CN108948744A - A kind of waterproof Ceramic silicon rubber material, preparation method and applications - Google Patents
A kind of waterproof Ceramic silicon rubber material, preparation method and applications Download PDFInfo
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- CN108948744A CN108948744A CN201810457903.0A CN201810457903A CN108948744A CN 108948744 A CN108948744 A CN 108948744A CN 201810457903 A CN201810457903 A CN 201810457903A CN 108948744 A CN108948744 A CN 108948744A
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- H—ELECTRICITY
- H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
- H02G—INSTALLATION OF ELECTRIC CABLES OR LINES, OR OF COMBINED OPTICAL AND ELECTRIC CABLES OR LINES
- H02G1/00—Methods or apparatus specially adapted for installing, maintaining, repairing or dismantling electric cables or lines
- H02G1/14—Methods or apparatus specially adapted for installing, maintaining, repairing or dismantling electric cables or lines for joining or terminating cables
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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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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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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
- 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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- C—CHEMISTRY; METALLURGY
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- 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
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Abstract
The present invention discloses a kind of waterproof Ceramic silicon rubber material, comprising: at porcelain filling, silicon rubber, silicone oil, boron oxide, coupling agent, vulcanizing agent；It include: silicon powder, mica, silica at porcelain filling.Preparation method include: after (1) grinds silicon powder again with it is other mixed at porcelain filling component, drying, obtain pretreated at porcelain filling；(2) whole components outside at porcelain filling, vulcanizing agent are mixed, is kneaded, pumping vacuum and mixing obtains organic silicon compounded rubber stock；(3) it is kneaded pretreated at porcelain filling and organic silicon compounded rubber stock；(4) vulcanizing agent is added to be kneaded.This waterproof Ceramic silicon rubber has good mechanical property at normal temperature, it is low at porcelain temperature and can environment temperature be 300-400 DEG C when not crack, at the ceramic body being converted to after porcelain, waterproof performance is good due to compact texture.Its application includes: a kind of cable fixing head, has the flame retardant coating made of waterproof Ceramic silicon rubber material, and stable mechanical property still has waterproofness under high temperature.
Description
Technical field
The present invention relates to ceramic polymer arts, and in particular to a kind of waterproof Ceramic silicon rubber material, preparation method
And its application.
Background technique
Cable fixing head also known as Waterproof connector of cable, cable connector, be widely used in mechanical equipment electrical, marine electrical equipment,
The fixation and protection of the wire and cable of corrosion protection equipment, main function are that cable outlet hole is made to keep sealing and water proof and dust proof, in turn
It causes a machine to safely and reliably run.Currently, cable fixing head mostly uses rubber material, but rubber material non-refractory, no
Resistance to burning, there are huge security risk, limits their use when there is fire or other high temperature accidents.Therefore, it opens
The cable fixing head material for sending out to have flame retarding function a kind of becomes project urgently to be resolved, and Ceramic silicon rubber material is to realize this
A little purposes provide possibility.
Ceramic silicon rubber material is a kind of novel polymer composite, and easy to process, production cost is low, in room temperature
Under it is nontoxic, tasteless, there is good flexibility and elasticity, when contacting flame can ablation be converted to the shell of ceramic-like, and
It is not to be burnt into powdery ashes, the shell of the ceramic-like forms one layer of hard protective layer, which stops the continuation of flame
Burning is played the role of completely cutting off extraneous flame, so that the object that protection is burnt is not damaged, the ablation time is longer, and temperature is higher,
Shell is harder.
But Ceramic silicon rubber material still has some problems in the use as cable fixing head.One, occur
The temperature of ceramic reaction is excessively high, and generally at 650 DEG C or more, and silicone rubber matrix will degrade at 200 DEG C or more, if
For environment temperature between 200-650 DEG C, silicone rubber matrix has occurred and that degradation, not yet occurs into porcelainization reaction, it is more likely that
Cable fixing head cracking, mechanical property is caused to reduce, the performances such as sealing, waterproof and dustproof go wrong, and it is safe and reliable to influence machine
Ground operation.Two, the ceramic body being converted to after Ceramic silicon rubber porcelainization is in itself although hard have self-supporting
It is porous, it is not fine and close, poor waterproof properties, when water leaching occurs in scene of fire, water is likely to directly through electricity
Cable fixing head infilters among cable outlet hole, influences machine and safely and reliably runs.
Application publication number discloses one kind for the Chinese invention patent of CN104629375A can ceramic fireproof silicon rubber
Glue is made by the raw material for including organic silicon compounded rubber stock and ceramic powder, and organic silicon compounded rubber stock is by including silicon raw rubber, gas phase two
The raw material of silica, antistructurizing agent and ceramic modifier is made, and the molecular formula of ceramic modifier is Fe (CO)3[(CH2
=CHMe2SiO)3SiR], R is methyl or phenyl.This Ceramic silicon rubber, the degradation temperature of silicone rubber matrix main body is 350
DEG C or so, ceramic reaction will occur at 350 DEG C or more, not only have preferable high-temperature flame-proof performance, remain to protect at 350 DEG C
Hold certain mechanics and insulation performance.But there are a large amount of porous structures for the ceramic body that is converted to of this material, are not fine and close
, poor waterproof properties；Moreover, what although the degradation temperature of silicone rubber matrix main body occurred in 350 DEG C or so and ceramic reaction
Temperature relatively, when environment temperature is at 300-400 DEG C, still will appear cracking, mechanical property reduction, cable caused to be fixed
The performances such as sealing, the waterproof and dustproof of head go wrong；In addition, the ceramic modifier structure preparation process used is complicated, price
It is expensive, at high cost.
Summary of the invention
It is an object of the present invention to be directed to the above-mentioned deficiency of the prior art, propose a kind of ceramic body being converted to because
With compact texture waterproof performance it is good, it is low at porcelain temperature and can environment temperature be 300-400 DEG C when still keep preferable power
Learn the waterproof Ceramic silicon rubber material of performance.
The present invention solve technical problem the technical solution adopted is that, a kind of waterproof Ceramic silicon rubber material is proposed, by matter
Measure part meter, comprising:
At 30-100 parts of porcelain filling, described include mass ratio at porcelain filling is (40-100): (20-100): the silicon powder of (20-80),
Mica and silica；The partial size of the silicon powder is less than 3 μm；
60-100 parts of silicon rubber, the silicon rubber general formula is (RnSiO(4-n)/2)m, R is carbon containing organic group, and n is to connect on silicon atom
Carbon containing organic radix, and n be 1,2 or 3, m is the degree of polymerization, m >=2；
2-30 parts of silicone oil；
15-80 parts of boron oxide；
0.1-15 parts of coupling agent；Preferably, the coupling agent is silane coupling agent；
0.1-10 parts of vulcanizing agent；Preferably, the vulcanizing agent is bis 25 vulcanizing agent.
Preferably, described at porcelain filling further include: acicular wollastonite, the quality of the acicular wollastonite and the silicon powder
Than for 0.2-0.35；The mass ratio of aluminosilicate fibre, the aluminosilicate fibre and the wollastonite is 0.4-0.6.
Preferably, the partial size at silicon powder in porcelain filling is 20-30nm.
Preferably, it is (15-30): (40-75) that the silicon rubber, which includes: mass ratio: the methyl silicone rubber of (15-50),
The methyl vinyl phenyl silicon rubber of the methyl vinyl silicone rubber of ethenyl blocking, methyl blocking；The first of the methyl blocking
In base ethenylphenyl silicon rubber, the molar ratio of phenyl and silicon atom is 0.25-0.35.
Preferably, it is (10-15): (20-35) that the methyl vinyl silicone rubber of the ethenyl blocking, which includes: mass ratio,
: the vinyl mass content of (10-15) is respectively the ethenyl blocking of 0.26-0.28%, 0.21-0.23%, 0.12-0.15%
Methyl vinyl silicone rubber.
Preferably, the partial size at mica in porcelain filling is 3-30 μm.
Preferably, the waterproof Ceramic silicon rubber material further includes aluminium dihydrogen phosphate, the aluminium dihydrogen phosphate and institute
The mass ratio for stating silicon rubber is 0.1-0.15.
It is another object of the present invention to propose a kind of above-mentioned waterproof ceramic for the above-mentioned deficiency of the prior art
The preparation method of silastic material, including the following steps:
Step 1: grinding 0.5-1h for silicon powder, then mix with all other at porcelain filling component, continues to grind 1.5-2.5h, so
2-6h is dried at 100-160 DEG C afterwards, is obtained pretreated at porcelain filling；
Step 2: it will be mixed in addition at whole components other than porcelain filling, vulcanizing agent, be warming up to 70-100 DEG C of mixing 1-1.5h；
It is warming up to 155-170 DEG C again, pumping vacuum and mixing 1.5-2.5 hours, obtains organic silicon compounded rubber stock；During the pumping vacuum and mixing
Holding vacuum degree is (- 0.1)-(- 0.05) MPa；
Step 3: pretreated be added in organic silicon compounded rubber stock at porcelain filling is mixed, in 25-90 DEG C of mixing 0.5-1.5h,
Form the ceramic rubber of bulk, natural cooling；
Step 4: the ceramic rubber of the bulk after cooling through open mill it is thin it is logical after, vulcanizing agent is added and is kneaded 0.5-1h, obtains
To waterproof Ceramic silicon rubber material.
Preferably, drying temperature is 125-135 DEG C in the step 1.
Preferably, melting temperature is 45-55 DEG C in the step 3.
It is another object of the present invention to propose a kind of cable fixing head, have for the above-mentioned deficiency of the prior art
Flame retardant coating, the flame retardant coating are made of above-mentioned waterproof Ceramic silicon rubber material.
A kind of waterproof Ceramic silicon rubber material provided by the invention has the following beneficial effects:
1, the silicon powder using partial size less than 3 μm is as the important component at porcelain filling, on the one hand, since the partial size of silicon powder is in micro-nano
Scale, silicon powder can fill up the hole that ceramic reaction generates as spackling, and the material after reacting ceramic has certain
Compactness, can prevent the infiltration of hydrone, oxygen molecule to a certain extent, promoted the waterproof of material after ceramic reaction,
Flame retardant property；On the other hand, the silicon powder large specific surface area of micro/nano-scale, reactivity is very high, when temperature rises to 300 DEG C,
The edge of silicon powder particle begins to melt, and the mica particles, silica dioxide granule, silicone rubber matrix for penetrating into surrounding, which decompose, to be generated
Silica dioxide granule in, it is adhered to one another at porcelain, it is very low at porcelain temperature, efficiently solve 300 DEG C or so silicone rubber matrix and start
Degradation and ceramic reaction at this time not yet occurs and causes what Ceramic silicon rubber material cracks, mechanical property were greatly reduced to ask
Topic.
2, at acicular wollastonite and aluminosilicate fibre are added in porcelain filling, since the silicon powder of the two and micro/nano-scale generates
Synergistic effect, the compactness of material is more preferable after ceramic, improves the waterproof performance of material after ceramic reaction.
3, at the partial size of silicon powder in porcelain filling be 20-30nm when, silicon powder partial size appropriate ensures good filling perforation effect,
Waterproof, flame retardant property are good；Moreover, 250 DEG C or more silicon powders begin to penetrate into the particle on periphery, it is lower at porcelain temperature.
4, it is (15-30): (40-75): methyl silicone rubber, the ethenyl blocking of (15-50) that silicon rubber, which includes: mass ratio,
The methyl vinyl phenyl silicon rubber of methyl vinyl silicone rubber, methyl blocking；Moreover, the methyl vinyl phenyl of methyl blocking
In silicon rubber, the molar ratio of phenyl and silicon atom is 0.25-0.35；The silicon rubber of optimization matches, and makes Ceramic silicon rubber matrix
Degradation temperature be promoted to 300 DEG C or so.
5, it is (10-15): (20-35): (10-15's) that the methyl vinyl silicone rubber of ethenyl blocking, which includes: mass ratio,
Vinyl mass content is respectively the methyl ethylene of the ethenyl blocking of 0.26-0.28%, 0.21-0.23%, 0.12-0.15%
Silicon rubber, said ratio make the degradation temperature of Ceramic silicon rubber matrix further be promoted to 350 DEG C or so.
It 6, is 3-30 μm at the partial size of mica in porcelain filling, on the one hand, since the partial size of mica itself is small, make anti-ceramic water
The mechanical property of SiClx rubber gets a promotion, and on the other hand, there are an order of magnitude for the partial size and the partial size of silicon powder for keeping mica
The gap of left and right, silicon powder can preferably play filling effect, and the compactness at material after porcelain is more preferable.
7, waterproof Ceramic silicon rubber material further includes aluminium dihydrogen phosphate, and the mass ratio of aluminium dihydrogen phosphate and silicon rubber is
0.1-0.15 introduces aluminium dihydrogen phosphate, improves the mechanical properties such as the tensile strength of Ceramic silicon rubber.
A kind of preparation method of waterproof Ceramic silicon rubber material provided by the invention has the following beneficial effects:
1, it differs larger at porcelain filling component partial size with other due to the silicon powder of micro/nano-scale, it is individually first ground into 0.5-1h,
Ensure itself enough dispersibility, then with it is other mixed at porcelain filling, can be reunited to avoid the silicon powder of micro/nano-scale due to itself
And it is difficult to sufficiently mixed among the gap of other component particles, the silicon powder filling effect of micro/nano-scale is given full play to, so that
The waterproof Ceramic silicon rubber material being finally prepared mechanical property at various temperatures, at material after porcelain compactness more
It is good.
2, the temperature dried in Optimization Steps one is 125-135 DEG C, and promotion temperature accelerates drying rate as far as possible, while really
Protect material property.Because drying temperature is excessively high, it will lead to silicon powder itself and aoxidize, between silicon powder, silicon powder and other at porcelain filling group
/ residual adhesion can occur, the partial size for being equivalent to silicon powder itself is bigger, it is difficult to give full play to the small advantage of silicon powder partial size
(filling effect).
3, melting temperature is 45-55 DEG C in Optimization Steps three, the energy saving as far as possible while ensuring melting effect.
A kind of cable fixing head provided by the invention has the following beneficial effects:
1, there is good mechanical property 250 DEG C or less, while there is very strong fire resistance, flame retardant coating can be sent out at high temperature
Green reacts to form one layer of hard protective layer, which stops burning away for flame, plays and completely cuts off extraneous flame
Effect, so that the object that protection is burnt is not damaged, the ablation time is longer, and temperature is higher, and shell is harder.
2, flame retardant coating still keeps preferable mechanical property at 300-400 DEG C, does not crack, it is ensured that cable fixing head sealing electricity
Cable outlet hole and water proof and dust proof, and then cause a machine to safely and reliably run.
3, there is good waterproof performance, the protective layer that flame retardant coating occurs to be formed after porcelainization reaction has densification under high temperature
Property, hydrone is difficult to infilter across flame retardant coating among cable outlet hole, it is ensured that machine is safely and reliably run.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention will be further described, but the present invention is simultaneously
It is not limited to these embodiments.
Embodiment 1
Waterproof Ceramic silicon rubber, is prepared using following methods:
Step 1: the silicon powder 40g that average grain diameter is 1 μm is ground into 1h, then the mica 20g with average grain diameter for 300 μm, titanium dioxide
Silicon 20g, acicular wollastonite 8g, aluminosilicate fibre 3.2g mixing, continue to grind 1.5h, then dry 6h at 100 DEG C, obtain
It is pretreated at porcelain filling.
Step 2: by silicon rubber (i.e. silicon raw rubber) 60g, silicone oil 2g, boron oxide 15g, silane coupling agent 0.1g, biphosphate
Aluminium 6g mixing, is warming up to 70 DEG C of mixing 1.5h；Methyl silicone rubber that silicon rubber is 15: 40: 15 by mass ratio, ethenyl blocking
The methyl vinyl phenyl silicon rubber composition of methyl vinyl silicone rubber, methyl blocking, wherein the methyl ethylene of methyl blocking
The molar ratio of phenyl and silicon atom is 0.25-0.35 in phenyl siloxane rubber；The methyl vinyl silicone rubber of ethenyl blocking is by matter
The vinyl mass content that amount ratio is 10: 20: 10 is respectively the vinyl of 0.26-0.28%, 0.21-0.23%, 0.12-0.15%
The methyl vinyl silicone rubber of sealing end forms.
It is warming up to 155 DEG C again, pumping vacuum and mixing 2.5 hours, obtains organic silicon compounded rubber stock；It is kept during pumping vacuum and mixing
Vacuum degree is (- 0.1)-(- 0.05) MPa.
Step 3: pretreated be added in organic silicon compounded rubber stock at porcelain filling is mixed, and in 25 DEG C of mixing 1.5h, is formed
The ceramic rubber of bulk, natural cooling；
Step 4: the ceramic rubber of the bulk after cooling through open mill it is thin it is logical after, it is mixed that 0.1g bis 25 vulcanizing agent is added
0.5h is refined, waterproof Ceramic silicon rubber material is obtained.
Embodiment 2
Waterproof Ceramic silicon rubber, is prepared using following methods:
Step 1: the silicon powder 40g that average grain diameter is 20nm is ground into 0.5h, then mica 100g, dioxy with average grain diameter for 3 μm
SiClx 80g, acicular wollastonite 14g, aluminosilicate fibre 8.4g mixing, continue to grind 2.5h, then dry 2h at 160 DEG C,
It obtains pretreated at porcelain filling.
Step 2: by silicon rubber (i.e. silicon raw rubber) 60g, silicone oil 30g, boron oxide 80g, silane coupling agent 15g, biphosphate
Aluminium 9g mixing, is warming up to 100 DEG C of mixing 1h；Methyl silicone rubber that silicon rubber is 15: 75: 50 by mass ratio, ethenyl blocking
The methyl vinyl phenyl silicon rubber composition of methyl vinyl silicone rubber, methyl blocking, wherein the methyl ethylene of methyl blocking
The molar ratio of phenyl and silicon atom is 0.25-0.35 in phenyl siloxane rubber；The methyl vinyl silicone rubber of ethenyl blocking is by matter
The vinyl mass content that amount ratio is 10: 35: 15 is respectively the vinyl of 0.26-0.28%, 0.21-0.23%, 0.12-0.15%
The methyl vinyl silicone rubber of sealing end forms.
It is warming up to 170 DEG C again, pumping vacuum and mixing 1.5 hours, obtains organic silicon compounded rubber stock；It is kept during pumping vacuum and mixing
Vacuum degree is (- 0.1)-(- 0.05) MPa.
Step 3: pretreated be added in organic silicon compounded rubber stock at porcelain filling is mixed, and in 90 DEG C of mixing 0.5h, is formed
The ceramic rubber of bulk, natural cooling；
Step 4: the ceramic rubber of the bulk after cooling through open mill it is thin it is logical after, 10g bis 25 vulcanizing agent is added and is kneaded
1h obtains waterproof Ceramic silicon rubber material.
Embodiment 3
Waterproof Ceramic silicon rubber, is prepared using following methods:
Step 1: by average grain diameter be 30nm silicon powder 40g grind 0.65h, then with average grain diameter be 30 μm mica 60g, two
Silica 50g, acicular wollastonite 14g, aluminosilicate fibre 5.6g mixing, continue to grind 1.75h, then dry at 125 DEG C
3h is obtained pretreated at porcelain filling.
Step 2: by silicon rubber (i.e. silicon raw rubber) 60g, silicone oil 16g, boron oxide 47.5g, silane coupling agent 7.55g, phosphoric acid
Aluminum dihydrogen 7.5g mixing, is warming up to 80 DEG C of mixing 1.15h；Silicon rubber by mass ratio be 15: 57.5: 32.5 methyl silicone rubber,
The methyl vinyl silicone rubber of ethenyl blocking, the methyl vinyl phenyl silicon rubber of methyl blocking form, wherein methyl blocking
Methyl vinyl phenyl silicon rubber in the molar ratio of phenyl and silicon atom be 0.25-0.35；The ethylene methacrylic of ethenyl blocking
Base silicon rubber by mass ratio be 10: 27.5: 12.5 vinyl mass content be respectively 0.26-0.28%, 0.21-0.23%,
The methyl vinyl silicone rubber of the ethenyl blocking of 0.12-0.15% forms.
It is warming up to 160 DEG C again, pumping vacuum and mixing 1.75 hours, obtains organic silicon compounded rubber stock；It is protected during pumping vacuum and mixing
Holding vacuum degree is (- 0.1)-(- 0.05) MPa.
Step 3: pretreated be added in organic silicon compounded rubber stock at porcelain filling is mixed, in 45 DEG C of mixing 0.75h, shape
At the ceramic rubber of bulk, natural cooling；
Step 4: the ceramic rubber of the bulk after cooling through open mill it is thin it is logical after, it is mixed that 2.5g bis 25 vulcanizing agent is added
0.65h is refined, waterproof Ceramic silicon rubber material is obtained.
Embodiment 4
Waterproof Ceramic silicon rubber, is prepared using following methods:
Step 1: by average grain diameter be 25nm silicon powder 100g grind 0.75h, then with average grain diameter be 10 μm mica 20g, two
Silica 20g, acicular wollastonite 27.5g, aluminosilicate fibre 13.75g mixing, continue to grind 2h, then dry at 135 DEG C
4h is obtained pretreated at porcelain filling.
Step 2: by silicon rubber (i.e. silicon raw rubber) 100g, silicone oil 2g, boron oxide 15g, silane coupling agent 0.1g, di(2-ethylhexyl)phosphate
Hydrogen aluminium 10g mixing, is warming up to 90 DEG C of mixing 1.25h；Silicon rubber by mass ratio be 30: 40: 15 methyl silicone rubber, vinyl seal
The methyl vinyl silicone rubber at end, the methyl vinyl phenyl silicon rubber of methyl blocking form, wherein the methyl second of methyl blocking
The molar ratio of phenyl and silicon atom is 0.25-0.35 in alkenyl phenyl siloxane rubber；The methyl vinyl silicone rubber of ethenyl blocking
It is respectively the second of 0.26-0.28%, 0.21-0.23%, 0.12-0.15% by the vinyl mass content that mass ratio is 15: 20: 10
The methyl vinyl silicone rubber composition of alkenyl sealing end.
It is warming up to 165 DEG C again, pumping vacuum and mixing 2.25 hours, obtains organic silicon compounded rubber stock；It is protected during pumping vacuum and mixing
Holding vacuum degree is (- 0.1)-(- 0.05) MPa.
Step 3: pretreated be added in organic silicon compounded rubber stock at porcelain filling is mixed, in 55 DEG C of mixing 1.25h, shape
At the ceramic rubber of bulk, natural cooling；
Step 4: the ceramic rubber of the bulk after cooling through open mill it is thin it is logical after, it is mixed that 7.5g bis 25 vulcanizing agent is added
0.85h is refined, waterproof Ceramic silicon rubber material is obtained.
Embodiment 5
Waterproof Ceramic silicon rubber, is prepared using following methods:
Step 1: by average grain diameter be 0.3 μm silicon powder 70g grind 0.9h, then with average grain diameter be 20 μm mica 20g, two
Silica 20g, acicular wollastonite 21g, aluminosilicate fibre 11g mixing, continue to grind 2.25h, then dry at 130 DEG C
5h is obtained pretreated at porcelain filling.
Step 2: by silicon rubber (i.e. silicon raw rubber) 80g, silicone oil 15g, boron oxide 40g, silane coupling agent 3g, biphosphate
Aluminium 10g mixing, is warming up to 85 DEG C of mixing 1.4h；Silicon rubber by mass ratio be 22.5: 60: 35 methyl silicone rubber, vinyl seal
The methyl vinyl silicone rubber at end, the methyl vinyl phenyl silicon rubber of methyl blocking form, wherein the methyl second of methyl blocking
The molar ratio of phenyl and silicon atom is 0.25-0.35 in alkenyl phenyl siloxane rubber；The methyl vinyl silicone rubber of ethenyl blocking
It is respectively 0.26-0.28%, 0.21-0.23%, 0.12-0.15% by the vinyl mass content that mass ratio is 12.5: 28: 13
The methyl vinyl silicone rubber of ethenyl blocking forms.
It is warming up to 162.5 DEG C again, pumping vacuum and mixing 2 hours, obtains organic silicon compounded rubber stock；It is kept during pumping vacuum and mixing
Vacuum degree is (- 0.1)-(- 0.05) MPa.
Step 3: pretreated be added in organic silicon compounded rubber stock at porcelain filling is mixed, in 50 DEG C of mixing 1h, the group of being formed
The ceramic rubber of shape, natural cooling；
Step 4: the ceramic rubber of the bulk after cooling through open mill it is thin it is logical after, 5g bis 25 vulcanizing agent is added and is kneaded
0.75h obtains waterproof Ceramic silicon rubber material.
Embodiment 6
Waterproof Ceramic silicon rubber, is prepared using following methods:
Step 1: the silicon powder 70g that average grain diameter is 25nm is ground into 1h, then the mica 60g with average grain diameter for 15 μm, titanium dioxide
Silicon 50g, acicular wollastonite 21g, aluminosilicate fibre 11g mixing, continue to grind 2.5h, then dry 4h at 130 DEG C, obtain
It is pretreated at porcelain filling.
Step 2: by silicon rubber (i.e. silicon raw rubber) 80g, silicone oil 15g, boron oxide 40g, silane coupling agent 3g, biphosphate
Aluminium 10g mixing, is warming up to 90 DEG C of mixing 1.5h；Silicon rubber by mass ratio be 22.5: 60: 35 methyl silicone rubber, vinyl seal
The methyl vinyl silicone rubber at end, the methyl vinyl phenyl silicon rubber of methyl blocking form, wherein the methyl second of methyl blocking
The molar ratio of phenyl and silicon atom is 0.25-0.35 in alkenyl phenyl siloxane rubber；The methyl vinyl silicone rubber of ethenyl blocking
It is respectively 0.26-0.28%, 0.21-0.23%, 0.12-0.15% by the vinyl mass content that mass ratio is 12.5: 28: 13
The methyl vinyl silicone rubber of ethenyl blocking forms.
It is warming up to 162.5 DEG C again, pumping vacuum and mixing 2 hours, obtains organic silicon compounded rubber stock；It is kept during pumping vacuum and mixing
Vacuum degree is (- 0.1)-(- 0.05) MPa.
Step 3: pretreated be added in organic silicon compounded rubber stock at porcelain filling is mixed, in 50 DEG C of mixing 1h, the group of being formed
The ceramic rubber of shape, natural cooling；
Step 4: the ceramic rubber of the bulk after cooling through open mill it is thin it is logical after, 5g bis 25 vulcanizing agent is added and is kneaded
0.75h obtains waterproof Ceramic silicon rubber material.
A kind of cable fixing head, outermost layer are the flame retardant coating of 0.1-1mm thickness, and the flame retardant coating is by above-mentioned waterproof ceramics SiClx
Rubber material is made, and has the following beneficial effects:
1, there is good mechanical property 250 DEG C or less, while there is very strong fire resistance, flame retardant coating can be sent out at high temperature
Green reacts to form one layer of hard protective layer, which stops burning away for flame, plays and completely cuts off extraneous flame
Effect, so that the object that protection is burnt is not damaged, the ablation time is longer, and temperature is higher, and shell is harder.
2, flame retardant coating still keeps preferable mechanical property at 300-400 DEG C, does not crack, it is ensured that cable fixing head sealing electricity
Cable outlet hole and water proof and dust proof, and then cause a machine to safely and reliably run.
3, there is good waterproof performance, the protective layer that flame retardant coating occurs to be formed after porcelainization reaction has densification under high temperature
Property, hydrone is difficult to infilter across flame retardant coating among cable outlet hole, it is ensured that machine is safely and reliably run.
Embodiment 7
It is basic experimental conditions (that is, if without specified otherwise, in addition to variable using the experiment condition of embodiment 6 using control variate method
Experiment condition with embodiment 6), silicon powder whether is added, silicon powder partial size, whether acicular wollastonite and manosil AS is added by changing
Salt fiber, the component of silicon rubber, mica partial size, whether be added aluminium dihydrogen phosphate, silicon powder with it is other mixed at porcelain filling before be
The conditions such as the temperature dried in no grinding, step 1, are prepared a variety of waterproof Ceramic silicon rubber materials as shown in Table 1,
Material described in table 1 is used for following comparative example experiments.
1 sample number into spectrum of table and corresponding variable
Comparative example 1
1#, 2#, 3#, 4# sample are tested for the property comparison, examine whether to be added silicon powder and silicon powder partial size to waterproof ceramic
The influence of silastic material performance, test result is as shown in table 2, and "/" indicates no valid data.
The comparison of 2 1#, 2#, 3#, 4# properties of sample of table
In table 2, pretreatment condition corresponding to the code name of pretreatment is as follows:
A0: without pretreatment；
A1:250 DEG C is heat-treated 7 days；
A2:250 DEG C is heat-treated 7 days, then at 350 DEG C of heat treatment 1h；
A3:250 DEG C is heat-treated 7 days, then at 350 DEG C of heat treatment 1h, then at 450 DEG C of heat treatment 1h；
A4:250 DEG C is heat-treated 7 days, then at 350 DEG C of heat treatment 1h, then at 450 DEG C of heat treatment 1h, then at 700 DEG C of heat treatment 1h.
In table 2, the test condition of material properties is as follows:
Hardness: Shao A, examination criteria ASTM D2240；
Tensile strength: MPa, examination criteria GB/T528-2009；
Elongation at break: %, examination criteria GB/T528-2009；
Tearing strength: kN/m, examination criteria GB/T529-2008；
Impermeability: the material of 1mm thickness tests water from the side of material and penetrates into other side institute under the hydraulic pressure of 0.2MPa
Need time (min).
It can be seen that from table 2
(1) 1#, 2# sample are still able to maintain certain impermeability after 250 DEG C, 350 DEG C, 450 DEG C, 700 DEG C of processing, moreover,
1# sample is compared compared with 2# sample, and impermeability is more preferable.This result shows that, the silicon powder that micro-nano-scale is added can effectively improve
The silicon powder that the impermeability of waterproof Ceramic silicon rubber, especially addition average grain diameter are 25nm or so, to waterproof ceramics SiClx
The performance of watertightness of rubber is promoted obvious.This is attributed to, and when the partial size of silicon powder is in micro/nano-scale, silicon powder can be used as spackling
The hole that ceramic reaction generates is filled up, makes Ceramic silicon rubber that there is certain compactness, water can be prevented to a certain extent
The infiltration of molecule, oxygen molecule promotes the waterproof performance of material after ceramic.
(2) 1#, 2# sample are able to maintain certain mechanical property after four kinds of different heat treatment, moreover, 1# sample compared with
2# sample is compared, and mechanical property is more preferable.This result shows that, anti-ceramic water can be effectively relieved in the silicon powder that micro-nano-scale is added
The problem of SiClx rubber softens at 300 DEG C or so, falls off, mechanical property declines to a great extent, especially addition average grain diameter are 25nm
The silicon powder of left and right, more preferable to the remission effect of this problem, mechanical property is more preferably also more stable.This is attributed to, micro/nano-scale
Silicon powder large specific surface area, reactivity is very high, and when temperature rises to 300 DEG C, the edge of silicon powder particle begins to melt, infiltration
To surrounding mica particles, silica dioxide granule, silicone rubber matrix decompose generate silica dioxide granule in, it is adhered to one another at
Porcelain, it is very low at porcelain temperature, efficiently solve 300 DEG C or so silicone rubber matrix start degradation and at this time ceramic reaction not yet send out
It is raw and cause Ceramic silicon rubber material cracks to fall off, mechanical properties decrease the problem of.
Comparative example 2
1#, 5# sample are tested for the property comparison, examine whether to be added acicular wollastonite and aluminosilicate fibre to waterproof pottery
The influence of porcelain SiClx rubber material performance, test result is as shown in table 3, pretreatment item corresponding to pretreated code name in table 3
For the test condition of part and material properties with comparative example 1, "/" indicates no valid data.
The comparison of 3 1#, 5# properties of sample of table
From can be seen that in table 3 1#, 5# sample through 250 DEG C, 350 DEG C, 450 DEG C, 700 DEG C processing after, be still able to maintain it is certain not
Water penetration；But after 350 DEG C, 450 DEG C, 700 DEG C of processing, the impermeability of 1# sample is obviously improved compared with 5# sample.
This is attributed to, after acicular wollastonite and aluminosilicate fibre is added in porcelain filling, due to the special pattern of the two, can with it is micro-
It receives the mutual filling pore of silicon powder of scale, generates synergistic effect, keep the compactness of material after ceramic more preferable, improve waterproof pottery
The waterproof performance of porcelain SiClx rubber, the waterproof performance of material especially after ceramic.
Comparative example 3
1#, 6#, 7#, 8#, 9#, 10#, 11# sample are tested for the property comparison, study the component of silicon rubber to waterproof ceramic
The influence of silastic material performance, test result is as shown in table 4, in table 4 test condition of material properties with comparative example 1,
"/" indicates no valid data.
The comparison of 4 1#, 6#, 7#, 8#, 9#, 10#, 11# properties of sample of table
In table 4, pretreatment condition corresponding to the code name of pretreatment is as follows:
A1:250 DEG C is heat-treated 7 days；
B1:250 DEG C is heat-treated 7 days, then at 300 DEG C of heat treatment 1h；
A2:250 DEG C is heat-treated 7 days, then at 350 DEG C of heat treatment 1h；
B2:250 DEG C is heat-treated 7 days, then at 400 DEG C of heat treatment 1h.
It can be seen that from table 4
Without valid data, this is attributed to 6# sample, and when all methyl silicone rubber of silicon rubber, silicone rubber matrix is just opened at 250 DEG C
Begin degradation, 250 DEG C heat treatment 7 days during silicone rubber matrix disintegrate, and at this time porcelainization reaction it is also weaker, it is difficult to formed from
Supporter causes 6# material to disintegrate in 250 DEG C of heat treatment processes.
Hardness and tensile strength of the 7# sample under the conditions of B1 are all obviously poorer than 1#, this is attributed to, all second of silicon rubber
When alkenyl mass content is the methyl vinyl silicone rubber of the ethenyl blocking of 0.15-0.25%, silicone rubber matrix is at 300 DEG C
Start to degrade, and porcelain reaction response rate is slower at this time, the self-supporter of formation is built on the sand；Under the conditions of A2, B2,7# sample
Hardness and tensile strength have promotion, this is attributed to the promotion of porcelain reaction response rate, and the self-supporter of formation is more and more steady
Gu.
Hardness and tensile strength of the 8# sample under the conditions of B1 are all obviously poorer than 1#, this is attributed to, all first of silicon rubber
When the methyl vinyl phenyl silicon rubber of base sealing end, silicone rubber matrix starts to degrade at 300 DEG C, and porcelain reaction response at this time
Rate is slower, and the self-supporter of formation is built on the sand；Under the conditions of B1, A2, B2, the hardness and tensile strength of 8# sample are all slightly above
7# sample, this degradation temperature for being attributed to methyl vinyl phenyl silicon rubber of methyl blocking itself are higher than vinyl mass content
For the methyl vinyl silicone rubber of the ethenyl blocking of 0.15-0.25%.
Hardness and tensile strength of 9#, 10#, 11# sample under the conditions of B1, A2, B2 all relatively, but all obviously compare 1#
Difference, this is attributed to, the vinyl mass content that the methyl vinyl silicone rubber of ethenyl blocking is 12.5: 28: 13 by mass ratio
When respectively the methyl vinyl silicone rubber of the ethenyl blocking of 0.26-0.28%, 0.21-0.23%, 0.12-0.15% forms, three
The methyl vinyl silicone rubber of the ethenyl blocking of kind differing ethylene base mass content generates synergistic effect, and silicone rubber matrix is being opened
The temperature for beginning to degrade is promoted to 350 DEG C or so；Hardness and stretching of 9#, 10#, 11# sample under the conditions of B1, A2, B2 are strong simultaneously
Degree all be higher than 6#, 7#, 8# sample, this is attributed to, silicon rubber by mass ratio be 22.5: 60: 35 methyl silicone rubber, vinyl seal
When the methyl vinyl silicone rubber at end, the methyl vinyl phenyl silicon rubber of methyl blocking form, synergistic effect is generated, ceramics are made
The degradation temperature of SiClx rubber matrix is promoted to 300 DEG C or so.
Comparative example 4
1#, 12#, 13#, 14# sample are tested for the property comparison, study the partial size of mica to waterproof Ceramic silicon rubber material
The influence of performance, test result is as shown in table 5, pretreatment condition corresponding to pretreated code name and material items in table 5
For the test condition of energy with comparative example 1, "/" indicates no valid data.
The comparison of 5 1#, 12#, 13#, 14# properties of sample of table
It can be seen that from table 5
Under the conditions of A2, the impermeability of 12#, 13#, 14# sample is successively promoted, this is attributed to, with the reduction of mica partial size, silicon
Powder can preferably play filling effect, and the compactness at material after porcelain is more preferable；1# and 14# sample impermeability are close, show
When mica partial size be reduced to differ less than three orders of magnitude with silicon powder partial size when, continue reduce mica partial size at material after porcelain
Compactness (impermeability) influence it is little；
Under the conditions of A2, the hardness and tensile strength of 12#, 13#, 14# sample are successively promoted, this is attributed to, with mica partial size
It reduces, silicon powder and mica generate synergistic effect, are easier to combine between the two, propose the mechanical property of waterproof Ceramic silicon rubber
It rises；The hardness and tensile strength of 1# and 14# sample are close, show to differ less than when being reduced to for mica partial size with silicon powder partial size
When three orders of magnitude, continuing, which reduces mica partial size, influences less the hardness of sample and tensile strength.
Comparative example 5
1#, 15# sample are tested for the property comparison, examine whether to be added aluminium dihydrogen phosphate to waterproof Ceramic silicon rubber material
The influence of performance, test result is as shown in table 6, pretreatment condition corresponding to pretreated code name and material items in table 6
For the test condition of energy with comparative example 1, "/" indicates no valid data.
The comparison of 6 1#, 15# properties of sample of table
It can be seen that from table 6
Mechanics and impermeability of the 1# sample under the conditions of A0, A1, A2, A3, A4 are each are all higher than or close to 15# sample, this returns
Because in, aluminium dihydrogen phosphate itself is a kind of adhesive, be introduced into aluminium dihydrogen phosphate can be promoted it is various in waterproof Ceramic silicon rubber
The binding force of component, to promote the mechanics and performance of watertightness of material.
Comparative example 6
1#, 16# sample are tested for the property comparison, research silicon powder mixes that preceding whether grind makes pottery to waterproof at porcelain filling with other
The influence of porcelain SiClx rubber material performance, test result is as shown in table 7, pretreatment item corresponding to pretreated code name in table 7
For the test condition of part and material properties with comparative example 1, "/" indicates no valid data.
The comparison of 7 1#, 16# properties of sample of table
It can be seen that from table 7
Mechanics and impermeability of the 1# sample under the conditions of A0, A1, A2, A3, A4 are each are all close to or higher than 16# sample, this returns
Because in silicon powder of micro/nano-scale itself can reunite, and the partial size for being equivalent to silicon powder itself is bigger, directly fill out with other at porcelain
Expect component mixing, it is difficult to give full play to the small advantage of silicon powder partial size (filling effect)；First silicon powder is individually ground, it is ensured that itself foot
Enough dispersibilities, then with it is other mixed at porcelain filling, can to avoid micro/nano-scale silicon powder due to itself reunite and be difficult to sufficiently
It is mixed among the gap of other component particles, the silicon powder filling effect of micro/nano-scale is given full play to, so that being finally prepared into
The waterproof Ceramic silicon rubber material arrived is more preferable at porcelain effect.
Comparative example 7
1#, 17# sample are tested for the property comparison, the temperature dried in research step one is to waterproof Ceramic silicon rubber material
The influence of performance, test result is as shown in table 8, pretreatment condition corresponding to pretreated code name and material items in table 8
For the test condition of energy with comparative example 1, "/" indicates no valid data.
The comparison of 8 1#, 17# properties of sample of table
It can be seen that from table 8
Mechanics and impermeability of the 1# sample under the conditions of A0, A1, A2, A3, A4 are each are all close to or higher than 17# sample, this returns
Because in drying temperature is excessively high, will lead to silicon powder itself and aoxidizes, and between silicon powder, silicon powder and other can send out between porcelain filling component
First portion adhesion, and the partial size for being equivalent to silicon powder itself are bigger, it is difficult to which giving full play to the small advantage of silicon powder partial size, (filling is made
With).
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (10)
1. a kind of waterproof Ceramic silicon rubber material, which is characterized in that in parts by mass, comprising:
At 30-100 parts of porcelain filling, described include mass ratio at porcelain filling is (40-100): (20-100): the silicon powder of (20-80),
Mica and silica；The partial size of the silicon powder is less than 3 μm；
60-100 parts of silicon rubber, the silicon rubber general formula is (RnSiO(4-n)/2)m, R is carbon containing organic group, and n is to connect on silicon atom
Carbon containing organic radix, and n be 1,2 or 3, m is the degree of polymerization, m >=2；
2-30 parts of silicone oil；
15-80 parts of boron oxide；
0.1-15 parts of coupling agent；
0.1-10 parts of vulcanizing agent.
2. a kind of waterproof Ceramic silicon rubber material according to claim 1, which is characterized in that described also to be wrapped at porcelain filling
It includes:
The mass ratio of acicular wollastonite, the acicular wollastonite and the silicon powder is 0.2-0.35；
The mass ratio of aluminosilicate fibre, the aluminosilicate fibre and the acicular wollastonite is 0.4-0.6.
3. a kind of waterproof Ceramic silicon rubber material according to claim 2, it is characterised in that:
The partial size at silicon powder in porcelain filling is 20-30nm.
4. a kind of waterproof Ceramic silicon rubber material according to claim 3, which is characterized in that the silicon rubber includes:
Mass ratio is (15-30): (40-75): the methyl silicone rubber of (15-50), ethenyl blocking methyl vinyl silicone rubber,
The methyl vinyl phenyl silicon rubber of methyl blocking；In the methyl vinyl phenyl silicon rubber of the methyl blocking, phenyl and silicon
The molar ratio of atom is 0.25-0.35.
5. a kind of waterproof Ceramic silicon rubber material according to claim 4, which is characterized in that the ethenyl blocking
Methyl vinyl silicone rubber includes:
Mass ratio is (10-15): (20-35): the vinyl mass content of (10-15) is respectively 0.26-0.28%, 0.21-
0.23%, the methyl vinyl silicone rubber of the ethenyl blocking of 0.12-0.15%.
6. a kind of waterproof Ceramic silicon rubber material according to claim 5, it is characterised in that:
The partial size at mica in porcelain filling is 3-30 μm.
7. a kind of waterproof Ceramic silicon rubber material according to claim 6, it is characterised in that further include:
The mass ratio of aluminium dihydrogen phosphate, the aluminium dihydrogen phosphate and the silicon rubber is 0.1-0.15.
8. a kind of preparation method of waterproof Ceramic silicon rubber material, feature described in any one of -7 according to claim 1
It is to include the following steps:
Step 1: grinding 0.5-1h for silicon powder, then mix with all other at porcelain filling component, continues to grind 1.5-2.5h, so
2-6h is dried at 100-160 DEG C afterwards, is obtained pretreated at porcelain filling；
Step 2: it will be mixed in addition at whole components other than porcelain filling, vulcanizing agent, be warming up to 70-100 DEG C of mixing 1-1.5h；
It is warming up to 155-170 DEG C again, pumping vacuum and mixing 1.5-2.5 hours, obtains organic silicon compounded rubber stock；During the pumping vacuum and mixing
Holding vacuum degree is (- 0.1)-(- 0.05) MPa；
Step 3: pretreated be added in organic silicon compounded rubber stock at porcelain filling is mixed, in 25-90 DEG C of mixing 0.5-1.5h,
Form the ceramic rubber of bulk, natural cooling；
Step 4: the ceramic rubber of the bulk after cooling through open mill it is thin it is logical after, vulcanizing agent is added and is kneaded 0.5-1h, obtains
To waterproof Ceramic silicon rubber material.
9. a kind of preparation method of waterproof Ceramic silicon rubber material according to claim 8, it is characterised in that:
In the step 1, drying temperature is 125-135 DEG C.
10. a kind of cable fixing head has flame retardant coating, it is characterised in that:
The flame retardant coating is made of the waterproof Ceramic silicon rubber material of any of claims 1-7.
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