CN109679348A - A kind of flame-proof silicon rubber and its continuous production technology and continuous production system - Google Patents

A kind of flame-proof silicon rubber and its continuous production technology and continuous production system Download PDF

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CN109679348A
CN109679348A CN201811425991.2A CN201811425991A CN109679348A CN 109679348 A CN109679348 A CN 109679348A CN 201811425991 A CN201811425991 A CN 201811425991A CN 109679348 A CN109679348 A CN 109679348A
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silicon rubber
flame
continuous production
silicone rubber
section
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CN109679348B (en
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潘鹤斌
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DONGGUAN LANGSHENG SILICON MATERIALS Co Ltd
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DONGGUAN LANGSHENG SILICON MATERIALS Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions 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
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer 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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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
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Abstract

The present invention relates to silicon rubber technical fields, more particularly to a kind of flame-proof silicon rubber and its continuous production technology and continuous production system, the flame-proof silicon rubber, the raw material including following parts by weight: 280-320 parts of composite silicone rubber, 140-160 parts of reinforcing agent, 5-10 parts of hydroxyl-terminated injecting two methyl siloxane, 0.3-0.6 parts of silane coupling agent, 270-320 parts of fire retardant, 0.3-0.6 parts of zinc stearate and 1.5-2.0 parts of plasticity regulator.Flame-proof silicon rubber of the invention improves the anti-flammability of silicon rubber by using fire retardant, simultaneously by using materials such as reinforcing agent, hydroxyl-terminated injecting two methyl siloxane and plasticity regulators, make silicon rubber obtained that there are the performances such as preferable tensile strength, elongation at break, tearing strength, high mechanical strength, stability is high, has a wide range of application.

Description

A kind of flame-proof silicon rubber and its continuous production technology and continuous production system
Technical field
The present invention relates to silicon rubber technical fields, and in particular to a kind of flame-proof silicon rubber and its continuous production technology and company Continuousization production system.
Background technique
Silicon rubber has a wide range of application since it is with preferable resistance to ag(e)ing and stability, and more application is in silicone tube, electricity In the products such as power covering material, but the anti-flammability of current silastic material is lower, and drop is easy to appear in encountering combustion process The phenomenon that falling reduces the mechanical strengths such as the tensile strength, elongation at break, tearing strength of silastic product and machine-shaping Property, is not able to satisfy requirement of the existing market to Silicone Rubber, using being subject to certain restrictions.
Summary of the invention
In order to overcome shortcoming and defect existing in the prior art, the purpose of the present invention is to provide a kind of fire-retardant silicon rubbers Glue, the flame-proof silicon rubber improve the anti-flammability of silicon rubber by using fire retardant, while by using reinforcing agent, terminal hydroxy group poly- two The materials such as methylsiloxane and plasticity regulator make silicon rubber obtained have preferable tensile strength, elongation at break, tear The performances such as resistance to spalling, high mechanical strength, stability is high, has a wide range of application.
Another object of the present invention is to provide a kind of preparation method of flame-proof silicon rubber, the preparation method simple process, Convenient operation and control, quality are stablized, and high production efficiency, production cost is low, and silicon rubber obtained can be made to have preferably stretching strong The mechanical performances such as degree, elongation at break, tearing strength and stability, can large-scale industrial production.
A further object of the present invention is to provide a kind of continuous production systems applied to silicon rubber continuous production technology System, the production system can be such that silicon rubber material squeezes continually by mixing equipment, kneader device, high-speed mixing equipment, twin-screw Equipment carries out the preparation of silicon rubber out, produces serialization, and centre, which does not generate, to be cut short, and is connected between each equipment, improves silicon rubber Production efficiency, and unbroken production procedure makes silicon rubber obtained have preferable tensile strength, elongation at break and tear Resistance to spalling.
The purpose of the invention is achieved by the following technical solution: a kind of flame-proof silicon rubber, the raw material including following parts by weight:
The present invention prepares silicon rubber by using the raw material of mentioned kind, improves the fire-retardant of silicon rubber by using fire retardant Property, while by using materials such as reinforcing agent, hydroxyl-terminated injecting two methyl siloxane and plasticity regulators, make silicon rubber obtained With the performances such as preferable tensile strength, elongation at break, tearing strength, high mechanical strength, stability is high, has a wide range of application.
Wherein, the mechanical strength of silicon rubber can be improved by using reinforcing agent;The hydroxyl-terminated injecting two methyl siloxane of use It is avoided that the structuring phenomenons such as silicon rubber is hardened in storage placement process, plasticity is lower, processing performance reduces, improves The stability of silicon rubber (needs to re-start mixing if the silicon rubber for structuring occurred or heat treatment goes to improve structuring Phenomenon, but process costs are increased simultaneously, and reduce production efficiency and quality), meanwhile, hydroxyl-terminated injecting two methyl siloxane energy It is reacted with the Si-OH base on reinforcing agent (precipitated silica) surface, is allowed to hydrophobization, more raising reinforcing agent is in silicon rubber system Dispersibility, and inhibit the structuring of silicon rubber;And pass through the dosage of strict control hydroxyl-terminated injecting two methyl siloxane, it can make to be made Silicon rubber there is preferable tensile strength if the dosage of hydroxyl-terminated injecting two methyl siloxane is excessive to reduce silicon rubber Plasticity and processing forming;And if the dosage of hydroxyl-terminated injecting two methyl siloxane is very few, reduces the bonding between raw material Associativity is easy to appear structuring phenomenon.
The silane coupling agent of use can significantly improve the performances such as tensile strength, elongation at break, the tearing strength of silicon rubber, And improve wetability and dispersibility of the material in silicon rubber system, inhibit form and aspect of silicon rubber material during sulfidization molding Variation makes finished surface obtained without sticking sense;The fire retardant of use can improve the anti-flammability of silicon rubber, prevent silicon rubber from sending out Cigarette can form carbon foam layer when silicon rubber burns, and do not generate dropping, do not generate toxic gas;The stearic acid of use Zinc had not only been avoided that silicon rubber recurring structure phenomenon in storage placement process, but also can improve the demolding performace of silicon rubber, made it It is easy to demould after shaping, improves its processing forming and stability;What the plasticity regulator of use can improve silicon rubber can Plasticity improves dispersibility of the silicon rubber in silicon rubber system, and inhibits the structuring of silicon rubber, improves the anti-yellowing property of silicon rubber And release property.
Preferably, the composite silicone rubber is by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B with weight ratio For the mixture of 1:0.8-1.2 composition;Wherein, the contents of ethylene of the methyl vinyl silicone rubber A is 0.04-0.12%, Methyl content is 99.88-99.96%, and molecular weight is 550,000-65 ten thousand;The contents of ethylene of the methyl vinyl silicone rubber B is 0.14-0.18%, methyl content 99.82-99.86%, molecular weight are 550,000-65 ten thousand.
The present invention compounds composition by using two kinds of different contents of ethylene, without the methyl vinyl silicone rubber of molecular weight Composite silicone rubber ingredient, and the contents of ethylene and molecular weight of both strict controls, the characteristic grown using high molecular weight, main chain, Intermolecular active force is larger, and silicon rubber obtained can be made to have preferable mechanical strength and processing forming, wherein according to Methyl vinyl silicone rubber A and methyl vinyl silicone rubber B contents of ethylene it is very few, then reduce silicon rubber hardness, The mechanical performances such as tensile strength and sulfurization reduce vulcanization if the contents of ethylene of methyl vinyl silicone rubber is excessive Silicon rubber heat-resisting afterwards;If the molecular weight of methyl vinyl silicone rubber A and methyl vinyl silicone rubber B are lower, reduce The mechanical strength and processing forming of silicon rubber finished product.
It is further preferred that the chemical formula of above-mentioned methyl vinyl silicone rubber A, methyl vinyl silicone rubber B are following institute Show:
Wherein, the n=8730-8780, m=3-10 of the methyl vinyl silicone rubber A;The methyl vinyl silicone rubber The n=8050-8150 of B, m=10-15.
Preferably, the reinforcing agent is specific surface area in 200-300m2The precipitated silica of/g;The silane coupling agent is At least one of vinyltrimethoxysilane, propyl trimethoxy silicane and vinyltriethoxysilane.
The present invention can improve significantly the resilience of silicon rubber, tensile strength, pull apart elongation by using precipitated silica The performances such as rate, tearing strength, and the specific surface area of strict control precipitated silica can improve precipitated silica and unclassified stores Contact area, make it easier to unclassified stores phase reaction, and partial size is small, precipitated silica can be made to be well dispersed in silicon rubber, Effectively improve the mechanical strength of silicon rubber.
And by using the silane coupling agent of mentioned kind, can significantly improve the tensile strength of silicon rubber, elongation at break, The performances such as tearing strength improve wetability and dispersibility of the material in silicon rubber system, and the polymerization of silicon rubber material is promoted to hand over Connection inhibits or mitigates the form and aspect variation in sulfidation, feels silastic surface obtained without adherency.More preferably, described Silane coupling agent is vinyltrimethoxysilane.
Preferably, the fire retardant is with weight ratio by aluminium hydroxide and melamine cyanurate for 250-300:50-70 The mixture of composition.
The present invention, as fire retardant, can improve the anti-flammability and anti-drip for improving silicon rubber by using mentioned kind; Wherein, the melamine cyanurate of use forms carbon foam layer in silicon rubber burning as in silicon rubber but flame retardant, And the aluminium hydroxide used matches effect with melamine cyanurate, can prevent as the inorganic fire-retarded additive in silicon rubber Only silicon rubber smoke does not generate dropping, does not generate toxic gas, and flame retardant effect is good.
Preferably, the plasticity regulator is made of hydroxy silicon oil and containing hydrogen silicone oil with weight ratio for 1:0.8-1.2 Mixture.
The present invention can effectively improve the plasticity of silicon rubber by using the plasticity regulator of mentioned kind, increase anti- Huang Xing, wherein the hydroxy silicon oil of use can effectively improve dispersibility of the precipitated silica in silicon rubber, and inhibit silicon rubber object The structuring of material adjusts the plasticity of silicon rubber;The containing hydrogen silicone oil of use can effectively adjust the plasticity of silicon rubber material, improve The anti-yellowing property of silicon rubber.
Another object of the present invention is achieved through the following technical solutions: a kind of serialization of flame-proof silicon rubber as described above Production technology includes the following steps:
(1) mixing: in parts by weight, composite silicone rubber being added and is stirred mixing into mixing equipment, and object is made Expect A;
(2) it mediates: according to parts by weight, by reinforcing agent, zinc stearate, hydroxyl-terminated injecting two methyl siloxane, silane coupling agent And material A made from step (1) is added into kneader device, stirs evenly, and mediates agglomerating rear obtained material B;
(3) it is kneaded: step (2) material B being added and is kneaded into high-speed mixing equipment, mixing materials are made;
(4) extrusion molding: mixing materials made from step (3) are added into twin-screw extrusion equipment, and twin-screw agitation is mixed Material, is added fire retardant by seven sections of extrusion moldings, and in the 5th section of extrusion molding, and being added at the 7th section of extrusion molding can Modeling degree regulator, is then filtered, and flame-proof silicon rubber is made.
The present invention prepares silicon rubber by using above-mentioned steps, and simple process, convenient operation and control, quality is stable, production High-efficient, production cost is low, and silicon rubber obtained can be made to have the machines such as preferable tensile strength, elongation at break, tearing strength Tool performance and stability, can large-scale industrial production;Wherein, joined by the addition sequence of strict control unclassified stores and processing Number is first added reinforcing agent, zinc stearate, hydroxyl-terminated injecting two methyl siloxane, silane coupling agent into composite silicone rubber, can mention While high silicon rubber intensity, inhibit the structuring phenomenon of silicon rubber, and improve the interior release property of silicon rubber, inhibits sulfidation In form and aspect variation, feel finished surface obtained without adherency;Then high speed mixing is carried out, material is adequately mixed, Extrusion molding, while fire retardant and plasticity regulator being added in extrusion process, improve the anti-flammability and plasticity of silicon rubber.
Preferably, in the step (3), the revolving speed of mixing is 1400-1600rpm;In the step (4), the filtering It is filtered using 180-220 mesh filter screen, the 4th section of the extrusion molding and the 6th section carries out vacuumize process, and vacuum degree is equal For -0.06MPa~-0.10MPa.
The present invention is filtered by using 180-220 mesh filter screen, is removed the bulky grain for generation of reuniting in material, is improved after carrying out The sophistication and uniformity of the continuous silicon rubber for carrying out sulfidization molding;And by carrying out vacuumize process during extrusion molding, Moisture and low molecular composition in material can be made to volatilize under vacuum, the compactness and quality of silicon rubber is improved, prevent Volatile harmful substance impacts the appearance and performance of product.
Preferably, in the step (4), the temperature of the first segment of extrusion molding is 115-125 DEG C, and the temperature of second segment is 125-135 DEG C, the temperature of third section is 135-145 DEG C, and the 4th section of temperature is 145-155 DEG C, and the 5th section of temperature is 145- 155 DEG C, the 6th section of temperature is 150-155 DEG C, and the 7th section of temperature is 155-165 DEG C.
The present invention passes through each section of strict control of temperature, can effectively adjust silicon rubber material cutting during extrusion molding It cuts heat, reduces material viscosity, accelerate mobility, reduce the harm of shear heat, while preventing melt from cooling down, keep constant temperature and sufficiently Exhaust, (reduction of melt pressure can be such that melt temperature declines simultaneously, and then change the friction inside extrusion equipment and shearing Degree, the plasticizing for aggravating material are bad), make silicon rubber obtained that there is preferable plasticity and processing forming, mechanical performance Good, stability is high.
Another object of the present invention is achieved through the following technical solutions: one kind being applied to above-mentioned silicon rubber continuous production work The continuous production system of skill, including mixing equipment, kneader device, high-speed mixing equipment, twin-screw extrusion equipment, filtering dress Set, the first feeder apparatus for supplying reinforcing agent, the second feeder apparatus for supplying zinc stearate, for supplying terminal hydroxy group The third feeder apparatus of dimethyl silicone polymer, the 4th feeder apparatus for supplying silane coupling agent, for supplying fire retardant The 5th feeder apparatus and the 6th feeder apparatus for supplying plasticity regulator, the twin-screw extrusion equipment include successively The feed inlet of connection, the first extruding zone, the second extruding zone, third extruding zone, the 4th extruding zone, the 5th extruding zone, the 6th squeeze out Section and the 7th extruding zone;
The output end of the mixing equipment, the output end of the first feeder apparatus, the output end of the second feeder apparatus, third supply The output end of the output end, the 4th feeder apparatus of expecting equipment is connected to the input terminal of the kneader device, the mixed at high speed The input terminal of equipment is connected to the output end of the kneader device, and the output end of the high-speed mixing equipment and the twin-screw squeeze The feed inlet connection of equipment out, the output end of the 5th feeder apparatus is connected to the input terminal of the 5th extruding zone, described The output end of 6th feeder apparatus is connected to the input terminal of the 7th extruding zone, the output end of the 7th extruding zone with it is described The input terminal of filter device is connected to.
The present invention by using above equipment as the production system for preparing silicon rubber, can continually by mixing equipment, Kneader device, high-speed mixing equipment, twin-screw extrusion equipment carry out the preparation of silicon rubber, produce serialization, and centre, which does not generate, cuts It is short, it is connected between each equipment, improves the production efficiency of silicon rubber, and unbroken production procedure has silicon rubber obtained Preferable tensile strength, elongation at break and tearing strength, will not make the mechanicalness of silicon rubber because of the manufacturing process of interruption Can be impacted, improve the stability of product.
Wherein, methyl vinyl silicone rubber A and methyl vinyl silicone rubber B, which is added into mixing equipment, carries out mixing, so Directly material A is delivered in kneader device afterwards, while being also delivered to reinforcing agent in kneader device by the first feeder apparatus, Zinc stearate is delivered in kneader device by the second feeder apparatus, hydroxyl-terminated injecting two methyl siloxane is fed by third Equipment is delivered in kneader device, silane coupling agent is delivered in kneader device by the 4th feeder apparatus, in kneader device Middle carry out mixing, kneading is agglomerating, and material B obtained is fed directly to high-speed mixing equipment by the output end of kneader device and carries out Mixed at high speed, the mixing materials after mixed at high speed are fed directly in twin-screw extrusion equipment by the output end of high-speed mixing equipment Extrusion molding is carried out, and fire retardant is delivered to the 5th extruding zone in twin-screw extrusion equipment by the 5th feeder apparatus, it is plastic Degree regulator is delivered to the 7th extruding zone in twin-screw extrusion equipment by the 6th feeder apparatus, realizes the continuous of silicon rubber Metaplasia produces, and in the process uninterruptedly, improves production efficiency, reduces the cost of production technology.
Preferably, the continuous production system further include the first vacuum evacuation device for being vacuumized to the 4th extruding zone and The second vacuum evacuation device for being vacuumized to the 6th extruding zone.
The present invention is vacuumized by the way that the first vacuum evacuation device and second is respectively set in the 4th extruding zone and the 6th extruding zone Device can make moisture and low molecular composition in material volatilize under vacuum, improve the compactness and quality of silicon rubber, prevent Only volatile harmful substance impacts the appearance and performance of product.
The beneficial effects of the present invention are: flame-proof silicon rubber of the invention improves the fire-retardant of silicon rubber by using fire retardant Property, while by using materials such as reinforcing agent, hydroxyl-terminated injecting two methyl siloxane and plasticity regulators, make silicon rubber obtained With the performances such as preferable tensile strength, elongation at break, tearing strength, high mechanical strength, stability is high, has a wide range of application.
The preparation method simple process of flame-proof silicon rubber of the present invention, convenient operation and control, quality are stablized, high production efficiency, Production cost is low, can make silicon rubber obtained have the mechanical performances such as preferable tensile strength, elongation at break, tearing strength and Stability, can large-scale industrial production.
The present invention is applied to the continuous production system of silicon rubber continuous production technology, can make silicon rubber material continuously The preparation that silicon rubber is carried out by mixing equipment, kneader device, high-speed mixing equipment, twin-screw extrusion equipment, produces serialization, Centre, which does not generate, to be cut short, and is connected between each equipment, is improved the production efficiency of silicon rubber, and unbroken production procedure makes to be made Silicon rubber have preferable tensile strength, elongation at break and tearing strength.
Detailed description of the invention
Fig. 1 is the system structure diagram of continuous production system of the present invention;
Appended drawing reference are as follows: 1-mixing equipment, 2-kneader devices, 3-high-speed mixing equipments, 4-twin-screw extrusion equipments, 41-feed inlets, the 42-the first extruding zone, the 43-the second extruding zone, 44-third extruding zones, the 45-the four extruding zone, 46-the Five extruding zones, the 47-the six extruding zone, the 48-the seven extruding zone, 5-filter devices, the 61-the first feeder apparatus, 62-the second Feeder apparatus, 63-thirds feed set, the 64-the four feeder apparatus, the 65-the five feeder apparatus, the 66-the six feeder apparatus, 71-the first vacuum evacuation device, the 72-the second vacuum evacuation device.
Specific embodiment
For the ease of the understanding of those skilled in the art, make below with reference to 1 couple of present invention of examples and drawings further Illustrate, the content that embodiment refers to not is limitation of the invention.
Embodiment 1
A kind of flame-proof silicon rubber, the raw material including following parts by weight:
The composite silicone rubber is with weight ratio by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B for 1:0.8 The mixture of composition;Wherein, the contents of ethylene of the methyl vinyl silicone rubber A is 0.04%, and methyl content is 99.96%, molecular weight is 550,000;The contents of ethylene of the methyl vinyl silicone rubber B is 0.14%, and methyl content is 99.86%, molecular weight is 550,000.
Above-mentioned methyl vinyl silicone rubber A, methyl vinyl silicone rubber B chemical formula be as follows:
Wherein, the n=8780, m=3 of the methyl vinyl silicone rubber A;The n=of the methyl vinyl silicone rubber B 8150, m=10.
The reinforcing agent is specific surface area in 200m2The precipitated silica of/g;The silane coupling agent is propyl trimethoxy Base silane.
The mixture that the fire retardant is made of aluminium hydroxide and melamine cyanurate with weight ratio for 250:50.
The mixture that the plasticity regulator is made of hydroxy silicon oil and containing hydrogen silicone oil with weight ratio for 1:0.8.
A kind of continuous production technology of flame-proof silicon rubber as described above, includes the following steps:
(1) mixing: in parts by weight, composite silicone rubber being added and is stirred mixing into mixing equipment, and object is made Expect A;
(2) it mediates: according to parts by weight, by reinforcing agent, zinc stearate, hydroxyl-terminated injecting two methyl siloxane, silane coupling agent And material A made from step (1) is added into kneader device, stirs evenly, and mediates agglomerating rear obtained material B;
(3) it is kneaded: step (2) material B being added and is kneaded into high-speed mixing equipment, mixing materials are made;
(4) extrusion molding: mixing materials made from step (3) are added into twin-screw extrusion equipment, and twin-screw agitation is mixed Material, is added fire retardant by seven sections of extrusion moldings, and in the 5th section of extrusion molding, and being added at the 7th section of extrusion molding can Modeling degree regulator, is then filtered, and flame-proof silicon rubber is made.
In the step (3), the revolving speed of mixing is 1400rpm;In the step (4), the filtering uses 180 mesh filter screens Filtering, the 4th section of the extrusion molding and the 6th section carries out vacuumize process, and vacuum degree is -0.06MPa.
In the step (4), the temperature of the first segment of extrusion molding is 115 DEG C, and the temperature of second segment is 125 DEG C, third The temperature of section is 135 DEG C, and the 4th section of temperature is 145 DEG C, and the 5th section of temperature is 145 DEG C, and the 6th section of temperature is 150 DEG C, 7th section of temperature is 155 DEG C.
Embodiment 2
A kind of flame-proof silicon rubber, the raw material including following parts by weight:
The composite silicone rubber is with weight ratio by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B for 1:1 group At mixture;Wherein, the contents of ethylene of the methyl vinyl silicone rubber A is 0.08%, methyl content 99.82%, Molecular weight is 600,000;The contents of ethylene of the methyl vinyl silicone rubber B is 0.16%, methyl content 99.84%, molecule Amount is 600,000.
Above-mentioned methyl vinyl silicone rubber A, methyl vinyl silicone rubber B chemical formula be as follows:
Wherein, the n=8750, m=7 of the methyl vinyl silicone rubber A;The n=of the methyl vinyl silicone rubber B 8100, m=13.
The reinforcing agent is specific surface area in 250m2The precipitated silica of/g;The silane coupling agent is vinyl front three Oxysilane.
The mixture that the fire retardant is made of aluminium hydroxide and melamine cyanurate with weight ratio for 270:60.
The mixture that the plasticity regulator is made of hydroxy silicon oil and containing hydrogen silicone oil with weight ratio for 1:1.
A kind of continuous production technology of flame-proof silicon rubber as described above, includes the following steps:
(1) mixing: in parts by weight, composite silicone rubber being added and is stirred mixing into mixing equipment, and object is made Expect A;
(2) it mediates: according to parts by weight, by reinforcing agent, zinc stearate, hydroxyl-terminated injecting two methyl siloxane, silane coupling agent And material A made from step (1) is added into kneader device, stirs evenly, and mediates agglomerating rear obtained material B;
(3) it is kneaded: step (2) material B being added and is kneaded into high-speed mixing equipment, mixing materials are made;
(4) extrusion molding: mixing materials made from step (3) are added into twin-screw extrusion equipment, and twin-screw agitation is mixed Material, is added fire retardant by seven sections of extrusion moldings, and in the 5th section of extrusion molding, and being added at the 7th section of extrusion molding can Modeling degree regulator, is then filtered, and flame-proof silicon rubber is made.
In the step (3), the revolving speed of mixing is 1500rpm;In the step (4), the filtering uses 200 mesh filter screens Filtering, the 4th section of the extrusion molding and the 6th section carries out vacuumize process, and vacuum degree is -0.08MPa.
In the step (4), the temperature of the first segment of extrusion molding is 120 DEG C, and the temperature of second segment is 130 DEG C, third The temperature of section is 140 DEG C, and the 4th section of temperature is 150 DEG C, and the 5th section of temperature is 150 DEG C, and the 6th section of temperature is 153 DEG C, 7th section of temperature is 160 DEG C.
Embodiment 3
A kind of flame-proof silicon rubber, the raw material including following parts by weight:
The composite silicone rubber is with weight ratio by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B for 1:1.2 The mixture of composition;Wherein, the contents of ethylene of the methyl vinyl silicone rubber A is 0.12%, and methyl content is 99.88%, molecular weight is 650,000;The contents of ethylene of the methyl vinyl silicone rubber B is 0.18%, and methyl content is 99.82%, molecular weight is 650,000.
Above-mentioned methyl vinyl silicone rubber A, methyl vinyl silicone rubber B chemical formula be as follows:
Wherein, the n=8730, m=10 of the methyl vinyl silicone rubber A;The n=of the methyl vinyl silicone rubber B 8050, m=15.
The reinforcing agent is specific surface area in 300m2The precipitated silica of/g;The silane coupling agent is three second of vinyl Oxysilane.
The mixture that the fire retardant is made of aluminium hydroxide and melamine cyanurate with weight ratio for 300:70.
The mixture that the plasticity regulator is made of hydroxy silicon oil and containing hydrogen silicone oil with weight ratio for 1:1.2.
A kind of continuous production technology of flame-proof silicon rubber as described above, includes the following steps:
(1) mixing: in parts by weight, composite silicone rubber being added and is stirred mixing into mixing equipment, and object is made Expect A;
(2) it mediates: according to parts by weight, by reinforcing agent, zinc stearate, hydroxyl-terminated injecting two methyl siloxane, silane coupling agent And material A made from step (1) is added into kneader device, stirs evenly, and mediates agglomerating rear obtained material B;
(3) it is kneaded: step (2) material B being added and is kneaded into high-speed mixing equipment, mixing materials are made;
(4) extrusion molding: mixing materials made from step (3) are added into twin-screw extrusion equipment, and twin-screw agitation is mixed Material, is added fire retardant by seven sections of extrusion moldings, and in the 5th section of extrusion molding, and being added at the 7th section of extrusion molding can Modeling degree regulator, is then filtered, and flame-proof silicon rubber is made.
In the step (3), the revolving speed of mixing is 1600rpm;In the step (4), 220 mesh filter screen mistakes are adopted in the filtering Filter, the 4th section of the extrusion molding and the 6th section carries out vacuumize process, and vacuum degree is -0.10MPa.
In the step (4), the temperature of the first segment of extrusion molding is 125 DEG C, and the temperature of second segment is 135 DEG C, third The temperature of section is 145 DEG C, and the 4th section of temperature is 155 DEG C, and the 5th section of temperature is 155 DEG C, and the 6th section of temperature is 155 DEG C, 7th section of temperature is 165 DEG C.
Embodiment 4
See Fig. 1, a kind of continuous production system applied to above-mentioned flame-proof silicon rubber continuous production technology, including mixing Equipment 1, kneader device 2, high-speed mixing equipment 3, twin-screw extrusion equipment 4, filter device 5, first for supplying reinforcing agent Feeder apparatus 61, the second feeder apparatus 62 for supplying zinc stearate, for supplying hydroxyl-terminated injecting two methyl siloxane Three feeder apparatus 63, the 4th feeder apparatus 64 for supplying silane coupling agent, the 5th feeder apparatus for supplying fire retardant 65 and the 6th feeder apparatus 66 for supplying plasticity regulator, the twin-screw extrusion equipment 4 include it is sequentially connected into Material mouth 41, the first extruding zone 42, the second extruding zone 43, third extruding zone 44, the 4th extruding zone 45, the 5th extruding zone the 46, the 6th Extruding zone 47 and the 7th extruding zone 48;
The output end of the mixing equipment 1, the output end of the first feeder apparatus 61, the second feeder apparatus 62 output end, The output end of third feeder apparatus 63, the 4th feeder apparatus 64 output end be connected to the input terminal of the kneader device 2, institute The input terminal for stating high-speed mixing equipment 3 is connected to the output end of the kneader device 2, the output end of the high-speed mixing equipment 3 It is connected to the feed inlet of the twin-screw extrusion equipment 4, the output end and the 5th extruding zone of the 5th feeder apparatus 65 46 input terminal connection, the output end of the 6th feeder apparatus 66 is connected to the input terminal of the 7th extruding zone 48, described The output end of 7th extruding zone 48 is connected to the input terminal of the filter device 5.
The continuous production system further includes the first vacuum evacuation device 71 and use for vacuumizing to the 4th extruding zone 45 In the second vacuum evacuation device 72 for vacuumizing 46 to the 6th extruding zone.
Comparative example 1
This comparative example and the difference of above-described embodiment 2 are:
A kind of silicon rubber, the raw material including following parts by weight:
The composite silicone rubber is with weight ratio by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B for 1:1 group At mixture;Wherein, the contents of ethylene of the methyl vinyl silicone rubber A is 0.08%, methyl content 99.82%, Molecular weight is 600,000;The contents of ethylene of the methyl vinyl silicone rubber B is 0.16%, methyl content 99.84%, molecule Amount is 600,000.
Above-mentioned methyl vinyl silicone rubber A, methyl vinyl silicone rubber B chemical formula be as follows:
Wherein, the n=8750, m=7 of the methyl vinyl silicone rubber A;The n=of the methyl vinyl silicone rubber B 8100, m=13.
The reinforcing agent is specific surface area in 250m2The precipitated silica of/g;The silane coupling agent is vinyl front three Oxysilane.
The mixture that the plasticity regulator is made of hydroxy silicon oil and containing hydrogen silicone oil with weight ratio for 1:1.
Comparative example 2
This comparative example and the difference of above-described embodiment 2 are:
A kind of flame-proof silicon rubber, the raw material including following parts by weight:
The composite silicone rubber is with weight ratio by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B for 1:1 group At mixture;Wherein, the contents of ethylene of the methyl vinyl silicone rubber A is 0.08%, methyl content 99.82%, Molecular weight is 600,000;The contents of ethylene of the methyl vinyl silicone rubber B is 0.16%, methyl content 99.84%, molecule Amount is 600,000.
Above-mentioned methyl vinyl silicone rubber A, methyl vinyl silicone rubber B chemical formula be as follows:
Wherein, the n=8750, m=7 of the methyl vinyl silicone rubber A;The n=of the methyl vinyl silicone rubber B 8100, m=13.
The reinforcing agent is specific surface area in 250m2The precipitated silica of/g;The silane coupling agent is vinyl front three Oxysilane.
The fire retardant is for aluminium hydroxide.
The mixture that the plasticity regulator is made of hydroxy silicon oil and containing hydrogen silicone oil with weight ratio for 1:1.
Comparative example 3
This comparative example and the difference of above-described embodiment 2 are:
A kind of flame-proof silicon rubber, the raw material including following parts by weight:
The composite silicone rubber is with weight ratio by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B for 1:1 group At mixture;Wherein, the contents of ethylene of the methyl vinyl silicone rubber A is 0.08%, methyl content 99.82%, Molecular weight is 600,000;The contents of ethylene of the methyl vinyl silicone rubber B is 0.16%, methyl content 99.84%, molecule Amount is 600,000.
Above-mentioned methyl vinyl silicone rubber A, methyl vinyl silicone rubber B chemical formula be as follows:
Wherein, the n=8750, m=7 of the methyl vinyl silicone rubber A;The n=of the methyl vinyl silicone rubber B 8100, m=13.
The reinforcing agent is specific surface area in 250m2The precipitated silica of/g;The silane coupling agent is vinyl front three Oxysilane.
The fire retardant is melamine cyanurate.
The mixture that the plasticity regulator is made of hydroxy silicon oil and containing hydrogen silicone oil with weight ratio for 1:1.
Comparative example 4
This comparative example and the difference of above-described embodiment 2 are:
A kind of silicon rubber, the raw material including following parts by weight:
The composite silicone rubber is with weight ratio by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B for 1:1 group At mixture;Wherein, the contents of ethylene of the methyl vinyl silicone rubber A is 0.08%, methyl content 99.82%, Molecular weight is 600,000;The contents of ethylene of the methyl vinyl silicone rubber B is 0.16%, methyl content 99.84%, molecule Amount is 600,000.
Above-mentioned methyl vinyl silicone rubber A, methyl vinyl silicone rubber B chemical formula be as follows:
Wherein, the n=8750, m=7 of the methyl vinyl silicone rubber A;The n=of the methyl vinyl silicone rubber B 8100, m=13.
The reinforcing agent is specific surface area in 250m2The precipitated silica of/g;The silane coupling agent is vinyl front three Oxysilane.
The mixture that the fire retardant is made of aluminium hydroxide and melamine cyanurate with weight ratio for 270:60.
Comparative example 5
This comparative example and the difference of above-described embodiment 2 are:
A kind of silicon rubber, the raw material including following parts by weight:
The composite silicone rubber is with weight ratio by methyl vinyl silicone rubber A and methyl vinyl silicone rubber B for 1:1 group At mixture;Wherein, the contents of ethylene of the methyl vinyl silicone rubber A is 0.08%, methyl content 99.82%, Molecular weight is 600,000;The contents of ethylene of the methyl vinyl silicone rubber B is 0.16%, methyl content 99.84%, molecule Amount is 600,000.
Above-mentioned methyl vinyl silicone rubber A, methyl vinyl silicone rubber B chemical formula be as follows:
Wherein, the n=8750, m=7 of the methyl vinyl silicone rubber A;The n=of the methyl vinyl silicone rubber B 8100, m=13.
The reinforcing agent is specific surface area in 250m2The precipitated silica of/g;The silane coupling agent is vinyl front three Oxysilane.
The mixture that the fire retardant is made of aluminium hydroxide and melamine cyanurate with weight ratio for 270:60.
The mixture that the plasticity regulator is made of hydroxy silicon oil and containing hydrogen silicone oil with weight ratio for 1:1.
Silicon rubber made from above-described embodiment 1-3 and comparative example 1-5 is subjected to anti-flammability, hardness, tensile strength, pulls apart and stretches The test of the mechanical and physical performances such as long rate, tearing strength, it is shown that test result is as follows:
Flame-proof silicon rubber of the invention improves the anti-flammability of silicon rubber by using fire retardant, while by using enhancing The materials such as agent, hydroxyl-terminated injecting two methyl siloxane and plasticity regulator, make silicon rubber obtained have preferable tensile strength, The performances such as elongation at break, tearing strength, high mechanical strength, stability is high, has a wide range of application.
Compared with Example 2, without using fire retardant in comparative example 1, silicon rubber flame-retardant obtained is lower, and stretches strong Degree, elongation at break, the performance of tearing strength are obvious relatively low, illustrate that the present invention can significantly improve silicon rubber by using fire retardant The anti-flammability of glue, and the performances such as tensile strength, elongation at break, tearing strength for improving silicon rubber.
Compared with Example 2, using the fire retardant (aluminium hydroxide) of one-component, silicon rubber obtained in comparative example 2 Glue anti-flammability is lower, and the performance of tensile strength, elongation at break, tearing strength is obvious relatively low, illustrates the present invention by adopting With the fire retardant of compounding component, the anti-flammability of silicon rubber can be effectively improved, and the aluminium hydroxide used is as the nothing in silicon rubber Machine flame-retardant additive matches effect with melamine cyanurate, can prevent silicon rubber smoke, does not generate dropping, does not generate Toxic gas, flame retardant effect are good.
Compared with Example 2, it is made in comparative example 3 using the fire retardant (melamine cyanurate) of one-component Silicon rubber flame-retardant it is lower, and the performance of tensile strength, elongation at break, tearing strength is obvious relatively low, and relative to right Using for inorganic fire retardant, physical and chemical performance is promoted ratio 2, illustrates the present invention by using the resistance of compounding component Agent is fired, and is combined with organic fire-retardant using inorganic fire retardants, can significantly improve the anti-flammability of silicon rubber, and the trimerization of use Cyanamide cyanuric acid forms carbon foam layer in silicon rubber burning, mutually ties with aluminium hydroxide as the nitrogenated flame retardant in silicon rubber It closes, silicon rubber smoke can be prevented, do not generate dropping, do not generate toxic gas, flame retardant effect is good.
Compared with Example 2, without using plasticity regulator in comparative example 4, the tensile strength of silicon rubber obtained is pulled The performances such as disconnected elongation, tearing strength are obvious relatively low, illustrate that the present invention can improve silicon rubber by using plasticity regulator Plasticity, improve silicon rubber material dispersibility, inhibit silicon rubber material structuring, improve anti-yellowing property, the demoulding of finished product Property and processing forming.
Compared with Example 2, without using hydroxyl-terminated injecting two methyl siloxane in comparative example 5, silicon rubber obtained is stretched The performances such as intensity, elongation at break, tearing strength are obvious relatively low, illustrate the present invention by using terminal hydroxy group polydimethylsiloxanes Alkane is avoided that the structuring phenomenons such as silicon rubber is hardened in storage placement process, plasticity is lower, processing performance reduces, and mentions The comprehensive performances such as tensile strength, elongation at break, the tearing strength of high silicon rubber.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be realized with other way, Do not depart under the premise of present inventive concept it is any obviously replace it is within the scope of the present invention.

Claims (10)

1. a kind of flame-proof silicon rubber, it is characterised in that: the raw material including following parts by weight:
2. a kind of flame-proof silicon rubber according to claim 1, it is characterised in that: the composite silicone rubber is by ethylene methacrylic Base silicon rubber A and methyl vinyl silicone rubber B is with the mixture that weight ratio is that 1:0.8-1.2 is formed;Wherein, the ethylene methacrylic The contents of ethylene of base silicon rubber A is 0.04-0.12%, and methyl content 99.88-99.96%, molecular weight is 550,000-65 ten thousand; The contents of ethylene of the methyl vinyl silicone rubber B is 0.14-0.18%, methyl content 99.82-99.86%, molecular weight It is 550,000-65 ten thousand.
3. a kind of flame-proof silicon rubber according to claim 1, it is characterised in that: the reinforcing agent is specific surface area in 200- 300m2The precipitated silica of/g;The silane coupling agent is vinyltrimethoxysilane, propyl trimethoxy silicane and ethylene At least one of ethyl triethoxy silicane alkane.
4. a kind of flame-proof silicon rubber according to claim 1, it is characterised in that: the fire retardant is by aluminium hydroxide and three Poly cyanamid cyanuric acid is with the mixture that weight ratio is that 250-300:50-70 is formed.
5. a kind of flame-proof silicon rubber according to claim 1, it is characterised in that: the plasticity regulator is by hydroxyl silicon The mixture that oil and containing hydrogen silicone oil are formed with weight ratio for 1:0.8-1.2.
6. a kind of continuous production technology of flame-proof silicon rubber as described in any one in claim 1-5, it is characterised in that: including Following steps:
(1) mixing: in parts by weight, composite silicone rubber being added and is stirred mixing into mixing equipment, and material A is made;
(2) mediate: according to parts by weight, by reinforcing agent, zinc stearate, hydroxyl-terminated injecting two methyl siloxane, silane coupling agent and Material A made from step (1) is added into kneader device, stirs evenly, and mediates agglomerating rear obtained material B;
(3) it is kneaded: step (2) material B being added and is kneaded into high-speed mixing equipment, mixing materials are made;
(4) extrusion molding: mixing materials made from step (3) are added into twin-screw extrusion equipment, and twin-screw stirs mixing, warp Seven sections of extrusion moldings are crossed, and fire retardant is added in the 5th section of extrusion molding, in the 7th section of addition plasticity of extrusion molding Then regulator filters, flame-proof silicon rubber is made.
7. a kind of continuous production technology of flame-proof silicon rubber according to claim 6, it is characterised in that: the step (3) in, the revolving speed of mixing is 1400-1600rpm;In the step (4), the filtering is filtered using 180-220 mesh filter screen, institute The 4th section and the 6th section for stating extrusion molding carries out vacuumize process, and vacuum degree is -0.06MPa~-0.10MPa.
8. a kind of continuous production technology of flame-proof silicon rubber according to claim 6, it is characterised in that: the step (4) in, the temperature of the first segment of extrusion molding is 115-125 DEG C, and the temperature of second segment is 125-135 DEG C, the temperature of third section It is 135-145 DEG C, the 4th section of temperature is 145-155 DEG C, and the 5th section of temperature is 145-155 DEG C, and the 6th section of temperature is 150-155 DEG C, the 7th section of temperature is 155-165 DEG C.
9. a kind of continuous production system of the continuous production technology applied to flame-proof silicon rubber described in claim 6, special Sign is: including mixing equipment, kneader device, high-speed mixing equipment, twin-screw extrusion equipment, filter device, being used to supply increasing First feeder apparatus of strong agent, the second feeder apparatus for supplying zinc stearate, for supplying terminal hydroxy group polydimethylsiloxanes The third feeder apparatus of alkane, the 4th feeder apparatus for supplying silane coupling agent, the 5th feed for supplying fire retardant are set Standby and the 6th feeder apparatus for supplying plasticity regulator, the twin-screw extrusion equipment include sequentially connected charging Mouth, the first extruding zone, the second extruding zone, third extruding zone, the 4th extruding zone, the 5th extruding zone, the 6th extruding zone and the 7th squeeze Section out;
Output end, the output end of the first feeder apparatus, the output end of the second feeder apparatus, the third feed of the mixing equipment are set The output end of standby output end, the 4th feeder apparatus is connected to the input terminal of the kneader device, the high-speed mixing equipment Input terminal be connected to the output end of the kneader device, the output end of the high-speed mixing equipment is set with the twin-screw extrusion Standby feed inlet connection, the output end of the 5th feeder apparatus are connected to the input terminal of the 5th extruding zone, and the described 6th The output end of feeder apparatus is connected to the input terminal of the 7th extruding zone, the output end of the 7th extruding zone and the filtering The input terminal of device is connected to.
10. a kind of continuous production system of continuous production technology applied to flame-proof silicon rubber according to claim 9 System, it is characterised in that: the continuous production system further include the first vacuum evacuation device for being vacuumized to the 4th extruding zone and The second vacuum evacuation device for being vacuumized to the 6th extruding zone.
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CN110564160A (en) * 2019-08-22 2019-12-13 四川塔牌电缆绕组线有限责任公司 Fire-resistant silicone rubber and preparation method thereof
CN111534105A (en) * 2020-04-02 2020-08-14 浙江翔宇密封件有限公司 Anti-aging silicone rubber sealing material for high-speed rail sealing element and preparation method thereof
CN111875968A (en) * 2020-07-17 2020-11-03 东莞市朗晟材料科技有限公司 Flame-retardant silicone rubber for low-pressure sealing and preparation method thereof

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CN101157801A (en) * 2007-09-19 2008-04-09 上海回天化工新材料有限公司 Highly ripping-resistant high temperature sulfidation silicon rubber and method for making same
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CN110564160A (en) * 2019-08-22 2019-12-13 四川塔牌电缆绕组线有限责任公司 Fire-resistant silicone rubber and preparation method thereof
CN111534105A (en) * 2020-04-02 2020-08-14 浙江翔宇密封件有限公司 Anti-aging silicone rubber sealing material for high-speed rail sealing element and preparation method thereof
CN111875968A (en) * 2020-07-17 2020-11-03 东莞市朗晟材料科技有限公司 Flame-retardant silicone rubber for low-pressure sealing and preparation method thereof

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