CN106009694B - The carbon black filled conductive shield silicon rubber preparation method of extrusion type of ageing-resistant high rebound - Google Patents
The carbon black filled conductive shield silicon rubber preparation method of extrusion type of ageing-resistant high rebound Download PDFInfo
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- 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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Abstract
The invention discloses a kind of preparation methods of the carbon black filled conductive shield silicon rubber of extrusion type of ageing-resistant high rebound, its step is: (1) raw material of the following mass parts of preparation: 100 parts of silicon rubber, 15~30 parts of superconduction carbon black of coupling agent modification, 4~8 parts of constitution controller, 6~10 parts of vulcanizing agent；(2) raw material described in step (1) are kneaded on open mill or kneader at normal temperature；(3) rubber vulcanization obtained by step (2) is handled, vulcanizing treatment is divided to two sections.The conductive shield silicon rubber of the method for the present invention preparation has good extrusion processability energy；Preparation process is simple, at low cost；The silicon rubber of the method for the present invention preparation, has good ageing-resistant performance and elasticity, is suitable as high performance seal sizing material and uses.
Description
Technical field
The present invention relates to carbon black type conductive shield silicon rubber manufacture field, in particular to a kind of extrusion type conductive shield silicon rubber
Glue method for preparing rubber.
Background technique
A large amount of energy exploitation has had been put into harm due to electrostatic and electromagnetism model to industry and the person, researcher
Conductive shielding material.Conductive silicon rubber not only has a series of silicon rubber such as resistance to high bottom temperature, weather-proof, preferable demolding performace general
The advantages of, and it is small with conductive filler affinity, resistance variations are small, to become high-end conductive shielding material, answer extensively
For in the electronic equipments such as aerospace, ship and computer.
The conductive shield silicon rubber and its product of industrial application are mainly the conductive shield silicon rubber of filled-type at present.According to
The additive filled can be divided into the metal powder etc. of carbon system, metal, metal oxide, dielectric medium and overlay coating.Carbon black is
Most common carbon system filler not only has excellent electric conductivity, but also has good reinforcing effect, is most popular
A kind of conductive silicon rubber additive.It is all had in N220 the and N330 carbon black of ordinary carbon black such as high structure addition silicon rubber certain
Electric conductivity, but the most commonly used is acetylene carbon blacks.The silicon rubber of acetylene carbon black filling not only conducts electricity very well, and (resistivity is 0.1
~10 Ω cm), and it is inexpensive, it is one of industrial widely used conductive rubber kind.However, in order to reach good conduction
Property, the loading of acetylene carbon black is larger, and the elasticity of conductive silicon rubber is caused to reduce, and is unfavorable for making for a long time for the application environments such as sealing
With requiring.Faced with this situation, researcher develops the carbon black filled silicon rubber of the higher superconduction of structure degree, due to structure
Degree is high, and maximum loading is relatively low, therefore causes elasticity much higher than common acetylene carbon black type silicon rubber.Conducting screen at present
Covering with the carbon black filled silicon rubber of superconduction is mainly molding type technique sizing material, and seldom reports extrusion type technique sizing material.Main cause
It is that common vulcanizing agent is peroxidating two (2,4- dichloro-benzoyl) (referred to as double 2,4), vulcanizing agent tool in extrusion type silicon rubber
Play the role of that silicon rubber short vulcanization is made to be formed, is particularly suitable for normal pressure and continuously squeezes out vulcanization use.But double 2,4 are easy to and carbon black
The group on surface reacts, and reduces its curing efficiency (or even can not vulcanize) and is therefore rarely employed in extrusion type silicone rubber compounds
A large amount of carbon blacks are used as filler (referring to patent " the extrusion molding melting silicone rubber of adhesion core wire ", application number
201410276155.8).And for requiring the carbon black type filled silicon rubber of (non-antistatic) with conductive shield, it needs to fill foot
The carbon black enough measured, therefore cause extrusion process and be difficult to carry out.Extrusion process is important silicon rubber formed technique, is particularly suitable for ruler
Prepared by very little hollow product of less demanding uses.Therefore it is badly in need of exploitation extrusion type and leads carbon black filled electrical shielding silicon rubber, meets work
The needs of industry.
Summary of the invention
It is an object of the invention to propose extrusion type conductive shield silicon rubber method for preparing rubber.
To achieve the above object, the present invention adopts the following technical scheme: the extrusion type of ageing-resistant high rebound is carbon black filled leads
Electrical shielding silicon rubber preparation method, includes the following steps:
(1) prepare the raw material of following mass parts
(2) raw material described in step (1) are kneaded on open mill or kneader at normal temperature:
(3) glue stuff compounding obtained by step (2) is vulcanized, is divided to two sections:
Glue stuff compounding is squeezed out according to the extruder shape of the mouth as one speaks, and the thickness or wall thickness of extruded product are no more than 12mm, continuous
Normal pressure carries out in pipeline hot-air cure device；Extrusion fuselage and head temperature are no more than 50 DEG C, extruded velocity and vulcanization plant
The conveyor belt speed of middle pipeline matches, to form continuous production；Pipeline in vulcanization plant is usually three sections of temperature controls, every segment length
Degree is not less than 2m, and successively temperature range is respectively 180~200 DEG C of preheating section temperature, and 200~220 DEG C of warming-up section, constant temperature vulcanizes section
240~260 DEG C, conveyor belt speed is 0.1~2m/min in pipeline.
Post-processing carries out in baking oven: for room temperature to 150 DEG C, the heating-up time is 1 hour；150 DEG C~200 DEG C, heating 1 is small
When；200 DEG C of 4~6 hours of processing.
The silicon rubber is the one or two of methyl vinyl silicone rubber or methyl vinyl phenyl silicon rubber.
The vulcanizing agent is cumyl peroxide.
Superconduction carbon black is the BP2000 of magnificent photoconductive carbon black, Cabot Co., Ltd, one kind of the EC-600JD of Aksu company
Or it is several；Coupling agent is amino silicane coupling agent KH550, KH560 and KH570 and vinyl silicane coupling agent A151 and A171
One or more.
By above-mentioned superconduction carbon black and coupling agent, according to mass ratio (5~10): 1 ratio is added in ethyl alcohol, next time at 80 DEG C
Stream 4~10 hours takes out after cooling, 120 DEG C or more at a temperature of dry, grind after to get the superconduction for arriving coupling agent treatment
Carbon black.
The constitution controller is one kind or several of methylol silicone oil, hydroxymethyl phenyl silicone oil or multi-vinyl silicone oil
Kind.
In step (2) mixing process, in order to improve dispersibility, superconduction carbon black and vulcanizing agent are both needed to substep and are added.
Step (3) adds infra red heating device before preheating section, to sizing material fast shaping.
Effect of the invention is that:
The present invention has abandoned the vulcanizing agent double 2,4 that silicon rubber is often used in an extrusion process, using excessive peroxidating
Diisopropylbenzene (DIPB) (abbreviation DCP) improves curingprocess rate and quantity-produced Technological adaptability；It is coupled using constitution controller and surface
The mobility (viscosity) of the entire paste systems of adjustings such as the superconduction carbon black of agent modification, is not only suitable for squeezing out, and maintain sizing material
Higher elasticity after vulcanization.Excessive vulcanizing agent can accelerate the aging of silicon rubber, but the superconduction carbon black of chemical modification maintains
The effect steady in a long-term between rubber molecule does not cause the extrusion type conductive shield silicon rubber of preparation using reasonable formula
Glue has low ageing-resistant performance than molding type conductive shield silastic material.
The conductive shield silicon rubber of the method for the present invention preparation has good extrusion processability energy；Preparation process is simple, at
This is low；The silicon rubber of the method for the present invention preparation, has good ageing-resistant performance and elasticity, is suitable as high performance conducting screen
Cover the use of function seal sizing material.
Detailed description of the invention
Fig. 1 is present invention process schematic diagram.
Specific embodiment
The present invention is further appreciated that by specific embodiment, and field technical staff can be according to summary of the invention to this hair
It is bright to do some nonessential adjustment and improvement.
Embodiment 1:
A kind of preparation method of the carbon black filled conductive shield silicon rubber of extrusion type of the present invention comprising following step
It is rapid:
1. preparing the following raw material (being mass parts)
100 parts of methyl vinyl silicone rubber (trade mark is middle indigo plant morning twilight 110-2)；
6 parts of vulcanizing agent (cumyl peroxide)；
15 parts of superconduction carbon black (Aksu EC-600JD of coupling agent KH550 processing)
Processing method are as follows: after being cooperated by mass parts KH550:EC-600JD=1:8 and ethanol in proper amount mixing, stirring are equal
It flows back 4 hours after even at 80 DEG C, carbon black is taken out, after 120 DEG C of drying in oven, grinding.
4 parts of constitution controller (methylol silicone oil)
2. raw material described in step (1) is kneaded on a mill at normal temperature；In mixing process, peroxidating two
Isopropylbenzene and the superconduction carbon black of processing need point 5 steps to be added, and keep being kneaded uniform.
3. squeezing out one section of condition of vulcanization: extruder fuselage and head temperature are respectively 42 and 49 DEG C；8 meters of long curing tubes point
For three sections, technological temperature is 200 DEG C of preheating section, 220 DEG C of warming-up section, 240 DEG C of constant temperature zone.Pipeline tape speed is 1.5m/
min.Extruded velocity and pipeline speeds match.
Post vulcanization carries out in baking oven: for room temperature to 150 DEG C, the heating-up time is 1 hour；150 DEG C to 200 DEG C, heating 1 is small
When；200 DEG C of 4 hours of processing.
Embodiment 2:
A kind of preparation method of the carbon black filled conductive shield silicon rubber of extrusion type of the present invention comprising following step
It is rapid:
1. preparing the following raw material (being mass parts)
100 parts of methyl vinyl silicone rubber (trade mark is middle indigo plant morning twilight 110-2)；
7 parts of vulcanizing agent (cumyl peroxide)；
18 parts of superconduction carbon black (BP2000 of the Cabot of coupling agent KH570 processing)
Processing method are as follows: after being cooperated by mass parts KH570:BP2000=1:6 and ethanol in proper amount mixing, stirring are equal
It flows back 4 hours after even at 80 DEG C, carbon black is taken out, after 120 DEG C of drying in oven.
5 parts of constitution controller (multi-vinyl silicone oil)
2. raw material described in step (1) is kneaded on a mill at normal temperature；In mixing process, peroxidating two
Isopropylbenzene and the superconduction carbon black of processing need point 5 steps to be added, and keep being kneaded uniform.
3. squeezing out one section of condition of vulcanization: extruder fuselage and head temperature are respectively 40 and 46 DEG C；8 meters long heat cure pipeline
It is divided into three sections, technological temperature is 180 DEG C of preheating section, 210 DEG C of warming-up section, 255 DEG C of constant temperature zone.Pipeline tape speed is 0.3m/
min.Extruded velocity and pipeline speeds match.
Post vulcanization carries out in baking oven: for room temperature to 150 DEG C, the heating-up time is 1 hour；150 DEG C to 200 DEG C, heating 1 is small
When；200 DEG C of 5 hours of processing.
Embodiment 3:
A kind of preparation method of the carbon black filled conductive shield silicon rubber of extrusion type of the present invention comprising following step
It is rapid:
1. preparing the following raw material (being mass parts)
100 parts of methyl vinyl phenyl silicon rubber (trade mark is Shanghai Resin Factory 120-1)；
9 parts of vulcanizing agent (cumyl peroxide)；
25 parts of superconduction carbon black (the magnificent photoconductive carbon black of coupling agent A151 processing)
Processing method are as follows: by mass parts A151: magnificent light carbon black=1:9 is mixed, and ethanol in proper amount is added, stirs evenly
Afterwards, it flows back 6 hours at 80 DEG C, carbon black is taken out, after 130 DEG C of drying in oven, grinding.
7 parts of constitution controller (hydroxymethyl phenyl silicone oil)
2. raw material described in step (1) is kneaded on a mill at normal temperature；In mixing process, peroxidating two
Isopropylbenzene and the superconduction carbon black of processing need point 6 steps to be added, and keep being kneaded uniform.
3. squeezing out one section of condition of vulcanization: extruder fuselage and head temperature are respectively 39 and 48 DEG C；12 meters long heat cure pipe
Road is divided into three sections, and technological temperature is 190 DEG C of preheating section, 210 DEG C of warming-up section, 250 DEG C of constant temperature zone.Pipeline tape speed is
0.6m/min.Extruded velocity and pipeline speeds match.
Post vulcanization carries out in baking oven: for room temperature to 150 DEG C, the heating-up time is 1 hour；150 DEG C to 200 DEG C, heating 1 is small
When；200 DEG C of 6 hours of processing.
Embodiment 4:
A kind of preparation method of the carbon black filled conductive shield silicon rubber of extrusion type of the present invention comprising following step
It is rapid:
1. preparing the following raw material (being mass parts)
100 parts of methyl vinyl silicone rubber (trade mark is middle indigo plant morning twilight 110-2)；
10 parts of vulcanizing agent (cumyl peroxide)；
18 parts of superconduction carbon black (EC-600JD of coupling agent KH560 processing)
Processing method are as follows: by mass parts coupling agent KH560: superconduction carbon black EC-600JD=1:6 is mixed, and is added appropriate
Ethyl alcohol flows back 5 hours at 80 DEG C after mixing evenly, carbon black is taken out, after 125 DEG C of drying in oven, grinding.
7 parts of constitution controller (hydroxymethyl phenyl silicone oil)
2. raw material described in step (1) is kneaded on a mill at normal temperature；In mixing process, peroxidating two
Isopropylbenzene and the superconduction carbon black of processing need point 4 steps to be added, and keep being kneaded uniform.
3. squeezing out one section of condition of vulcanization: extruder fuselage and head temperature are respectively 44 and 50 DEG C；10 meters of heat cure pipelines
It is divided into three sections, technological temperature is 185 DEG C of preheating section, 220 DEG C of warming-up section, 260 DEG C of constant temperature zone.Pipeline tape speed is 0.9m/
min.Extruded velocity and pipeline speeds match.
Post vulcanization carries out in baking oven: for room temperature to 150 DEG C, the heating-up time is 1 hour；150 DEG C to 200 DEG C, heating 1 is small
When；200 DEG C of 4 hours of processing.
Embodiment 5:
A kind of preparation method of the carbon black filled conductive shield silicon rubber of extrusion type of the present invention comprising following step
It is rapid:
1. preparing the following raw material (being mass parts)
100 parts of methyl vinyl phenyl silicon rubber (trade mark is Shanghai Resin Factory 120-1)；
9 parts of vulcanizing agent (cumyl peroxide)；
30 parts of superconduction carbon black (the magnificent light carbon black of coupling agent A171 processing)
Processing method are as follows: by mass parts A151: magnificent light carbon black=1:7 is mixed, and ethanol in proper amount is added, stirs evenly
Afterwards, it flows back 6 hours at 80 DEG C, carbon black is taken out, after 135 DEG C of drying in oven, grinding.
6 parts of constitution controller (methylol silicone oil)
2. raw material described in step (1) is kneaded on a mill at normal temperature；In mixing process, peroxidating two
Isopropylbenzene and the superconduction carbon black of processing need point 4 steps to be added, and keep being kneaded uniform.
3. squeezing out one section of condition of vulcanization: extruder fuselage and head temperature are respectively 32 and 43 DEG C；10 meters long heat cure pipe
Road is divided into three sections, and technological temperature is 200 DEG C of preheating section, 220 DEG C of warming-up section, 240 DEG C of constant temperature zone.Pipeline tape speed is
0.9m/min.Extruded velocity and pipeline speeds match.
Post vulcanization carries out in baking oven: for room temperature to 150 DEG C, the heating-up time is 1 hour；150 DEG C to 200 DEG C, heating 1 is small
When；200 DEG C of 4 hours of processing.
Implement comparative example 1:
Since vulcanizing agent has used more than common cooperation dosage in the present invention, it is thus possible to will cause the old in advance of sizing material
Change, leads to performance degradation.Therefore rubber mass compounding is carried out using the vulcanizing agent of routine dose in the present invention, it is prepared for comparison and implements
The conductive shield silastic material of example comprising following steps:
1. preparing the following raw material (being mass parts)
100 parts of methyl vinyl silicone rubber (trade mark is middle indigo plant morning twilight 110-2)；
3 parts of vulcanizing agent cumyl peroxide；
15 parts of superconduction carbon black (Aksu EC-600JD of coupling agent KH550 processing)
Processing method are as follows: after being cooperated by mass parts KH550:EC-600JD=1:8 and ethanol in proper amount mixing, stirring are equal
It flows back 4 hours after even at 80 DEG C, carbon black is taken out, after 120 DEG C of drying in oven.
2. raw material described in step (1) is kneaded on a mill at normal temperature；In mixing process, peroxidating
Diisopropylbenzene (DIPB) and the superconduction carbon black of processing need substep to be added, and keep being kneaded uniform.
3. 160 DEG C of conditions of vulcanization of molding vulcanizes 20 minutes.Post vulcanization condition is room temperature to 150 DEG C, the heating-up time 1
Hour；It 150 DEG C to 200 DEG C, heats up 1 hour；200 DEG C of 4 hours of processing.
For the ease of comparison, Examples 1 to 5 and the Silicone Rubber for implementing counter-example are listed in Table 1.It is squeezed out to show
Type silicon rubber has good ageing-resistant performance, carries out accelerated aging test in 30 days at 110 DEG C.With compression set
It can change and be used as evaluation index.The compression set performance column of embodiment 1 and comparative example 1 under the conditions of 30% compression ratio
In table 2.By table as it can be seen that conductive shield silicon rubber of the invention can't reduce aging because excess curative is added
Energy.Table 3 is volume resistivity situation of change of the embodiment 1 at 110 DEG C in 30 days.During accelerated ageing, volume resistance
Rate does not change substantially.
Table 1
Note: hardness refers to GB531 in test method, tensile property test referring to GB528, compression set according to
GB7759, volume resistivity are carried out according to GB2439, electromagnet shield effect according to GJB6190.
Table 2
Table 3
Unspecified part of the present invention belongs to common sense well known to those skilled in the art.
Claims (7)
1. the carbon black filled conductive shield silicon rubber preparation method of extrusion type of ageing-resistant high rebound, it is characterised in that including walking as follows
It is rapid:
(1) prepare the raw material of following mass parts
The vulcanizing agent is cumyl peroxide；
(2) raw material described in step (1) are kneaded on open mill or kneader at normal temperature:
(3) glue stuff compounding obtained by step (2) is vulcanized, is divided to two sections:
Glue stuff compounding is squeezed out according to the extruder shape of the mouth as one speaks, and normal pressure carries out in continuous conduit hot-air cure device；Extruder
Body and head temperature are no more than 50 DEG C, and the conveyor belt speed of extruded velocity and pipeline in vulcanization plant matches, continuous to be formed
Production；Pipeline in vulcanization plant is usually three sections of temperature controls, and every segment length is not less than 2m, and successively temperature range is respectively preheating section
180~200 DEG C of temperature, 200~220 DEG C of warming-up section, constant temperature vulcanize 240~260 DEG C of section, in pipeline conveyor belt speed be 0.1~
2m/min；
Post-processing carries out in baking oven: for room temperature to 150 DEG C, the heating-up time is 1 hour；It 150 DEG C~200 DEG C, heats up 1 hour；200
DEG C processing 4~6 hours.
2. the carbon black filled conductive shield silicon rubber preparation method of extrusion type of ageing-resistant high rebound according to claim 1,
It is characterized by: the silicon rubber is the one or two of methyl vinyl silicone rubber or methyl vinyl phenyl silicon rubber.
3. the carbon black filled conductive shield silicon rubber preparation method of extrusion type of ageing-resistant high rebound according to claim 1,
It is characterized by: superconduction carbon black is magnificent photoconductive carbon black, the BP2000 of Cabot Co., Ltd, the one of the EC-600JD of Aksu company
Kind is several；Coupling agent be amino silicane coupling agent KH550, KH560 and KH570 and vinyl silicane coupling agent A151 and
The one or more of A171.
4. the carbon black filled conductive shield silicon rubber preparation method of extrusion type of ageing-resistant high rebound according to claim 3,
It is characterized by: according to mass ratio (5~10): 1 ratio is added in ethyl alcohol, at 80 DEG C by above-mentioned superconduction carbon black and coupling agent
Lower reflux 4~10 hours, takes out after cooling, 120 DEG C or more at a temperature of dry, grind after to get arriving coupling agent treatment
Superconduction carbon black.
5. the carbon black filled conductive shield silicon rubber preparation method of extrusion type of ageing-resistant high rebound according to claim 1,
It is characterized by: the constitution controller be methylol silicone oil, hydroxymethyl phenyl silicone oil or multi-vinyl silicone oil one kind or
It is several.
6. the carbon black filled conductive shield silicon rubber preparation method of extrusion type of ageing-resistant high rebound according to claim 1,
It is characterized by:, in order to improve dispersibility, superconduction carbon black and vulcanizing agent are both needed to substep and are added in step (2) mixing process.
7. the carbon black filled conductive shield silicon rubber preparation method of extrusion type of ageing-resistant high rebound according to claim 1,
It is characterized by: step (3) adds infra red heating device before preheating section, to sizing material fast shaping.
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| CN108841181A (en) * | 2018-07-18 | 2018-11-20 | 合肥梵腾环保科技有限公司 | A kind of conductive shield silicon rubber and preparation method thereof |
| CN109486193B (en) * | 2018-09-29 | 2021-10-01 | 航天材料及工艺研究所 | Extrusion type silicone rubber system and preparation method and application thereof |
| CN110591373A (en) * | 2019-08-22 | 2019-12-20 | 四川塔牌电缆绕组线有限责任公司 | Fireproof flame-retardant cable and manufacturing method thereof |
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