CN109971044A - A kind of electromagnetic shielding preparation method of composite conductive rubber - Google Patents
A kind of electromagnetic shielding preparation method of composite conductive rubber Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of electromagnetic shielding composite conductive rubber, belong to technical field of function materials.Copper nitrate solution is then added dropwise in sisal fiber, biogas slurry, sucrose, water mixed fermentation by the present invention, and ammonium hydroxide is then added dropwise and adjusts pH, is stirred, filters, freezes, crushes, dry, and high temperature carbonization cools down to get modified filler；By wood powder, secondary settling tank sludge, carbomer, water mixed fermentation, then dropwise addition ammonium hydroxide adjusts pH, and Frozen-thawed cycled filters, and washs, dry, carbonizes, obtains modified auxiliary material；Natural rubber is mixed with butadiene rubber, and butadiene-styrene rubber and epoxy resin is added, is kneaded, blend glue stuff is obtained, by blend glue stuff, modified filler and low-melting alloy mixing, and stearic acid is added, curing agent, modified auxiliary material, vulcanizing agent and promotor, mixed milling, blank is obtained, blank is vulcanized, electromagnetic shielding composite conductive rubber is obtained.The electromagnetic shielding of technical solution of the present invention preparation has the characteristics that excellent electric conductivity with composite conductive rubber.
Description
Technical field
The invention discloses a kind of preparation methods of electromagnetic shielding composite conductive rubber, belong to functional material technology neck
Domain.
Background technique
With the fast development in electronic information epoch, more and more electronic products and equipment have come into the daily life of people
It is living.While improving people's living standard, electronic product and equipment are also inevitably brought largely because of electromagnetic leakage
Electromagnetic pollution.Electromagnetic leakage will lead to electromagnetic interference, electromagnetic information is divulged a secret and electromagnetic environmental pollution, to the mankind and other organisms
Health care belt while carry out high risks, also affecting in industry, medical treatment and military field etc. electronic device and equipment just
Often operation, serious person can injure the information security of national military core institution.Electromangnetic spectrum is to utilize conductive material pair
Two spaces region is isolated, to block electromagnetic wave from an area of space to the induction of another area of space and radiation.
In practical applications, using shielding material by electronic device and equipment be easy leakage electromagnetic wave position (such as shell seam crossing,
At hole) it is sealed, it can both prevent the electromagnetic wave outside of electronic device and equipment from revealing in this way, and can also prevent external electromagnetic
The interference of field.Currently, common electromagnetic shielding material has metal material, ferromagnetic material, conductive polymer material and conductive rubber
Composite material.The electromagnet shield effect highest of metal good conductor material, but due to its quality weight, price height and in labyrinth
The application range of disadvantage poor for applicability, metal good conductor material is more narrow.With the development of polymer-based composite, answer
Conductive rubber for being electromagnetically shielded field is widely studied and applied, and is gradually replaced in some specific fields
Metal shield materials.
For existing cushion seal requirement, for the occasion for ensuring electromagnetic wave shielding again, rubber elastomer electromagnetism wave screen
Material is covered with irreplaceable role.It and is exactly to a certain extent to material electrical property to the investigation of composite material shielding properties
The investigation of energy.So should be just placed in the raising to conductivity of composite material first to the shielding properties starting point obtained.
It is only likely to further be adjusted the overall structure of composite material based on good electric conductivity, designing has more
The structural composite material of high shield effectiveness.In consideration of it, using electromagnetic wave shielding composite silica rubber as main study subject, research
The principle of solidification of composite silica rubber, the preparation process of silicon rubber and under different conductive fillers and filling number it is required solid
The optimum amount of agent.The result shows that: it is in certain linear relationship between the dosage and filler number of curing agent, with same side
The optimum amount of curing agent needed for formula obtains N234, HG-CB and Ni powder filled composite type silicon rubber respectively.To composite silica
The electrical conduction mechanism of rubber is classified and summarizes, it is found that above-mentioned model is adapted to its respective conductive filler.Experimental result
Teach that, for carbon black-filled composite silica rubber, with high degree of structuration magnificent light carbon black to be significantly better than in it is super resistance to
Grind carbon black N234.
Conductive rubber is a kind of polymer-based conducing composite material, and matrix is vulcanized rubber, and the filler of matrix is conductive
Grain, and playing electromagnetic shielding action is the conductive particle in conductive rubber.The electric conductivity of conductive particle, magnetic property and its
The electromagnet shield effect arranged evenly that can all influence conductive rubber in the base, while the sulfuration process of conductive rubber
The shield effectiveness of conductive rubber can be produced bigger effect.
And the electric conductivity of traditional electromagnetic shielding composite conductive rubber the problem of can not also further increasing.Therefore, such as
What improves the shortcomings that tradition electromagnetic shielding composite conductive rubber, is that it is promoted and answers to obtain the promotion of more high combination property
For broader field, meet industrial production demand urgent problem to be solved.
Summary of the invention
The present invention solves the technical problem of: it can not for traditional electromagnetic shielding composite conductive rubber electric conductivity
The problem of further increasing provides a kind of preparation method of electromagnetic shielding composite conductive rubber.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of electromagnetic shielding preparation method of composite conductive rubber, specific preparation process is as follows:
(1) according to parts by weight, by 20~30 parts of sisal fibers, 2~3 parts of biogas slurries, 1~2 portion of sucrose, 20~30 parts of water mixing hairs
Ferment, is then added dropwise 0.1~0.2 times of sisal fiber quality of copper nitrate solution, and ammonium hydroxide is then added dropwise and adjusts pH to 8.0~8.3, stirs
Mixing is mixed, is filtered, is freezed, is crushed, dry, high temperature carbonization cools down to get modified filler；
(2) according to parts by weight, by 20~30 parts of wood powders, 2~3 parts of secondary settling tank sludge, 3~5 parts of carbomers, 20~30 parts of water are mixed
Fermentation is closed, ammonium hydroxide is then added dropwise and adjusts pH to 8.1~8.3, Frozen-thawed cycled 5~8 times, filters, washs, dry, charing obtains modification
Auxiliary material；
(3) according to parts by weight, 60~80 parts of natural rubbers, 20~30 parts of butadiene rubbers, 10~20 parts of butylbenzene rubbers are successively weighed
Glue, 2~3 parts of vulcanizing agents, 50~60 parts of modified fillers, 1~2 part of promotor, 3~5 parts of stearic acid, 30~40 parts of epoxy resin, 3
~5 parts of curing agent, 10~20 parts of modified auxiliary materials, 8~10 parts of low-melting alloys, 1~2 part of silane coupling agent, 1~2 part of phosphatide, 1
Natural rubber is mixed with butadiene rubber, and butadiene-styrene rubber and epoxy resin is added by~2 parts of pitches, is kneaded, is obtained blend glue stuff,
By blend glue stuff, modified filler, low-melting alloy, silane coupling agent, phosphatide, pitch mixing, and stearic acid is added, curing agent,
Modified auxiliary material, vulcanizing agent and promotor, mixed milling obtain blank, blank are vulcanized, and obtain electromagnetic shielding composite conductive rubber.
Step (2) the carbomer carbomer 934, any one in Carbopol 941 or Acritamer 940.
Step (3) vulcanizing agent is sulphur, any one in sulfur monochloride or benzoyl peroxide.
Step (3) promotor is Vulcanization accelerator TMTD, any one in captax or promotor ZDMC.
Step (3) epoxy resin is any one in epoxy resin E51, epoxy resin E44 or epoxy resin E20.
Step (3) curing agent is dihexyl triamine, any one in diethylaminopropylamine or triethylene tetramine.
Step (3) low-melting alloy is bismuth tin alloy, each component mass content in bismuth tin alloy are as follows: bismuth accounts for 51%
(ω), tin account for 30%(ω), lead accounts for 8%(ω), indium accounts for 11%(ω).
Step (3) silane coupling agent is silane resin acceptor kh-550, silane coupling agent KH-560 or silane coupling agent
Any one in KH-570.
Step (3) phosphatide is milk phosphatide, any one in peanut phosphatide or yolk phospholipid.
Step (3) pitch is coal tar pitch, any one in asphalt or bitumen.
The beneficial effects of the present invention are:
(1) present invention passes through addition modified filler and low-melting alloy, firstly, in modified filler preparation process, by sisal hemp fibre
Dimension, biogas slurry, sucrose, water mixed fermentation decompose part organic matter in sisal fiber using bacteriogenic enzyme, so that sisal fiber
Internal permeance property gets a promotion, and since bacterium surface cell is negatively charged, can be enriched with positively charged copper ion, together
When, since the permeance property of sisal fiber is improved, enables more copper ions by Enrichment of bacteria, ammonium hydroxide is then added dropwise
So that copper ion precipitates, then by freezing, so that fibrous inside forms ice crystal, using ball milling, so that the ice of fibrous inside
Crystalline substance, which is under pressure, to be acted on and ruptures, so that fiber splits into the fibrous crystal palpus of micro/nano level, then, and under the high temperature conditions, system
In organic matter charing, while its internal Kocide SD deposited precipitates dehydration, generates copper oxide precipitating, with system temperature by
Edge up height, and the carbonaceous in system is reacted with copper oxide, so that copper oxide restores again, secondly, during the preparation process, it is low in system
Melting alloy melted by heat, alloy after fusing can be inside partial penetration to modified filler, and is dispersed in around elemental copper,
After alloy graining, so that metallurgical bonding is formed between filler, so that the interface resistance between filler reduces, to further improve production
The electric conductivity of product；
(2) present invention is by adding modified auxiliary material and low-melting alloy, in modified auxiliary material preparation process, by wood powder, secondary settling tank
Sludge, carbomer, water mixed fermentation, in the process, the enzyme that the microorganism in biogas slurry generates are decomposed the organic matter in wood powder, are made
The permeance property for obtaining wood powder gets a promotion, and is conducive to carbomer and penetrates into system, then adjusts pH, ammonium hydroxide by the way that ammonium hydroxide is added dropwise
It can be reacted with carbomer, so that the carboxylic ions on carbomer strand, since like charges are mutually exclusive, carbomer point
Fermentation mixed liquor is then passed through Frozen-thawed cycled, largely so that the gap inside wood powder is further widened by subchain disperse stretching, extension
Water enters in wood powder, increases into the water in wood powder by cryocoagulation volume, then melts volume and reduce, by multiple jelly
Melt circulation, so that the gap inside wood powder is gradually increased, is then passed through charing so that generating a large amount of tar in wood powder, is heating
In solidification process, tar can low-melting alloy in enrichment system, low-melting alloy melted by heat, the low melting point after fusing closes
Gold can be fully penetrated into being modified inside auxiliary material, after system cooled and solidified, so that forming metallurgical bonding between modified auxiliary material, reduces
Interface resistance between modified filler, so that the electric conductivity of system is further promoted.
Specific embodiment
According to parts by weight, by 20~30 parts of sisal fibers, 2~3 parts of biogas slurries, 1~2 portion of sucrose, 20~30 parts of water are placed in 1
In number fermentation cauldron, it is 30~35 DEG C in temperature, under the conditions of revolving speed is 100~200r/min, is stirred fermentation 3~5 days, then
The copper nitrate solution that 0.1~0.2 times of mass fraction of sisal fiber quality is 10~20% is added dropwise into No. 1 fermentation cauldron, then to 1
Ammonium hydroxide is added dropwise in number fermentation cauldron and adjusts pH to 8.0~8.3, under the conditions of revolving speed is 400~600r/min, it is stirred 40~
60min obtains mixed serum, then mixed serum is filtered, and obtains filter cake, then filter cake is placed in liquid nitrogen and is freezed, obtain frozen block, connect
Frozen block is placed in ball mill grinding in ball mill, obtain ball milling material, then ball milling material be placed in drying box, in temperature be 105
It is dry to constant weight under the conditions of~110 DEG C, dry ball abrasive material is obtained, then dry ball abrasive material is placed in retort, and with 60~
90mL/min rate is filled with nitrogen into furnace, under the conditions of temperature is 1100~1200 DEG C, after 2~3h of high temperature carbonization, drops with furnace
To room temperature to get modified filler；According to parts by weight, by 20~30 parts of wood powders, 2~3 parts of secondary settling tank sludge, 3~5 parts of card waves
Nurse, 20~30 parts of water are placed in No. 2 fermentation cauldrons, are 30~35 DEG C in temperature, under the conditions of revolving speed is 100~200r/min, are stirred
Mixed fermentation 3~5 day, the ammonium hydroxide that mass fraction is 20~30% is then added dropwise into No. 2 fermentation cauldrons and adjusts pH to 8.1~8.3,
Mixed fermentation liquid obtains pretreated fermentation liquid then by mixed fermentation liquid Frozen-thawed cycled 5~8 times, then by pretreated fermentation liquid mistake
Filter, obtains filter residue, then the filter residue after washing is then placed in residue washing No. 5~8 times in drying box to, Yu Wen with deionized water
It is dry to constant weight under the conditions of degree is 105~110 DEG C, dry filter residue is obtained, then dry filter residue is placed in retort, and with 60
~90mL/min rate is filled with argon gas into furnace, under the conditions of temperature is 650~750 DEG C, carbonizes 2~3h, obtains modified auxiliary material；It presses
Parts by weight meter, successively weighs 60~80 parts of natural rubbers, 20~30 parts of butadiene rubbers, 10~20 parts of butadiene-styrene rubber, and 2~3 parts
Vulcanizing agent, 50~60 parts of modified fillers, 1~2 part of promotor, 3~5 parts of stearic acid, 30~40 parts of epoxy resin, 3~5 parts of solidifications
Agent, 10~20 parts of modified auxiliary materials, 8~10 parts of low-melting alloys, 1~2 part of silane coupling agent, 1~2 part of phosphatide, 1~2 part of pitch,
Natural rubber and butadiene rubber are mixed in kneading machine, and butadiene-styrene rubber and epoxy resin E-44 are added into kneading machine, in
Temperature is kneaded under conditions of being 100~130 DEG C, obtains blend glue stuff, by blend glue stuff, modified filler, low-melting alloy, silane idol
Join agent, phosphatide, and stearic acid is added in pitch mixing, curing agent, modified auxiliary material, vulcanizing agent and promotor, in temperature be 120~
Mixed milling under conditions of 135 DEG C, obtains blank, vulcanizes under conditions of being 170~185 DEG C in temperature by blank, must be electromagnetically shielded
Use composite conductive rubber.The carbomer carbomer 934, any one in Carbopol 941 or Acritamer 940.The vulcanization
Agent is sulphur, any one in sulfur monochloride or benzoyl peroxide.The promotor is Vulcanization accelerator TMTD, captax or rush
Into any one in agent ZDMC.The epoxy resin is any in epoxy resin E51, epoxy resin E44 or epoxy resin E20
It is a kind of.The curing agent is dihexyl triamine, any one in diethylaminopropylamine or triethylene tetramine.The low melting point is closed
Gold is bismuth tin alloy, each component mass content in bismuth tin alloy are as follows: bismuth accounts for 51%(ω), tin accounts for 30%(ω), lead accounts for 8%(ω), indium
Account for 11%(ω).The silane coupling agent is silane resin acceptor kh-550, silane coupling agent KH-560 or Silane coupling reagent KH-570
In any one.The phosphatide is milk phosphatide, any one in peanut phosphatide or yolk phospholipid.The pitch is coal tar
Any one in pitch, asphalt or bitumen.
Example 1
According to parts by weight, by 30 parts of sisal fibers, 3 parts of biogas slurries, 2 portions of sucrose, 30 parts of water are placed in No. 1 fermentation cauldron, Yu Wendu
It is 35 DEG C, under the conditions of revolving speed is 200r/min, is stirred fermentation 5 days, sisal fiber quality is then added dropwise into No. 1 fermentation cauldron
Ammonium hydroxide is then added dropwise into No. 1 fermentation cauldron and adjusts pH to 8.3, is in revolving speed for the copper nitrate solution that 0.2 times of mass fraction is 20%
Under the conditions of 600r/min, it is stirred 60min, mixed serum is obtained, then mixed serum is filtered, obtains filter cake, then set filter cake
It is freezed in liquid nitrogen, obtains frozen block, frozen block is then placed in ball mill grinding in ball mill, obtain ball milling material, then by ball milling material
It is placed in drying box, it is dry to constant weight under the conditions of temperature is 110 DEG C, dry ball abrasive material is obtained, is then placed in dry ball abrasive material
In retort, and nitrogen is filled with into furnace with 90mL/min rate, under the conditions of temperature is 1200 DEG C, after high temperature carbonization 3h, with
Furnace is down to room temperature to get modified filler；According to parts by weight, by 30 parts of wood powders, 3 parts of secondary settling tank sludge, 5 parts of carbomers, 30 parts
Water is placed in No. 2 fermentation cauldrons, is 35 DEG C in temperature, under the conditions of revolving speed is 200r/min, fermentation 5 days is stirred, then to No. 2
The ammonium hydroxide that mass fraction is 30% is added dropwise in fermentation cauldron and adjusts pH to 8.3, mixed fermentation liquid is obtained, then by mixed fermentation liquid freeze thawing
Circulation 8 times, obtains pretreated fermentation liquid, then pretreated fermentation liquid is filtered, obtains filter residue, then with deionized water by residue washing 8
It is secondary, then the filter residue after washing is placed in drying box, under the conditions of temperature is 110 DEG C, drying to constant weight obtains dry filter residue,
Then dry filter residue is placed in retort, and argon gas is filled with into furnace with 90mL/min rate, in temperature be 750 DEG C of conditions
Under, 3h is carbonized, modified auxiliary material is obtained；According to parts by weight, 80 parts of natural rubbers, 30 parts of butadiene rubbers, 120 parts of butylbenzene are successively weighed
Rubber, 3 parts of vulcanizing agents, 60 parts of modified fillers, 2 parts of promotors, 5 parts of stearic acid, 40 parts of epoxy resin, 5 parts of curing agent, 20 parts change
Property auxiliary material, 10 parts of low-melting alloys, 2 parts of silane coupling agents, 2 parts of phosphatide, 2 parts of pitches mix natural rubber with butadiene rubber
In kneading machine, and butadiene-styrene rubber and epoxy resin E-44 are added into kneading machine, are kneaded under conditions of being 130 DEG C in temperature,
Blend glue stuff is obtained, by blend glue stuff, modified filler, low-melting alloy mixing, silane coupling agent, phosphatide, pitch, and tristearin is added
Acid, curing agent, modified auxiliary material, vulcanizing agent and promotor, mixed milling under conditions of being 135 DEG C in temperature, obtain blank, by blank
Vulcanize under conditions of being 185 DEG C in temperature, obtains electromagnetic shielding composite conductive rubber.The carbomer carbomer 934.The sulphur
Agent is sulphur.The promotor is Vulcanization accelerator TMTD.The epoxy resin is epoxy resin E51.The curing agent be two oneself
Base triamine.The low-melting alloy is bismuth tin alloy, each component mass content in bismuth tin alloy are as follows: bismuth accounts for 51%(ω), tin accounts for
30%(ω), lead accounts for 8%(ω), indium accounts for 11%(ω).The silane coupling agent is silane resin acceptor kh-550.The phosphatide is ox
Milk phosphatide.The pitch is coal tar pitch.
Example 2
According to parts by weight, by 30 parts of wood powders, 3 parts of secondary settling tank sludge, 5 parts of carbomers, 30 parts of water are placed in No. 2 fermentation cauldrons, in
Temperature is 35 DEG C, under the conditions of revolving speed is 200r/min, is stirred fermentation 5 days, mass fraction then is added dropwise into No. 2 fermentation cauldrons
PH to 8.3 is adjusted for 30% ammonium hydroxide, mixed fermentation liquid is obtained, then by mixed fermentation liquid Frozen-thawed cycled 8 times, obtains pretreated fermentation
Liquid, then pretreated fermentation liquid is filtered, filter residue is obtained, then with deionized water by residue washing 8 times, then by the filter residue after washing
It is placed in drying box, it is dry to constant weight under the conditions of temperature is 110 DEG C, dry filter residue is obtained, dry filter residue is then placed in charing
In furnace, and argon gas is filled with into furnace with 90mL/min rate, under the conditions of temperature is 750 DEG C, carbonizes 3h, obtain modified auxiliary material；It presses
Parts by weight meter successively weighs 80 parts of natural rubbers, 30 parts of butadiene rubbers, 120 parts of butadiene-styrene rubber, 3 parts of vulcanizing agents, 2 parts of promotions
Agent, 5 parts of stearic acid, 40 parts of epoxy resin, 5 parts of curing agent, 20 parts of modified auxiliary materials, 10 parts of low-melting alloys, 2 parts silane coupled
Natural rubber and butadiene rubber are mixed in kneading machine by agent, 2 parts of phosphatide, 2 parts of pitches, and butylbenzene rubber is added into kneading machine
Glue and epoxy resin E-44 are kneaded under conditions of being 130 DEG C in temperature, obtain blend glue stuff, by blend glue stuff, low-melting alloy,
Silane coupling agent, phosphatide, pitch mixing, and stearic acid is added, curing agent is modified auxiliary material, vulcanizing agent and promotor, is in temperature
Mixed milling under conditions of 135 DEG C, obtains blank, vulcanizes under conditions of being 185 DEG C in temperature by blank, must be electromagnetically shielded with compound
Conductive rubber.The carbomer carbomer 934.The vulcanizing agent is sulphur.The promotor is Vulcanization accelerator TMTD.The epoxy
Resin is epoxy resin E51.The curing agent is dihexyl triamine.The low-melting alloy is bismuth tin alloy, in bismuth tin alloy
Each component mass content are as follows: bismuth accounts for 51%(ω), tin accounts for 30%(ω), lead accounts for 8%(ω), indium accounts for 11%(ω).It is described silane coupled
Agent is silane resin acceptor kh-550.The phosphatide is milk phosphatide.The pitch is coal tar pitch.
Example 3
According to parts by weight, by 30 parts of sisal fibers, 3 parts of biogas slurries, 2 portions of sucrose, 30 parts of water are placed in No. 1 fermentation cauldron, Yu Wendu
It is 35 DEG C, under the conditions of revolving speed is 200r/min, is stirred fermentation 5 days, sisal fiber quality is then added dropwise into No. 1 fermentation cauldron
Ammonium hydroxide is then added dropwise into No. 1 fermentation cauldron and adjusts pH to 8.3, is in revolving speed for the copper nitrate solution that 0.2 times of mass fraction is 20%
Under the conditions of 600r/min, it is stirred 60min, mixed serum is obtained, then mixed serum is filtered, obtains filter cake, then set filter cake
It is freezed in liquid nitrogen, obtains frozen block, frozen block is then placed in ball mill grinding in ball mill, obtain ball milling material, then by ball milling material
It is placed in drying box, it is dry to constant weight under the conditions of temperature is 110 DEG C, dry ball abrasive material is obtained, is then placed in dry ball abrasive material
In retort, and nitrogen is filled with into furnace with 90mL/min rate, under the conditions of temperature is 1200 DEG C, after high temperature carbonization 3h, with
Furnace is down to room temperature to get modified filler；According to parts by weight, 80 parts of natural rubbers are successively weighed, 30 parts of butadiene rubbers, 120 parts
Butadiene-styrene rubber, 3 parts of vulcanizing agents, 60 parts of modified fillers, 2 parts of promotors, 5 parts of stearic acid, 40 parts of epoxy resin, 5 parts of curing agent, 10
Natural rubber and butadiene rubber are mixed in kneading machine by part low-melting alloy, 2 parts of silane coupling agents, 2 parts of phosphatide, 2 parts of pitches
In, and butadiene-styrene rubber and epoxy resin E-44 are added into kneading machine, it is kneaded under conditions of being 130 DEG C in temperature, obtains epoxy glue
Material by blend glue stuff, modified filler, low-melting alloy, silane coupling agent, phosphatide, pitch mixing, and is added stearic acid, solidifies
Agent, vulcanizing agent and promotor, mixed milling under conditions of being 135 DEG C in temperature, obtain blank, by blank in temperature be 185 DEG C
Under the conditions of vulcanize, obtain electromagnetic shielding composite conductive rubber.The vulcanizing agent is sulphur.The promotor is Vulcanization accelerator TMTD.
The epoxy resin is epoxy resin E51.The curing agent is dihexyl triamine.The low-melting alloy is bismuth tin alloy, bismuth
Each component mass content in tin alloy are as follows: bismuth accounts for 51%(ω), tin accounts for 30%(ω), lead accounts for 8%(ω), indium accounts for 11%(ω).It is described
Silane coupling agent is silane resin acceptor kh-550.The phosphatide is milk phosphatide.The pitch is coal tar pitch.
Example 4
According to parts by weight, by 30 parts of sisal fibers, 3 parts of biogas slurries, 2 portions of sucrose, 30 parts of water are placed in No. 1 fermentation cauldron, Yu Wendu
It is 35 DEG C, under the conditions of revolving speed is 200r/min, is stirred fermentation 5 days, sisal fiber quality is then added dropwise into No. 1 fermentation cauldron
Ammonium hydroxide is then added dropwise into No. 1 fermentation cauldron and adjusts pH to 8.3, is in revolving speed for the copper nitrate solution that 0.2 times of mass fraction is 20%
Under the conditions of 600r/min, it is stirred 60min, mixed serum is obtained, then mixed serum is filtered, obtains filter cake, then set filter cake
It is freezed in liquid nitrogen, obtains frozen block, frozen block is then placed in ball mill grinding in ball mill, obtain ball milling material, then by ball milling material
It is placed in drying box, it is dry to constant weight under the conditions of temperature is 110 DEG C, dry ball abrasive material is obtained, is then placed in dry ball abrasive material
In retort, and nitrogen is filled with into furnace with 90mL/min rate, under the conditions of temperature is 1200 DEG C, after high temperature carbonization 3h, with
Furnace is down to room temperature to get modified filler；According to parts by weight, by 30 parts of wood powders, 3 parts of secondary settling tank sludge, 5 parts of carbomers, 30 parts
Water is placed in No. 2 fermentation cauldrons, is 35 DEG C in temperature, under the conditions of revolving speed is 200r/min, fermentation 5 days is stirred, then to No. 2
The ammonium hydroxide that mass fraction is 30% is added dropwise in fermentation cauldron and adjusts pH to 8.3, mixed fermentation liquid is obtained, then by mixed fermentation liquid freeze thawing
Circulation 8 times, obtains pretreated fermentation liquid, then pretreated fermentation liquid is filtered, obtains filter residue, then with deionized water by residue washing 8
It is secondary, then the filter residue after washing is placed in drying box, under the conditions of temperature is 110 DEG C, drying to constant weight obtains dry filter residue,
Then dry filter residue is placed in retort, and argon gas is filled with into furnace with 90mL/min rate, in temperature be 750 DEG C of conditions
Under, 3h is carbonized, modified auxiliary material is obtained；According to parts by weight, 80 parts of natural rubbers, 30 parts of butadiene rubbers, 120 parts of butylbenzene are successively weighed
Rubber, 3 parts of vulcanizing agents, 60 parts of modified fillers, 2 parts of promotors, 5 parts of stearic acid, 40 parts of epoxy resin, 5 parts of curing agent, 20 parts change
Property auxiliary material, 2 parts of silane coupling agents, 2 parts of phosphatide, natural rubber and butadiene rubber be mixed in kneading machine by 2 parts of pitches, and to
Butadiene-styrene rubber and epoxy resin E-44 are added in kneading machine, is kneaded under conditions of being 130 DEG C in temperature, obtains blend glue stuff, will mix
Sizing material, modified filler, silane coupling agent, phosphatide, pitch mixing are closed, and stearic acid is added, curing agent, modified auxiliary material, vulcanizing agent
And promotor, mixed milling under conditions of being 135 DEG C in temperature obtain blank, sulphur under conditions of being 185 DEG C in temperature by blank
Change, obtains electromagnetic shielding composite conductive rubber.The carbomer carbomer 934.The vulcanizing agent is sulphur.The promotor is
Vulcanization accelerator TMTD.The epoxy resin is epoxy resin E51.The curing agent is dihexyl triamine.The silane coupling agent is
Silane resin acceptor kh-550.The phosphatide is milk phosphatide.The pitch is coal tar pitch.
Comparative example: according to parts by weight, successively weighing 80 parts of natural rubbers, 30 parts of butadiene rubbers, 120 parts of butadiene-styrene rubber, and 3
Part vulcanizing agent, 2 parts of promotors, 5 parts of stearic acid, 40 parts of epoxy resin, 5 parts of curing agent, 2 parts of silane coupling agents, 2 parts of phosphatide, 2 parts
Natural rubber and butadiene rubber are mixed in kneading machine by pitch, and butadiene-styrene rubber and epoxy resin E- are added into kneading machine
44, it is kneaded under conditions of being 130 DEG C in temperature, obtains blend glue stuff, by blend glue stuff, silane coupling agent, phosphatide, pitch mixing,
And stearic acid is added, curing agent, vulcanizing agent and promotor, mixed milling under conditions of being 135 DEG C in temperature obtain blank, by base
Expect in temperature be 185 DEG C under conditions of vulcanize, obtain electromagnetic shielding composite conductive rubber.The vulcanizing agent is sulphur.The rush
It is Vulcanization accelerator TMTD into agent.The epoxy resin is epoxy resin E51.The curing agent is dihexyl triamine.The silane is even
Connection agent is silane resin acceptor kh-550.The phosphatide is milk phosphatide.The pitch is coal tar pitch.
Example 1 to 4 resulting electromagnetic shielding composite conductive rubber of example and comparative example product is subjected to performance detection, is had
Body detecting method is as follows:
The electric conductivity of conductive rubber is evaluated by its volume resistivity.Follow GB/T 528-1998 " vulcanized rubber or heat
The measurement of plastic elongation ess-strain performance " in sample size regulation, first to 160 × 160 × 2
mm3Conductive rubber slice cut.Then according to its volume of the resistance calculations of CEPS-002 standard testing conductive rubber
Resistivity, each sample surveys 6 groups of data, and takes maximum value therein as characterization value.
Specific testing result is as shown in table 1:
The 1 specific testing result of electromagnetic shielding composite conductive rubber of table
By 1 testing result of table it is found that the electromagnetic shielding composite conductive rubber of technical solution of the present invention preparation has excellent lead
The characteristics of electrical property, has broad prospects in the development of functional material technology industry.
Claims (10)
1. the preparation method that a kind of electromagnetic shielding uses composite conductive rubber, it is characterised in that specific preparation process is as follows:
(1) according to parts by weight, by 20~30 parts of sisal fibers, 2~3 parts of biogas slurries, 1~2 portion of sucrose, 20~30 parts of water mixing hairs
Ferment, is then added dropwise 0.1~0.2 times of sisal fiber quality of copper nitrate solution, and ammonium hydroxide is then added dropwise and adjusts pH to 8.0~8.3, stirs
Mixing is mixed, is filtered, is freezed, is crushed, dry, high temperature carbonization cools down to get modified filler；
(2) according to parts by weight, by 20~30 parts of wood powders, 2~3 parts of secondary settling tank sludge, 3~5 parts of carbomers, 20~30 parts of water are mixed
Fermentation is closed, ammonium hydroxide is then added dropwise and adjusts pH to 8.1~8.3, Frozen-thawed cycled 5~8 times, filters, washs, dry, charing obtains modification
Auxiliary material；
(3) according to parts by weight, 60~80 parts of natural rubbers, 20~30 parts of butadiene rubbers, 10~20 parts of butylbenzene rubbers are successively weighed
Glue, 2~3 parts of vulcanizing agents, 50~60 parts of modified fillers, 1~2 part of promotor, 3~5 parts of stearic acid, 30~40 parts of epoxy resin, 3
~5 parts of curing agent, 10~20 parts of modified auxiliary materials, 8~10 parts of low-melting alloys, 1~2 part of silane coupling agent, 1~2 part of phosphatide, 1
Natural rubber is mixed with butadiene rubber, and butadiene-styrene rubber and epoxy resin is added by~2 parts of pitches, is kneaded, is obtained blend glue stuff,
By blend glue stuff, modified filler, low-melting alloy, silane coupling agent, phosphatide, pitch mixing, and stearic acid is added, curing agent,
Modified auxiliary material, vulcanizing agent and promotor, mixed milling obtain blank, blank are vulcanized, and obtain electromagnetic shielding composite conductive rubber.
2. a kind of electromagnetic shielding preparation method of composite conductive rubber according to claim 1, it is characterised in that: step
(2) the carbomer carbomer 934, any one in Carbopol 941 or Acritamer 940.
3. a kind of electromagnetic shielding preparation method of composite conductive rubber according to claim 1, it is characterised in that: step
(3) vulcanizing agent is sulphur, any one in sulfur monochloride or benzoyl peroxide.
4. a kind of electromagnetic shielding preparation method of composite conductive rubber according to claim 1, it is characterised in that: step
(3) promotor is Vulcanization accelerator TMTD, any one in captax or promotor ZDMC.
5. a kind of electromagnetic shielding preparation method of composite conductive rubber according to claim 1, it is characterised in that: step
(3) epoxy resin is any one in epoxy resin E51, epoxy resin E44 or epoxy resin E20.
6. a kind of electromagnetic shielding preparation method of composite conductive rubber according to claim 1, it is characterised in that: step
(3) curing agent is dihexyl triamine, any one in diethylaminopropylamine or triethylene tetramine.
7. a kind of electromagnetic shielding preparation method of composite conductive rubber according to claim 1, it is characterised in that: step
(3) low-melting alloy is bismuth tin alloy, each component mass content in bismuth tin alloy are as follows: bismuth accounts for 51%(ω), tin accounts for 30%
(ω), lead account for 8%(ω), indium accounts for 11%(ω).
8. a kind of electromagnetic shielding preparation method of composite conductive rubber according to claim 1, it is characterised in that: step
(3) silane coupling agent is silane resin acceptor kh-550, appointing in silane coupling agent KH-560 or Silane coupling reagent KH-570
It anticipates one kind.
9. a kind of electromagnetic shielding preparation method of composite conductive rubber according to claim 1, it is characterised in that: step
(3) phosphatide is milk phosphatide, any one in peanut phosphatide or yolk phospholipid.
10. a kind of electromagnetic shielding preparation method of composite conductive rubber according to claim 1, it is characterised in that: step
(3) pitch is coal tar pitch, any one in asphalt or bitumen.
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| CN113337231A (en) * | 2021-06-01 | 2021-09-03 | 中国科学院合肥物质科学研究院 | Epoxy composite material with heterostructure and preparation method thereof |
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Application publication date: 20190705 |