CN106398231A - Ceramic fire-resistant and flame-retardant silicone rubber and preparation method thereof - Google Patents
Ceramic fire-resistant and flame-retardant silicone rubber and preparation method thereof Download PDFInfo
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- CN106398231A CN106398231A CN201610827211.1A CN201610827211A CN106398231A CN 106398231 A CN106398231 A CN 106398231A CN 201610827211 A CN201610827211 A CN 201610827211A CN 106398231 A CN106398231 A CN 106398231A
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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
- C08K2201/011—Nanostructured additives
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—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
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention relates to the technical field of silicone rubber, and particularly relates to a ceramic fire-resistant and flame-retardant silicone rubber and a preparation method thereof. The ceramic fire-resistant and flame-retardant silicone rubber is composed of a component A and a component B in a weight ratio of 0.8-1.2: 1. The component A comprises the following raw materials in weight part: 60-140 parts of silicone rubber A, 35-45 parts of reinforcing agent, 60-100 parts of filler A, 11.4-17.2 parts of silane auxiliary agent A, 0.15-0.25 part of lubricant A, 0.1-0.3 part of flame retardant, and 0.5-1.5 parts of vulcanizing agent. The component B comprises the following raw materials in weight part: 60-140 parts of silicone rubber B, 230-290 parts of filler B, 3-6 parts of silane auxiliary agent B, and 0.2-0.4 part of lubricant B. According to the technical scheme of the invention, the ceramic fire-resistant and flame-retardant silicone rubber is good in fire-resistant and flame-retardant property, and excellent in comprehensive performance.
Description
Technical field
The present invention relates to silicon rubber technical field is and in particular to a kind of ceramic fire resistant flame retardant silicone rubber and its preparation side
Method.
Background technology
, in fire incident, there is electric wire not fire resisting in the generally not fire-retardant not fire resisting of silicone rubber itself, meet fiery easy firing and ask
Topic, this area lacks a kind of silicone rubber of fire resisting it is desirable to not only can possess the excellent specific property of rubber during normal use, and
There are preferable fire resistance and fire resistance, the product made using it can play certain protective effect in big fire, can
Reduce the loss bringing in fire, reduce harm.
Content of the invention
In order to overcome shortcoming and defect present in prior art, it is an object of the invention to provide a kind of ceramic fire resisting
Flame-proof silicon rubber, this ceramic fire resistant flame retardant silicone rubber has preferable fire resistant flame retardant performance, excellent combination property.
Another object of the present invention is to providing a kind of preparation method of ceramic fire resistant flame retardant silicone rubber, this preparation method
Process is simple, convenient operation and control, steady quality, production efficiency is high, and low production cost can large-scale industrial production.
The purpose of the present invention is achieved through the following technical solutions：A kind of ceramic fire resistant flame retardant silicone rubber, it by component A and
Component B compares 0.8-1.2 with weight:1 composition, wherein, component A includes the raw material of following weight portion：
Silicone rubber A 60-140 part
Reinforcing agent 35-45 part
Filler A 60-100 part
Silane adjuvant A 11.4-17.2 part
Lubricant A 0.15-0.25 part
Fire retardant 0.1-0.3 part
Vulcanizing agent 0.5-1.5 part；
Component B includes the raw material of following weight portion：
Silicone rubber B 60-140 part
Filler B 230-290 part
Silane adjuvant B 3-6 part
Lubricant B 0.2-0.4 part.
The present invention is by adopting above-mentioned raw materials, and strictly controls the weight proportion of each raw material, prepared ceramic fire resisting resistance
Combustion silicone rubber has preferable fire resistant flame retardant performance, excellent combination property.
Preferably, described silicone rubber A is to compare 30- by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B with weight
70：The mixture of 30-70 composition；Wherein, the contents of ethylene of methyl vinyl silicone rubber A is 0.02-0.06%, and molecular weight is
64-66 ten thousand；The contents of ethylene of methyl vinyl silicone rubber B is 0.21-0.25%, and molecular weight is 64-66 ten thousand.
It is 0.02-0.06% that the present invention passes through using contents of ethylene, and molecular weight is the methyl ethylene silicon rubber of 64-66 ten thousand
Glue A, it has high molecular, and main chain is longer, and intermolecular force is big, can effectively improve the mechanical strength of silicone rubber；The present invention
By being 0.21-0.25% using contents of ethylene, molecular weight is the methyl vinyl silicone rubber B of 64-66 ten thousand, and it has high score
Son amount, main chain is longer, and intermolecular force is big, can effectively improve the mechanical strength of silicone rubber.
The present invention is by being used as silicone rubber using the methyl vinyl silicone rubber of two kinds of differing ethylenes and content and molecular weight
A, and control its weight than for 30-70：30-70, prepared ceramic fire resistant flame retardant silicone rubber has higher intensity and hardness.
Preferably, described reinforcing agent be particle diameter in 10-50nm, specific surface area in 200-300m2The gas-phase silica of/g.
The present invention passes through using particle diameter in 10-50nm, specific surface area in 200-300m2The gas-phase silica of/g is as reinforcement
Agent, its particle diameter is little, is dispersed in the mechanical strength that can improve silicone rubber in silicone rubber.
Preferably, described filler A is to compare 15-25 by mica powder, glass dust, montmorillonite and wollastonite with weight：15-
25：15-25：The mixture of 15-25 composition.
The present invention, by adopting mica powder, forms hard and continuous ceramic layer on burning polymer surface, plays resistance
Every effect, reduce HRR；The present invention, by adopting glass dust, reaches more preferable porcelain effect with Muscovitum cooperation, can
To reduce porcelain temperature；The present invention, by adopting montmorillonite, reaches more preferable porcelain effect with Muscovitum cooperation；The present invention passes through to adopt
With wollastonite, reach more preferable porcelain effect with Muscovitum cooperation.
The present invention is by being used as filler A compounding use using mica powder, glass dust, montmorillonite and wollastonite, and controls
Its weight is than for 15-25：15-25：15-25：15-25, prepared ceramic fire resistant flame retardant silicone rubber has preferable fire resisting resistance
Combustion performance, excellent combination property.
Preferably, described silane adjuvant A be by hydroxyl-terminated injecting two methyl siloxane, tetramethyl divinyl disilazane,
Vinyltrimethoxy silane and VTES compare 10-14 with weight：1-2：0.2-0.6：0.2-0.6 composition
Mixture.
The present invention is by adopting hydroxyl-terminated injecting two methyl siloxane, it can be avoided that knot in storage placement process for the silicone rubber
The generation of structure phenomenon；The present invention, by adopting tetramethyl divinyl disilazane, energy effective process gas-phase silica, increases
Organic silicon rubber and the compatibility of gas-phase silica, so that gas-phase silica is uniformly dispersed, are conducive to improving intensity；This
Bright by silane coupler is used as using vinyltrimethoxy silane, can increase substantially enhancing compound physical mechanical property,
And improve wettability in sizing material for the filler and dispersibility；The present invention is even by being used as silane using vinyltrimethoxy silane
Connection agent, can increase substantially enhancing compound physical mechanical property, and improve wettability in sizing material for the filler and dispersibility.
The present invention passes through using hydroxyl-terminated injecting two methyl siloxane, tetramethyl divinyl disilazane, vinyl front three
TMOS and VTES are as silane adjuvant compounding use, and control its weight than for 10-14：1-2：
0.2-0.6：0.2-0.6, prepared ceramic fire resistant flame retardant silicone rubber has higher intensity and processing characteristics.
Preferably, described lubricant A is to compare 0.05-0.15 by zinc stearate and stearic acid with weight:0.05-0.15 group
The mixture becoming.
The present invention is by being used as lubricant A compounding use using zinc stearate and stearic acid, and controls its weight ratio to be
0.05-0.15:0.05-0.15, can effectively improve the demolding performace of silicone rubber.
Described fire retardant is the platinum fire retardant of 1000-3000ppm for platinum mass content.
It is the platinum fire retardant of 1000-3000ppm that the present invention passes through using platinum mass content, can play ceramic effect, its
Oxidation, degraded are promoted on the silastic surface with air contact, forms high cross-linked structure, form the siloxanes being similar to not fire
Film shields air, and therefore flame no longer spreads and self-extinguishment to the inside of silicone rubber.
Described vulcanizing agent is 2,5- dimethyl -2,5- two（Tert-butyl hydroperoxide）Hexane.
The present invention passes through using 2,5- dimethyl -2,5- two（Tert-butyl hydroperoxide）Hexane as vulcanizing agent, imitate by its sulfuration
Really good, prepared ceramic fire resistant flame retardant silicone rubber has preferable fire resistant flame retardant performance, excellent combination property.
Preferably, described silicone rubber B is to compare 30- by methyl vinyl silicone rubber a and methyl vinyl silicone rubber b with weight
70：The mixture of 30-70 composition；Wherein, the contents of ethylene of methyl vinyl silicone rubber a is 0.02-0.06%, and molecular weight is
64-66 ten thousand；The contents of ethylene of methyl vinyl silicone rubber b is 0.12-0.20%, and molecular weight is 64-66 ten thousand.
It is 0.02-0.06% that the present invention passes through using contents of ethylene, and molecular weight is the methyl ethylene silicon rubber of 64-66 ten thousand
Glue a, it has high molecular, and main chain is longer, and intermolecular force is big, can effectively improve the mechanical strength of silicone rubber；The present invention
By using contents of ethylene for contents of ethylene be 0.12-0.20%, molecular weight be 64-66 ten thousand methyl vinyl silicone rubber
B, it has high molecular, and main chain is longer, and intermolecular force is big, can effectively improve the mechanical strength of silicone rubber.
The present invention is by being used as silicone rubber using the methyl vinyl silicone rubber of two kinds of differing ethylenes and content and molecular weight
B, and control its weight than for 30-70：30-70, prepared ceramic fire resistant flame retardant silicone rubber has higher intensity and hardness.
Preferably, described filler B is by ultrafine aluminium hydroxide micropowder, super fine magnesium hydroxide micropowder, Calcium Carbonate and oxidation
Zinc compares 200-220 with weight：20-30：5-20：The mixture of 5-20 composition.
The present invention passes through using ultrafine aluminium hydroxide micropowder, its as environment friendly flame retardant, stable performance, non-volatile；This
Invention is by using super fine magnesium hydroxide micropowder, its thermal decomposition dehydration temperaturre is 300 degree, and heat stability is good；The present invention passes through to adopt
With Calcium Carbonate, its residue is hard and densification, plays ceramic effect；The present invention by adopting zinc oxide, energy during burning
Absorb free radical, block burning, play fire-retardant synergism.
The present invention is filled out by being used as using ultrafine aluminium hydroxide micropowder, super fine magnesium hydroxide micropowder, Calcium Carbonate and zinc oxide
Fill agent B compounding use, and control its weight than for 200-220：20-30：5-20：5-20, prepared ceramic fire resistant flame retardant silicon
Rubber has preferable fire resistant flame retardant performance, excellent combination property.
Described silane adjuvant B is to compare 2-4 by vinyltrimethoxy silane and hexamethyldisiloxane with weight：1-2 group
The mixture becoming.
The present invention, by adopting vinyltrimethoxy silane, can improve the intensity of ceramic fire resistant flame retardant silicone rubber；
The present invention, by adopting hexamethyldisiloxane, can improve hydrophobicity.
The present invention by silane adjuvant compounding use is used as using vinyltrimethoxy silane and hexamethyldisiloxane,
And control its weight than for 2-4：1-2, prepared fluorinated silicone rubber gross rubber has higher intensity and processing characteristics.
Described lubricant B is zinc stearate.
The present invention, by being used as lubricant B using zinc stearate, can effectively improve the demolding performace of silicone rubber.
A kind of preparation method of ceramic fire resistant flame retardant silicone rubber, comprises the steps：
（One）The preparation of component A：
1st, first in banbury, put into raw material silicone rubber A, stir 4-6min；
2nd, put into lubricant A and part reinforcing agent, filler A, then put into silane adjuvant A；
3rd, after the part reinforcing agent putting into, filler A mix, more remaining reinforcing agent, filler A are put in five times；
4th, after will be agglomerating for above mixing raw materials, intensification refining glue, obtain banburying glue；
5th, banburying glue is carried out discharging, in input mill, mill is uniform, lower roll, set aside for use；
（Two）The preparation of component B：
1）, first in banbury, put into raw material silicone rubber B, stir 4-6min；
2）, put into lubricant B and partially filled agent B, then put into silane adjuvant B；
3）, after partially filled agent B that puts into mixes, then put into remaining filler B in five times；
4）, will be agglomerating for above mixing raw materials after, intensification refining glue, obtain banburying glue；
5）, banburying glue carried out discharging, put in mill mill uniformly, lower roll, set aside for use；
（Three）The preparation of ceramic fire resistant flame retardant silicone rubber：
（1）, component A and component B are put in mill mill uniformly in proportion, add fire retardant, lower roll after thin logical five times, put
Enter filter, filtered with 150 mesh filter screens, obtain glue of beginning to pratise；
（2）, vulcanizing agent added to begin to pratise mix in glue, put into mould and carry out sulfidization molding, prepared ceramic fire resistant flame retardant silicon rubber
Glue.
Preferably, in described step 4, the technological parameter of intensification refining glue is：After temperature rises to 90-110 DEG C, mediate 100-
140min, then evacuation 40-80min, vacuum is in -0.06～-0.10Mpa；Described step 4）In, the technique ginseng of intensification refining glue
Number is：After temperature rises to 90-110 DEG C, mediate 40-80min, then evacuation 40-80min, vacuum -0.06～-
0.10Mpa；Described step（2）In, curing temperature is 160-180 DEG C, and cure time is 8-12min.
The beneficial effects of the present invention is：The ceramic fire resistant flame retardant silicone rubber of the present invention has preferable fire resistant flame retardant
Can, excellent combination property.
The preparation method process is simple of the present invention, convenient operation and control, steady quality, production efficiency is high, low production cost,
Can large-scale industrial production.
Specific embodiment
For the ease of the understanding of those skilled in the art, with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying refers to not limitation of the invention.
Embodiment 1
A kind of ceramic fire resistant flame retardant silicone rubber, it compares 0.8 by component A and component B with weight:1 composition, wherein, component A includes
The raw material of following weight portion：
60 parts of silicone rubber A
35 parts of reinforcing agent
60 parts of filler A
11.4 parts of silane adjuvant A
0.15 part of lubricant A
0.1 part of fire retardant
0.5 part of vulcanizing agent；
Component B includes the raw material of following weight portion
60 parts of silicone rubber B
230 parts of filler B
3 parts of silane adjuvant B
0.2 part of lubricant B.
Described silicone rubber A is to compare 30 by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B with weight：30 compositions
Mixture；Wherein, the contents of ethylene of methyl vinyl silicone rubber A is 0.02%, and molecular weight is 640,000；Methyl ethylene silicon
The contents of ethylene of rubber B is 0.21%, and molecular weight is 640,000.
Described reinforcing agent be particle diameter in 10nm, specific surface area in 200m2The gas-phase silica of/g.
Described filler A is to compare 15 by mica powder, glass dust, montmorillonite and wollastonite with weight：15：15：15 compositions
Mixture.
Described silane adjuvant A is by hydroxyl-terminated injecting two methyl siloxane, tetramethyl divinyl disilazane, vinyl three
Methoxy silane and VTES compare 10 with weight：1：0.2：The mixture of 0.2 composition.
Described lubricant A is to compare 0.05 by zinc stearate and stearic acid with weight:The mixture of 0.05 composition；Described resistance
Combustion agent is the platinum fire retardant of 1000ppm for platinum mass content；Described vulcanizing agent is 2,5- dimethyl -2,5- two（Tert-butyl group mistake
Oxidation）Hexane.
Described silicone rubber B is to compare 30 by methyl vinyl silicone rubber a and methyl vinyl silicone rubber b with weight：30 compositions
Mixture；Wherein, the contents of ethylene of methyl vinyl silicone rubber a is 0.02%, and molecular weight is 640,000；Methyl ethylene silicon
The contents of ethylene of rubber b is 0.12%, and molecular weight is 640,000.
Described filler B is with weight by ultrafine aluminium hydroxide micropowder, super fine magnesium hydroxide micropowder, Calcium Carbonate and zinc oxide
Ratio 200：20：5：The mixture of 5 compositions；Described silane adjuvant B is by vinyltrimethoxy silane and hexamethyldisiloxane
Compare 2 with weight：The mixture of 1 composition；Described lubricant B is zinc stearate.
A kind of preparation method of ceramic fire resistant flame retardant silicone rubber, comprises the steps：
（One）The preparation of component A：
1st, first in banbury, put into raw material silicone rubber A, stir 4min；
2nd, put into lubricant A and part reinforcing agent, filler A, then put into silane adjuvant A；
3rd, after the part reinforcing agent putting into, filler A mix, more remaining reinforcing agent, filler A are put in five times；
4th, after will be agglomerating for above mixing raw materials, intensification refining glue, obtain banburying glue；
5th, banburying glue is carried out discharging, in input mill, mill is uniform, lower roll, set aside for use；
（Two）The preparation of component B：
1）, first in banbury, put into raw material silicone rubber B, stir 4min；
2）, put into lubricant B and partially filled agent B, then put into silane adjuvant B；
3）, after partially filled agent B that puts into mixes, then put into remaining filler B in five times；
4）, will be agglomerating for above mixing raw materials after, intensification refining glue, obtain banburying glue；
5）, banburying glue carried out discharging, put in mill mill uniformly, lower roll, set aside for use；
（Three）The preparation of ceramic fire resistant flame retardant silicone rubber：
（1）, component A and component B are put in mill mill uniformly in proportion, add fire retardant, lower roll after thin logical five times, put
Enter filter, filtered with 150 mesh filter screens, obtain glue of beginning to pratise；
（2）, vulcanizing agent added to begin to pratise mix in glue, put into mould and carry out sulfidization molding, prepared ceramic fire resistant flame retardant silicon rubber
Glue.
In described step 4, the technological parameter of intensification refining glue is：After temperature rises to 90 DEG C, mediate 140min, then evacuation
40min, vacuum is in -0.06Mpa；Described step 4）In, the technological parameter of intensification refining glue is：After temperature rises to 90 DEG C, mediate
80min, then evacuation 40min, vacuum is in -0.06Mpa；Described step（2）In, curing temperature is 160 DEG C, and cure time is
12min.
Embodiment 2
A kind of ceramic fire resistant flame retardant silicone rubber, it compares 1 by component A and component B with weight:1 composition, wherein, component A include as
The raw material of lower weight portion：
100 parts of silicone rubber A
35 parts of reinforcing agent
80 parts of filler A
14.8 parts of silane adjuvant A
0.2 part of lubricant A
0.2 part of fire retardant
1.2 parts of vulcanizing agent；
Component B includes the raw material of following weight portion
100 parts of silicone rubber B
250 parts of filler B
4.5 parts of silane adjuvant B
0.3 part of lubricant B.
Described silicone rubber A is to compare 70 by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B with weight：30 compositions
Mixture；Wherein, the contents of ethylene of methyl vinyl silicone rubber A is 0.04%, and molecular weight is 650,000；Methyl ethylene silicon
The contents of ethylene of rubber B is 0.23%, and molecular weight is 650,000.
Described reinforcing agent be particle diameter in 20nm, specific surface area in 220m2The gas-phase silica of/g.
Described filler A is to compare 20 by mica powder, glass dust, montmorillonite and wollastonite with weight：20：20：20 compositions
Mixture.
Described silane adjuvant A is by hydroxyl-terminated injecting two methyl siloxane, tetramethyl divinyl disilazane, vinyl three
Methoxy silane and VTES compare 12 with weight：2：0.4：The mixture of 0.4 composition.
Described lubricant A is to compare 0.1 by zinc stearate and stearic acid with weight:The mixture of 0.1 composition；Described fire-retardant
Agent is the platinum fire retardant of 1500ppm for platinum mass content；Described vulcanizing agent is 2,5- dimethyl -2,5- two（T-butyl peroxy
Change）Hexane.
Described silicone rubber B is to compare 50 by methyl vinyl silicone rubber a and methyl vinyl silicone rubber b with weight：50 compositions
Mixture；Wherein, the contents of ethylene of methyl vinyl silicone rubber a is 0.04%, and molecular weight is 650,000；Methyl ethylene silicon
The contents of ethylene of rubber b is 0.14%, and molecular weight is 650,000.
Described filler B is with weight by ultrafine aluminium hydroxide micropowder, super fine magnesium hydroxide micropowder, Calcium Carbonate and zinc oxide
Ratio 200：30：10：The mixture of 10 compositions；Described silane adjuvant B is by vinyltrimethoxy silane and hexamethyl two silicon nitrogen
Alkane compares 3 with weight：The mixture of 1.5 compositions；Described lubricant B is zinc stearate.
A kind of preparation method of ceramic fire resistant flame retardant silicone rubber, comprises the steps：
（One）The preparation of component A：
1st, first in banbury, put into raw material silicone rubber A, stir 4.5min；
2nd, put into lubricant A and part reinforcing agent, filler A, then put into silane adjuvant A；
3rd, after the part reinforcing agent putting into, filler A mix, more remaining reinforcing agent, filler A are put in five times；
4th, after will be agglomerating for above mixing raw materials, intensification refining glue, obtain banburying glue；
5th, banburying glue is carried out discharging, in input mill, mill is uniform, lower roll, set aside for use；
（Two）The preparation of component B：
1）, first in banbury, put into raw material silicone rubber B, stir 4.5min；
2）, put into lubricant B and partially filled agent B, then put into silane adjuvant B；
3）, after partially filled agent B that puts into mixes, then put into remaining filler B in five times；
4）, will be agglomerating for above mixing raw materials after, intensification refining glue, obtain banburying glue；
5）, banburying glue carried out discharging, put in mill mill uniformly, lower roll, set aside for use；
（Three）The preparation of ceramic fire resistant flame retardant silicone rubber：
（1）, component A and component B are put in mill mill uniformly in proportion, add fire retardant, lower roll after thin logical five times, put
Enter filter, filtered with 150 mesh filter screens, obtain glue of beginning to pratise；
（2）, vulcanizing agent added to begin to pratise mix in glue, put into mould and carry out sulfidization molding, prepared ceramic fire resistant flame retardant silicon rubber
Glue.
In described step 4, the technological parameter of intensification refining glue is：After temperature rises to 95 DEG C, mediate 130min, then evacuation
50min, vacuum is in -0.07Mpa；Described step 4）In, the technological parameter of intensification refining glue is：After temperature rises to 95 DEG C, mediate
70min, then evacuation 50min, vacuum is in -0.07Mpa；Described step（2）In, curing temperature is 165 DEG C, and cure time is
11min.
Embodiment 3
A kind of ceramic fire resistant flame retardant silicone rubber, it compares 0.8-1.2 by component A and component B with weight:1 composition, wherein, component A
Raw material including following weight portion：
100 parts of silicone rubber A
42 parts of reinforcing agent
75 parts of filler A
14.8 parts of silane adjuvant A
0.2 part of lubricant A
0.2 part of fire retardant
1.2 parts of vulcanizing agent；
Component B includes the raw material of following weight portion
100 parts of silicone rubber B
260 parts of filler B
4.5 parts of silane adjuvant B
0.3 part of lubricant B.
Described silicone rubber A is to compare 50 by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B with weight：50 compositions
Mixture；Wherein, the contents of ethylene of methyl vinyl silicone rubber A is 0.04%, and molecular weight is 650,000；Methyl ethylene silicon
The contents of ethylene of rubber B is 0.23%, and molecular weight is 650,000.
Described reinforcing agent be particle diameter in 30nm, specific surface area in 250m2The gas-phase silica of/g.
Described filler A is to compare 20 by mica powder, glass dust, montmorillonite and wollastonite with weight：20：20：15 compositions
Mixture.
Described silane adjuvant A is by hydroxyl-terminated injecting two methyl siloxane, tetramethyl divinyl disilazane, vinyl three
Methoxy silane and VTES compare 12 with weight：2：0.4：The mixture of 0.4 composition.
Described lubricant A is to compare 0.1 by zinc stearate and stearic acid with weight:The mixture of 0.1 composition；Described fire-retardant
Agent is the platinum fire retardant of 2000ppm for platinum mass content；Described vulcanizing agent is 2,5- dimethyl -2,5- two（T-butyl peroxy
Change）Hexane.
Described silicone rubber B is to compare 70 by methyl vinyl silicone rubber a and methyl vinyl silicone rubber b with weight：30 compositions
Mixture；Wherein, the contents of ethylene of methyl vinyl silicone rubber a is 0.04%, and molecular weight is 650,000；Methyl ethylene silicon
The contents of ethylene of rubber b is 0.16%, and molecular weight is 650,000.
Described filler B is with weight by ultrafine aluminium hydroxide micropowder, super fine magnesium hydroxide micropowder, Calcium Carbonate and zinc oxide
Ratio 220：30：5：The mixture of 5 compositions；Described silane adjuvant B is by vinyltrimethoxy silane and hexamethyldisiloxane
Compare 3 with weight：The mixture of 1.5 compositions；Described lubricant B is zinc stearate.
A kind of preparation method of ceramic fire resistant flame retardant silicone rubber, comprises the steps：
（One）The preparation of component A：
1st, first in banbury, put into raw material silicone rubber A, stir 5min；
2nd, put into lubricant A and part reinforcing agent, filler A, then put into silane adjuvant A；
3rd, after the part reinforcing agent putting into, filler A mix, more remaining reinforcing agent, filler A are put in five times；
4th, after will be agglomerating for above mixing raw materials, intensification refining glue, obtain banburying glue；
5th, banburying glue is carried out discharging, in input mill, mill is uniform, lower roll, set aside for use；
（Two）The preparation of component B：
1）, first in banbury, put into raw material silicone rubber B, stir 5min；
2）, put into lubricant B and partially filled agent B, then put into silane adjuvant B；
3）, after partially filled agent B that puts into mixes, then put into remaining filler B in five times；
4）, will be agglomerating for above mixing raw materials after, intensification refining glue, obtain banburying glue；
5）, banburying glue carried out discharging, put in mill mill uniformly, lower roll, set aside for use；
（Three）The preparation of ceramic fire resistant flame retardant silicone rubber：
（1）, component A and component B are put in mill mill uniformly in proportion, add fire retardant, lower roll after thin logical five times, put
Enter filter, filtered with 150 mesh filter screens, obtain glue of beginning to pratise；
（2）, vulcanizing agent added to begin to pratise mix in glue, put into mould and carry out sulfidization molding, prepared ceramic fire resistant flame retardant silicon rubber
Glue.
In described step 4, the technological parameter of intensification refining glue is：After temperature rises to 100 DEG C, mediate 120min, then evacuation
60min, vacuum is in -0.08Mpa；Described step 4）In, the technological parameter of intensification refining glue is：After temperature rises to 100 DEG C, mediate
60min, then evacuation 60min, vacuum is in -0.08Mpa；Described step（2）In, curing temperature is 170 DEG C, and cure time is
10min.
Embodiment 4
A kind of ceramic fire resistant flame retardant silicone rubber, it compares 0.8-1.2 by component A and component B with weight:1 composition, wherein, component A
Raw material including following weight portion：
100 parts of silicone rubber A
45 parts of reinforcing agent
80 parts of filler A
14.8 parts of silane adjuvant A
0.2 part of lubricant A
0.2 part of fire retardant
1.2 parts of vulcanizing agent；
Component B includes the raw material of following weight portion
100 parts of silicone rubber B
260 parts of filler B
4.5 parts of silane adjuvant B
0.3 part of lubricant B.
Described silicone rubber A is to compare 30 by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B with weight：70 compositions
Mixture；Wherein, the contents of ethylene of methyl vinyl silicone rubber A is 0.04%, and molecular weight is 650,000；Methyl ethylene silicon
The contents of ethylene of rubber B is 0.23%, and molecular weight is 650,000.
Described reinforcing agent be particle diameter in 40nm, specific surface area in 280m2The gas-phase silica of/g.
Described filler A is to compare 20 by mica powder, glass dust, montmorillonite and wollastonite with weight：20：20：20 compositions
Mixture.
Described silane adjuvant A is by hydroxyl-terminated injecting two methyl siloxane, tetramethyl divinyl disilazane, vinyl three
Methoxy silane and VTES compare 12 with weight： 2：0.4：The mixture of 0.4 composition.
Described lubricant A is to compare 0.1 by zinc stearate and stearic acid with weight:The mixture of 0.1 composition；Described fire-retardant
Agent is the platinum fire retardant of 2500ppm for platinum mass content；Described vulcanizing agent is 2,5- dimethyl -2,5- two（T-butyl peroxy
Change）Hexane.
Described silicone rubber B is to compare 30 by methyl vinyl silicone rubber a and methyl vinyl silicone rubber b with weight：70 compositions
Mixture；Wherein, the contents of ethylene of methyl vinyl silicone rubber a is 0.04%, and molecular weight is 650,000；Methyl ethylene silicon
The contents of ethylene of rubber b is 0.16%, and molecular weight is 650,000.
Described filler B is with weight by ultrafine aluminium hydroxide micropowder, super fine magnesium hydroxide micropowder, Calcium Carbonate and zinc oxide
Ratio 200：20：20：The mixture of 20 compositions；Described silane adjuvant B is by vinyltrimethoxy silane and hexamethyl two silicon nitrogen
Alkane compares 3 with weight：The mixture of 1.5 compositions；Described lubricant B is zinc stearate.
A kind of preparation method of ceramic fire resistant flame retardant silicone rubber, comprises the steps：
（One）The preparation of component A：
1st, first in banbury, put into raw material silicone rubber A, stir 5.5min；
2nd, put into lubricant A and part reinforcing agent, filler A, then put into silane adjuvant A；
3rd, after the part reinforcing agent putting into, filler A mix, more remaining reinforcing agent, filler A are put in five times；
4th, after will be agglomerating for above mixing raw materials, intensification refining glue, obtain banburying glue；
5th, banburying glue is carried out discharging, in input mill, mill is uniform, lower roll, set aside for use；
（Two）The preparation of component B：
1）, first in banbury, put into raw material silicone rubber B, stir 5.5min；
2）, put into lubricant B and partially filled agent B, then put into silane adjuvant B；
3）, after partially filled agent B that puts into mixes, then put into remaining filler B in five times；
4）, will be agglomerating for above mixing raw materials after, intensification refining glue, obtain banburying glue；
5）, banburying glue carried out discharging, put in mill mill uniformly, lower roll, set aside for use；
（Three）The preparation of ceramic fire resistant flame retardant silicone rubber：
（1）, component A and component B are put in mill mill uniformly in proportion, add fire retardant, lower roll after thin logical five times, put
Enter filter, filtered with 150 mesh filter screens, obtain glue of beginning to pratise；
（2）, vulcanizing agent added to begin to pratise mix in glue, put into mould and carry out sulfidization molding, prepared ceramic fire resistant flame retardant silicon rubber
Glue.
In described step 4, the technological parameter of intensification refining glue is：After temperature rises to 105 DEG C, mediate 110min, then evacuation
70min, vacuum is in -0.09Mpa；Described step 4）In, the technological parameter of intensification refining glue is：After temperature rises to 105 DEG C, mediate
50min, then evacuation 70min, vacuum is in -0.09Mpa；Described step（2）In, curing temperature is 175 DEG C, and cure time is
9min.
Embodiment 5
A kind of ceramic fire resistant flame retardant silicone rubber, it compares 1.2 by component A and component B with weight:1 composition, wherein, component A includes
The raw material of following weight portion：
140 parts of silicone rubber A
45 parts of reinforcing agent
100 parts of filler A
17.2 parts of silane adjuvant A
0.25 part of lubricant A
0.3 part of fire retardant
1.5 parts of vulcanizing agent；
Component B includes the raw material of following weight portion
140 parts of silicone rubber B
290 parts of filler B
6 parts of silane adjuvant B
0.4 part of lubricant B.
Described silicone rubber A is to compare 70 by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B with weight：70 compositions
Mixture；Wherein, the contents of ethylene of methyl vinyl silicone rubber A is 0.06%, and molecular weight is 660,000；Methyl ethylene silicon
The contents of ethylene of rubber B is 0.25%, and molecular weight is 660,000.
Described reinforcing agent be particle diameter in 50nm, specific surface area in 300m2The gas-phase silica of/g.
Described filler A is to compare 25 by mica powder, glass dust, montmorillonite and wollastonite with weight：25：25：25 compositions
Mixture.
Described silane adjuvant A is by hydroxyl-terminated injecting two methyl siloxane, tetramethyl divinyl disilazane, vinyl three
Methoxy silane and VTES compare 14 with weight：2：0.6：The mixture of 0.6 composition.
Described lubricant A is to compare 0.15 by zinc stearate and stearic acid with weight:The mixture of 0.15 composition；Described resistance
Combustion agent is the platinum fire retardant of 3000ppm for platinum mass content；Described vulcanizing agent is 2,5- dimethyl -2,5- two（Tert-butyl group mistake
Oxidation）Hexane.
Described silicone rubber B is to compare 70 by methyl vinyl silicone rubber a and methyl vinyl silicone rubber b with weight：70 compositions
Mixture；Wherein, the contents of ethylene of methyl vinyl silicone rubber a is 0.06%, and molecular weight is 660,000；Methyl ethylene silicon
The contents of ethylene of rubber b is 0.18%, and molecular weight is 660,000.
Described filler B is with weight by ultrafine aluminium hydroxide micropowder, super fine magnesium hydroxide micropowder, Calcium Carbonate and zinc oxide
Ratio 220：30：20：The mixture of 20 compositions；Described silane adjuvant B is by vinyltrimethoxy silane and hexamethyl two silicon nitrogen
Alkane compares 4 with weight：The mixture of 2 compositions；Described lubricant B is zinc stearate.
A kind of preparation method of ceramic fire resistant flame retardant silicone rubber, comprises the steps：
（One）The preparation of component A：
1st, first in banbury, put into raw material silicone rubber A, stir 6min；
2nd, put into lubricant A and part reinforcing agent, filler A, then put into silane adjuvant A；
3rd, after the part reinforcing agent putting into, filler A mix, more remaining reinforcing agent, filler A are put in five times；
4th, after will be agglomerating for above mixing raw materials, intensification refining glue, obtain banburying glue；
5th, banburying glue is carried out discharging, in input mill, mill is uniform, lower roll, set aside for use；
（Two）The preparation of component B：
1）, first in banbury, put into raw material silicone rubber B, stir 6min；
2）, put into lubricant B and partially filled agent B, then put into silane adjuvant B；
3）, after partially filled agent B that puts into mixes, then put into remaining filler B in five times；
4）, will be agglomerating for above mixing raw materials after, intensification refining glue, obtain banburying glue；
5）, banburying glue carried out discharging, put in mill mill uniformly, lower roll, set aside for use；
（Three）The preparation of ceramic fire resistant flame retardant silicone rubber：
（1）, component A and component B are put in mill mill uniformly in proportion, add fire retardant, lower roll after thin logical five times, put
Enter filter, filtered with 150 mesh filter screens, obtain glue of beginning to pratise；
（2）, vulcanizing agent added to begin to pratise mix in glue, put into mould and carry out sulfidization molding, prepared ceramic fire resistant flame retardant silicon rubber
Glue.
In described step 4, the technological parameter of intensification refining glue is：After temperature rises to 110 DEG C, mediate 100min, then evacuation
80min, vacuum is in -0.10Mpa；Described step 4）In, the technological parameter of intensification refining glue is：After temperature rises to 110 DEG C, mediate
40min, then evacuation 80min, vacuum is in -0.10Mpa；Described step（2）In, curing temperature is 180 DEG C, and cure time is
8min.
The mechanical and physical performance of the ceramic fire resistant flame retardant silicone rubber that embodiment 1-5 is obtained is as shown in table 1：
Table 1
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Shore hardness（A） | 86 | 88 | 88 | 90 | 89 |
| Resilience | 46 | 50 | 50 | 48 | 49 |
| Tensile strength（MPa） | 8.2 | 8.5 | 8 | 8.8 | 8.6 |
| Elongation at break（%） | 110 | 120 | 130 | 150 | 140 |
| Tearing strength（kN/M） | 13 | 15 | 14 | 16 | 15 |
| Specific insulation（Ω·cm） | 3.5×1015 | 5×1015 | 2.7×1015 | 2.3×1015 | 4.2×1015 |
| Proportion | 1.22 | 1.23 | 1.23 | 1.24 | 1.25 |
As can be seen from the above table, the ceramic fire resistant flame retardant silicone rubber of the present invention has preferable fire resistant flame retardant performance, also has
Preferably hardness, intensity, resilience and percentage elongation, excellent combination property.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can be realized with alternate manner,
Without departing from obvious replacement any on the premise of present inventive concept all within protection scope of the present invention.
Claims (10)
1. a kind of ceramic fire resistant flame retardant silicone rubber it is characterised in that：It compares 0.8-1.2 by component A and component B with weight:1 group
Become, wherein, component A includes the raw material of following weight portion：
Silicone rubber A 60-140 part
Reinforcing agent 35-45 part
Filler A 60-100 part
Silane adjuvant A 11.4-17.2 part
Lubricant A 0.15-0.25 part
Fire retardant 0.1-0.3 part
Vulcanizing agent 0.5-1.5 part；
Component B includes the raw material of following weight portion：
Silicone rubber B 60-140 part
Filler B 230-290 part
Silane adjuvant B 3-6 part
Lubricant B 0.2-0.4 part.
2. a kind of ceramic fire resistant flame retardant silicone rubber according to claim 1 it is characterised in that：Described silicone rubber A be by
Methyl vinyl silicone rubber A and methyl vinyl silicone rubber B compares 30-70 with weight：The mixture of 30-70 composition；Wherein, methyl
The contents of ethylene of vinylsiloxane rubber A is 0.02-0.06%, and molecular weight is 64-66 ten thousand；The ethylene of methyl vinyl silicone rubber B
Base content is 0.21-0.25%, and molecular weight is 64-66 ten thousand.
3. a kind of ceramic fire resistant flame retardant silicone rubber according to claim 1 it is characterised in that：Described reinforcing agent is particle diameter
In 10-50nm, specific surface area in 200-300m2The gas-phase silica of/g.
4. a kind of ceramic fire resistant flame retardant silicone rubber according to claim 1 it is characterised in that：Described filler A be by
Mica powder, glass dust, montmorillonite and wollastonite compare 15-25 with weight：15-25：15-25：The mixture of 15-25 composition.
5. a kind of ceramic fire resistant flame retardant silicone rubber according to claim 1 it is characterised in that：Described silane adjuvant A is
By hydroxyl-terminated injecting two methyl siloxane, tetramethyl divinyl disilazane, vinyltrimethoxy silane and vinyl three second
TMOS compares 10-14 with weight：1-2：0.2-0.6：The mixture of 0.2-0.6 composition.
6. a kind of ceramic fire resistant flame retardant silicone rubber according to claim 1 it is characterised in that：Described lubricant A be by
Zinc stearate and stearic acid compare 0.05-0.15 with weight:The mixture of 0.05-0.15 composition；Described fire retardant contains for platinum quality
Measure the platinum fire retardant for 1000-3000ppm；Described vulcanizing agent is 2,5- dimethyl -2,5- two（Tert-butyl hydroperoxide）Hexane.
7. a kind of ceramic fire resistant flame retardant silicone rubber according to claim 1 it is characterised in that：Described silicone rubber B be by
Methyl vinyl silicone rubber a and methyl vinyl silicone rubber b compares 30-70 with weight：The mixture of 30-70 composition；Wherein, methyl
The contents of ethylene of vinylsiloxane rubber a is 0.02-0.06%, and molecular weight is 64-66 ten thousand；The ethylene of methyl vinyl silicone rubber b
Base content is 0.12-0.20%, and molecular weight is 64-66 ten thousand.
8. a kind of ceramic fire resistant flame retardant silicone rubber according to claim 1 it is characterised in that：Described filler B be by
Ultrafine aluminium hydroxide micropowder, super fine magnesium hydroxide micropowder, Calcium Carbonate and zinc oxide compare 200-220 with weight：20-30：5-20：5-
The mixture of 20 compositions；Described silane adjuvant B is to compare 2- by vinyltrimethoxy silane and hexamethyldisiloxane with weight
4：The mixture of 1-2 composition；Described lubricant B is zinc stearate.
9. a kind of ceramic fire resistant flame retardant silicone rubber as described in any one of claim 1-8 preparation method it is characterised in that：
Comprise the steps：
（One）The preparation of component A：
1st, first in banbury, put into raw material silicone rubber A, stir 4-6min；
2nd, put into lubricant A and part reinforcing agent, filler A, then put into silane adjuvant A；
3rd, after the part reinforcing agent putting into, filler A mix, more remaining reinforcing agent, filler A are put in five times；
4th, after will be agglomerating for above mixing raw materials, intensification refining glue, obtain banburying glue；
5th, banburying glue is carried out discharging, in input mill, mill is uniform, lower roll, set aside for use；
（Two）The preparation of component B：
1）, first in banbury, put into raw material silicone rubber B, stir 4-6min；
2）, put into lubricant B and partially filled agent B, then put into silane adjuvant B；
3）, after partially filled agent B that puts into mixes, then put into remaining filler B in five times；
4）, will be agglomerating for above mixing raw materials after, intensification refining glue, obtain banburying glue；
5）, banburying glue carried out discharging, put in mill mill uniformly, lower roll, set aside for use；
（Three）The preparation of ceramic fire resistant flame retardant silicone rubber：
（1）, component A and component B are put in mill mill uniformly in proportion, add fire retardant, lower roll after thin logical five times, put
Enter filter, filtered with 150 mesh filter screens, obtain glue of beginning to pratise；
（2）, vulcanizing agent added to begin to pratise mix in glue, put into mould and carry out sulfidization molding, prepared ceramic fire resistant flame retardant silicon rubber
Glue.
10. a kind of ceramic fire resistant flame retardant silicone rubber according to claim 9 preparation method it is characterised in that：Described
In step 4, the technological parameter of intensification refining glue is：After temperature rises to 90-110 DEG C, mediate 100-140min, then evacuation 40-
80min, vacuum is in -0.06～-0.10Mpa；Described step 4）In, the technological parameter of intensification refining glue is：Temperature rises to 90-
After 110 DEG C, mediate 40-80min, then evacuation 40-80min, vacuum is in -0.06～-0.10Mpa；Described step（2）In,
Curing temperature is 160-180 DEG C, and cure time is 8-12min.
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| CN115458871A (en) * | 2022-10-12 | 2022-12-09 | 东莞市朗晟材料科技有限公司 | Novel fireproof high-temperature-resistant insulated high-voltage battery connecting piece and manufacturing process |
| CN115491037A (en) * | 2022-10-18 | 2022-12-20 | 浙江葆润应用材料有限公司 | Blending production method of flame-retardant, heat-insulating and fireproof material for battery |
| CN115491037B (en) * | 2022-10-18 | 2023-12-26 | 浙江葆润应用材料有限公司 | Method for producing flame-retardant heat-insulating fireproof material for battery by blending |
| CN116041962A (en) * | 2023-01-31 | 2023-05-02 | 安徽迈腾新材料有限公司 | Low-compressibility flame-retardant silicone rubber material |
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