CN109021579A - A kind of conductive silicon rubber and preparation method thereof - Google Patents
A kind of conductive silicon rubber and preparation method thereof Download PDFInfo
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- CN109021579A CN109021579A CN201810726695.XA CN201810726695A CN109021579A CN 109021579 A CN109021579 A CN 109021579A CN 201810726695 A CN201810726695 A CN 201810726695A CN 109021579 A CN109021579 A CN 109021579A
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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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
- C08K2201/001—Conductive additives
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Abstract
The invention belongs to silicon rubber technical fields, and in particular to a kind of conductive silicon rubber and preparation method thereof.Magnesia and ferriferrous oxide particles are made by pelletizer after magnesium oxide powder and ferroferric oxide powder are mixed; methyl vinyl silicone rubber and white carbon black are kneaded to obtain basic glue; magnesia and ferriferrous oxide particles are added into basic glue and silane coupling agent is kneaded to obtain rubber compound, obtain conductive silicon rubber after vulcanizing agent vulcanization is added into rubber compound.This hair controls the additional proportion of white carbon black and magnesia and ferroso-ferric oxide, so that conductive silicon rubber is provided simultaneously with preferable electric conductivity and higher mechanical strength.
Description
Technical field
The invention belongs to silicon rubber technical fields, and in particular to a kind of conductive silicon rubber and preparation method thereof.
Background technique
Silicon rubber has excellent heat resistance, low temperature resistant, insulating properties, antidetonation, resistance to compression, wear-resistant and good biology special
Property, it makes it have and is widely applied range, such as building, communications and transportation, electronic apparatus, chemical industry, biomaterial and aviation boat
Its material etc..Conductive high-temperature silicon sulfide rubber is the polysiloxane raw rubber with high molecular weight, is equipped with reinforced filling, structure control
The various additives such as preparation, vulcanizing agent, homogeneous sizing material made of being kneaded in mixing machinery.Because of its excellent high-low temperature resistant, resistance to
The characteristics such as weathering aging, endurance, insulating properties, highly-breathable, resistance to certain solvents and physiological inertia are widely used in space flight, boat
The every field of the national economy and people's lives such as sky, electronics, electrical, machinery, automobile, daily sealing, health care, in national defence
It is also played an important role in military project, high-tech industry.Conductive silicon rubber has good because it has good conductive property
Electromagnetic sealing and water vapor seal ability and the neck such as be widely used in electronics, electric power, telecommunications, military project, Aeronautics and Astronautics, ships
In domain.Current market sales of conductive silicon rubber is most of to be prepared with raw material acetylene carbon black, and disadvantage is exactly
For the health of environmental protection and operator, preparation process is more complex, acetylene carbon black addition in current this conductive silicon rubber
Measure larger, conductive silicon rubber mechanical performance is poor.Traditional conductive silicon rubber exploitation, be by the way that various conductive fillers are added, as
The fillers such as metal powder or conductive black, after additional amount is more than certain proportion, silica gel begins to conduction, in order to realize silicon rubber
White carbon black will be usually added in the reinforcement of glue, and white carbon black is insulator, its addition can reduce the electric conductivity of silicon rubber.Therefore,
The additional amount for controlling white carbon black and conductive agent, guarantees that silicon rubber is provided simultaneously with preferable electric conductivity and mechanical strength, has important
Meaning.
Patent CN103665875A discloses a kind of preparation method of conductive silicon rubber.Acetylene carbon black, aluminum oxide,
After acetylene carbon black and aluminum oxide particle is made in addition pelletizer after hydroxy silicon oil and the water for accounting for acetylene carbon black weight 1% mix
It is kneaded again.Silicon rubber of the present invention has the advantages that high thermal conductivity, heat resistance and low compressibility, and tensile strength is greater than
9.6MPa, tearing strength is in 36N/mm or more, and volume resistivity is less than 45 Ω cm.
Patent CN107141809A discloses a kind of low resistance conductive silicon rubber, each component including following parts by weight, first
Base vinylsiloxane rubber: 100 parts, acetylene carbon black: 25~45 parts, acid powder: 2~6 parts, nano powder: 1~2 part, inner pattern releasing agent applicable:
0.2~0.5 part, silane coupling agent: 0.1~0.5 part, which is reduced to 10 for the sheet resistance of silicon rubber
Ohms, while solving easy roll banding phenomenon.
Patent CN107964247A discloses a kind of preparation method of Conductive high-temperature silicon sulfide rubber, the conductive silicon rubber
Be by polysiloxane, gas-phase silica, carbon nanotube mixture, dimethyl silicone polymer, silane coupling agent, release agent,
Vulcanizing agent composition.The characteristics of invention is to joined new material carbon nanotube mixture, so that the conductive silicon rubber is with good
Good electric conductivity and excellent mechanical performance, and simple production process, it is easy to operate.
Patent CN108003626A discloses a kind of conductive silicon rubber and preparation method thereof, this method comprises: (1) receives carbon
Mitron and graphene are kneaded with silicon rubber and vulcanizing agent, to obtain rubber compound, wherein the carbon nanotube and the stone
At least one of black alkene passes through modification；(2) rubber compound is subjected to vulcanizing treatment, to obtain conductive silicon rubber.
The preparation method after being modified at least one of carbon nanotube and graphene with silicon rubber and vulcanizing agent by answering as a result,
Match, its electric conductivity can be improved while improving silicone rubber mechanical performance, and resulting conductive silicon rubber is with higher scattered
Hot property.
Summary of the invention
The object of the present invention is to provide a kind of conductive silicon rubbers and preparation method thereof.By magnesium oxide powder and ferroso-ferric oxide
Magnesia and ferriferrous oxide particles are made by pelletizer after powder mixing, methyl vinyl silicone rubber and white carbon black are kneaded
Basic glue is obtained, magnesia and ferriferrous oxide particles are added into basic glue and silane coupling agent is kneaded to obtain rubber compound,
Conductive silicon rubber is obtained after vulcanizing agent vulcanization is added into rubber compound.This hair controls white carbon black and magnesia and ferroso-ferric oxide
Additional proportion so that conductive silicon rubber is provided simultaneously with preferable electric conductivity and higher mechanical strength.
The technical solution of the present invention is as follows:
A kind of preparation method of conductive silicon rubber, comprising the following steps:
(1) weight ratio for the magnesium oxide powder and ferroferric oxide powder of 3~5:1~2 and is accounted for into its total weight 0.8%
Deionized water mixing after be added pelletizer magnesia and ferriferrous oxide particles is made；
(2) on the double roll mill by 80~100 parts by weight methyl vinyl silicone rubbers and 65~90 parts by weight white carbon blacks
Keeping temperature is that 5~8min is kneaded at 25 DEG C~29 DEG C, obtains basic glue；
(3) be added into the basic glue of step (2) 23~36 parts by weight magnesia and ferriferrous oxide particles and 1.2~
1.7 parts by weight silane coupling agents are kneaded 25~40min at 25 DEG C~30 DEG C, obtain rubber compound；
(4) into the rubber compound of step (3) be added 2~4 parts by weight vulcanizing agents, at 125 DEG C~165 DEG C vulcanize 2~
6min obtains conductive silicon rubber.
Preferably, above-mentioned silane coupling agent is vinyltriethoxysilane, vinyltrimethoxysilane, vinyl three
One of (beta-methoxy ethyoxyl) silane.
Preferably, above-mentioned vulcanizing agent is 2,4- dichlorobenzoperoxide, 1,1 di-tert-butyl peroxide -3,3,5- front three
Butylcyclohexane, the peroxidating -2- ethyl acid tert-butyl ester, the peroxidating -2- ethylhexyl carbonate tert-butyl ester, 2,5- di-t-butyl peroxide
One of change -2,5- dimethylhexane, cumyl peroxide.
Preferably, above-mentioned white carbon black is fume colloidal silica or precipitated silica.
The conductive silicon rubber that the above method is prepared.
Beneficial effects of the present invention are as follows:
The present invention is made magnesia and four by pelletizer after mixing magnesium oxide powder and ferroferric oxide powder and aoxidizes
Methyl vinyl silicone rubber and white carbon black are kneaded to obtain basic glue by three iron particles, and magnesia and four oxygen are added into basic glue
Change three iron particles and silane coupling agent is kneaded to obtain rubber compound, obtains conductive silicon rubber after vulcanizing agent vulcanization is added into rubber compound
Glue.This hair controls the additional proportion of white carbon black and magnesia and ferroso-ferric oxide, so that conductive silicon rubber is provided simultaneously with preferably
Electric conductivity and higher mechanical strength.
Specific embodiment
With reference to embodiment, technical solution of the present invention is described in further detail, but do not constituted pair
Any restrictions of the invention.
Embodiment 1
A kind of preparation method of conductive silicon rubber, comprising the following steps:
(1) by weight ratio be 3:1 magnesium oxide powder and ferroferric oxide powder and account for its total weight 0.8% go from
Pelletizer is added after sub- water mixing, magnesia and ferriferrous oxide particles is made；
(2) 80 parts by weight methyl vinyl silicone rubbers and 70 parts by weight fume colloidal silicas are kept on the double roll mill
Temperature is to be kneaded 6min at 26 DEG C, obtains basic glue；
(3) 25 parts by weight magnesia and ferriferrous oxide particles and 1.5 parts by weight are added into the basic glue of step (2)
Silane coupling agent vinyl triethoxysilane is kneaded 30min at 28 DEG C, obtains rubber compound；
(4) 4 parts by weight vulcanizing agents 2,4- dichlorobenzoperoxide, at 145 DEG C are added into the rubber compound of step (3)
Vulcanize 5min, obtains conductive silicon rubber.
The conductive silicon rubber tensile strength that the present embodiment is prepared is 11.2MPa, tearing strength 39N/mm, volume electricity
Resistance rate is 44 Ω cm.
Embodiment 2
A kind of preparation method of conductive silicon rubber, comprising the following steps:
(1) by weight ratio be 5:2 magnesium oxide powder and ferroferric oxide powder and account for its total weight 0.8% go from
Pelletizer is added after sub- water mixing, magnesia and ferriferrous oxide particles is made；
(2) 84 parts by weight methyl vinyl silicone rubbers and 68 parts by weight fume colloidal silicas are kept on the double roll mill
Temperature is to be kneaded 5min at 28 DEG C, obtains basic glue；
(3) 29 parts by weight magnesia and ferriferrous oxide particles and 1.6 parts by weight are added into the basic glue of step (2)
Silane coupling agent vinyl trimethoxy silane is kneaded 36min at 28 DEG C, obtains rubber compound；
(4) 2.4 parts by weight vulcanizing agent, 1,1 di-tert-butyl peroxide -3,3,5- front three is added into the rubber compound of step (3)
Butylcyclohexane vulcanizes 3min at 148 DEG C, obtains conductive silicon rubber.
The conductive silicon rubber tensile strength that the present embodiment is prepared is 10.9MPa, tearing strength 41N/mm, volume electricity
Resistance rate is 46 Ω cm.
Embodiment 3
A kind of preparation method of conductive silicon rubber, comprising the following steps:
(1) by weight ratio be 2:1 magnesium oxide powder and ferroferric oxide powder and account for its total weight 0.8% go from
Pelletizer is added after sub- water mixing, magnesia and ferriferrous oxide particles is made；
(2) 97 parts by weight methyl vinyl silicone rubbers and 72 parts by weight precipitated silicas are kept on the double roll mill
Temperature is to be kneaded 8min at 29 DEG C, obtains basic glue；
(3) 32 parts by weight magnesia and ferriferrous oxide particles and 1.4 parts by weight are added into the basic glue of step (2)
Silane coupling agent (beta-methoxy ethyoxyl) silane, is kneaded 36min at 29 DEG C, obtains rubber compound；
(4) the 2.8 parts by weight vulcanizing agent peroxidating -2- ethylhexyl carbonate tert-butyl esters are added into the rubber compound of step (3),
Vulcanize 3min at 138 DEG C, obtains conductive silicon rubber.
The conductive silicon rubber tensile strength that the present embodiment is prepared is 11.9MPa, tearing strength 43N/mm, volume electricity
Resistance rate is 42 Ω cm.
Embodiment 4
A kind of preparation method of conductive silicon rubber, comprising the following steps:
(1) by weight ratio be 4:1 magnesium oxide powder and ferroferric oxide powder and account for its total weight 0.8% go from
Pelletizer is added after sub- water mixing, magnesia and ferriferrous oxide particles is made；
(2) 97 parts by weight methyl vinyl silicone rubbers and 92 parts by weight precipitated silicas are kept on the double roll mill
Temperature is to be kneaded 7min at 29 DEG C, obtains basic glue；
(3) 35 parts by weight magnesia and ferriferrous oxide particles and 1.6 parts by weight are added into the basic glue of step (2)
Silane coupling agent (beta-methoxy ethyoxyl) silane, is kneaded 33min at 30 DEG C, obtains rubber compound；
(4) 3 parts by weight vulcanizing agent 2,5- di-tert-butyl peroxide -2,5- dimethyl are added into the rubber compound of step (3)
Hexane vulcanizes 4.5min at 135 DEG C, obtains conductive silicon rubber.
The conductive silicon rubber tensile strength that the present embodiment is prepared is 12.1MPa, tearing strength 46N/mm, volume electricity
Resistance rate is 40 Ω cm.
Embodiment 5
A kind of preparation method of conductive silicon rubber, comprising the following steps:
(1) by weight ratio be 4:1 magnesium oxide powder and ferroferric oxide powder and account for its total weight 0.8% go from
Pelletizer is added after sub- water mixing, magnesia and ferriferrous oxide particles is made；
(2) 86 parts by weight methyl vinyl silicone rubbers and 92 parts by weight precipitated silicas are kept on the double roll mill
Temperature is to be kneaded 6min at 29 DEG C, obtains basic glue；
(3) 31 parts by weight magnesia and ferriferrous oxide particles and 1.7 parts by weight are added into the basic glue of step (2)
Silane coupling agent vinyl triethoxysilane is kneaded 38min at 30 DEG C, obtains rubber compound；
(4) the 2 parts by weight vulcanizing agent peroxidating -2- ethyl acid tert-butyl esters are added into the rubber compound of step (3), 135
Vulcanize 6min at DEG C, obtains conductive silicon rubber.
The conductive silicon rubber tensile strength that the present embodiment is prepared is 11.5MPa, tearing strength 43.7N/mm, volume
Resistivity is 44 Ω cm.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of conductive silicon rubber, which comprises the following steps:
(1) weight ratio for the magnesium oxide powder and ferroferric oxide powder of 3~5:1~2 and is accounted for into going for its total weight 0.8%
Pelletizer is added after ionized water mixing, magnesia and ferriferrous oxide particles is made；
(2) 80~100 parts by weight methyl vinyl silicone rubbers and 65~90 parts by weight white carbon blacks are kept on the double roll mill
Temperature is that 5~8min is kneaded at 25 DEG C~29 DEG C, obtains basic glue；
(3) 23~36 parts by weight magnesia and ferriferrous oxide particles and 1.2~1.7 are added into the basic glue of step (2)
Parts by weight silane coupling agent is kneaded 25~40min at 25 DEG C~30 DEG C, obtains rubber compound；
(4) 2~4 parts by weight vulcanizing agents are added into the rubber compound of step (3), vulcanizes 2~6min at 125 DEG C~165 DEG C, obtains
To conductive silicon rubber.
2. a kind of preparation method of conductive silicon rubber according to claim 1, which is characterized in that the silane coupling agent is
One of vinyltriethoxysilane, vinyltrimethoxysilane, vinyl three (beta-methoxy ethyoxyl) silane.
3. a kind of preparation method of conductive silicon rubber according to claim 1, which is characterized in that the vulcanizing agent is 2,4-
Dichlorobenzoperoxide, 1,1 di-tert-butyl peroxide -3,3,5- trimethyl-cyclohexanes, the tertiary fourth of peroxidating -2- ethyl acid
Ester, the peroxidating -2- ethylhexyl carbonate tert-butyl ester, 2,5- di-tert-butyl peroxide -2,5- dimethylhexane, peroxidating diisopropyl
One of benzene.
4. a kind of preparation method of conductive silicon rubber according to claim 1, which is characterized in that the white carbon black is gas phase
Method white carbon black or precipitated silica.
5. the conductive silicon rubber that any preparation method is prepared described in Claims 1-4.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005320462A (en) * | 2004-05-11 | 2005-11-17 | Shin Etsu Chem Co Ltd | Addition reaction-curable silicone rubber composition for heat-resistant applications and silicone adhesive |
| CN103665875A (en) * | 2013-11-29 | 2014-03-26 | 山东永泰化工有限公司 | Preparation method of electroconductive silicone rubber |
| CN104098795A (en) * | 2013-04-12 | 2014-10-15 | 中国石油化工股份有限公司 | Conductive thermoplastic elastomer and preparation method thereof |
| CN104725872A (en) * | 2014-12-17 | 2015-06-24 | 苏州锦腾电子科技有限公司 | Abrasion-resistance conductive silicon rubber and preparation method thereof |
-
2018
- 2018-07-04 CN CN201810726695.XA patent/CN109021579A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005320462A (en) * | 2004-05-11 | 2005-11-17 | Shin Etsu Chem Co Ltd | Addition reaction-curable silicone rubber composition for heat-resistant applications and silicone adhesive |
| CN104098795A (en) * | 2013-04-12 | 2014-10-15 | 中国石油化工股份有限公司 | Conductive thermoplastic elastomer and preparation method thereof |
| CN103665875A (en) * | 2013-11-29 | 2014-03-26 | 山东永泰化工有限公司 | Preparation method of electroconductive silicone rubber |
| CN104725872A (en) * | 2014-12-17 | 2015-06-24 | 苏州锦腾电子科技有限公司 | Abrasion-resistance conductive silicon rubber and preparation method thereof |
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