardant foam silastic material, it is characterised in that include by weight percentage:Silicon rubber 40-
60%, auxiliary agent 30-50%, foaming agent 0.5 ~ 2%, crosslinking agent 1 ~ 3%, catalyst 0.5 ~ 2%, inhibitor 0.5 ~ 2%, colorant 0.5-
1.5%。
2. high rebound closed pore flame-retardant foam silastic material according to claim 1, it is characterised in that:The silicon rubber is
107 silicon rubber(α, alpha, omega-dihydroxy methylsiloxane), end-vinyl methyl silicone rubber, methyl vinyl phenyl silicon rubber, more second
One or more of alkenyl silicon rubber, wherein the silicon rubber viscosity is 2000 ~ 50000 mPa.s.
3. high rebound closed pore flame-retardant foam silastic material according to claim 1, it is characterised in that:The foaming agent is
At least one of hydroxy silicon oil, hollow microsphere, normal heptane, sodium bicarbonate, azodicarbonamide, urea.
4. high rebound closed pore flame-retardant foam silastic material according to claim 1, it is characterised in that:The auxiliary agent is by weight
It includes following component to measure percentage:Blowing promotor 2.5 ~ 4%, reinforcing agent 41 ~ 62%, fire retardant 30 ~ 45%, intercalator 2.5 ~ 10%.
5. high rebound closed pore flame-retardant foam silastic material according to claim 4, it is characterised in that:The blowing promotor
For four acicular type zinc oxide crystal whisker, reinforcing agent is gas-phase silica, precipitated silica, silicon powder, diatomite, calcium carbonate, titanium dioxide
At least two in titanium;Fire retardant is at least one of aluminium hydroxide, magnesium hydroxide, antimony oxide;Intercalator is to pass through
The interlamellar spacing of long chain alkane quaternary ammonium salt treated organo montmorillonite, organo montmorillonite is 1.3 ~ 3.9 nm.
6. high rebound closed pore flame-retardant foam silastic material according to claim 1, it is characterised in that:The crosslinking agent is
At least one of containing hydrogen silicone oil, ethyl orthosilicate, cumyl peroxide, dibenzoyl peroxide.
7. high rebound closed pore flame-retardant foam silastic material according to claim 1, it is characterised in that:The inhibitor is
At least one of silanization alkynol, ethynylcyclohexanol, ethyl maleate, more vinyl polysiloxanes.
8. high rebound closed pore flame-retardant foam silastic material according to claim 1, it is characterised in that:The catalyst is
Tin dilaurate dioctyl tin, dibutyl tin laurate, more alkoxy titanates, chloroplatinic acid, platinum-vinyl siloxane complex compound
At least one of.
9. a kind of preparation method of high rebound closed pore flame-retardant foam silastic material, it is characterised in that include the following steps:
Step 1: by weight percentage by silicon rubber 40-60%, auxiliary agent 30-50%, foaming agent 0.5 ~ 2%, catalyst 0.5 ~ 2%, suppression
Preparation 0.5 ~ 2%, colorant 0.5-1.5% are added in planetary stirrer, are vacuumized at 110 DEG C -160 DEG C and 30-40 is mixed
Min stands object to be mixed and restores to room temperature;
Step 2: adding crosslinking agent 1 ~ 3% in mixture into planetary stirrer, SAPMAC method system is opened, control temperature exists
5 DEG C -10 DEG C, 10-20 min are quickly mixed and obtain spare sizing material to uniformly mixed;
Step 3: the spare sizing material obtained to step 2 respectively covers a polyester film layer and rolls through twin pressure roller calender up and down, later
Enter high temperature oven by conveyer belt, normal pressure foaming vulcanization 5-15 min is carried out at 60-120 DEG C, to molding continuous foamed
Silica gel plate is wound, and high rebound closed pore flame-retardant foam silastic material coiled material is obtained.
10. the preparation method of high rebound closed pore flame-retardant foam silastic material according to claim 9, it is characterised in that:
The auxiliary agent includes following component by weight percentage:Blowing promotor 2.5 ~ 4%, reinforcing agent 41 ~ 62%, are inserted fire retardant 30 ~ 45%
Layer agent 2.5 ~ 10%;The wherein described blowing promotor be four acicular type zinc oxide crystal whisker, reinforcing agent be gas-phase silica, precipitated silica,
At least two in silicon powder, diatomite, calcium carbonate, titanium dioxide;Fire retardant is aluminium hydroxide, magnesium hydroxide, three oxidations two
At least one of antimony;Intercalator is by long chain alkane quaternary ammonium salt treated organo montmorillonite, the interlayer of organo montmorillonite
Away from for 1.3 ~ 3.9 nm.
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