CN110041554A - A kind of preparation method of conductive seal agent - Google Patents
A kind of preparation method of conductive seal agent Download PDFInfo
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- CN110041554A CN110041554A CN201910362120.9A CN201910362120A CN110041554A CN 110041554 A CN110041554 A CN 110041554A CN 201910362120 A CN201910362120 A CN 201910362120A CN 110041554 A CN110041554 A CN 110041554A
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- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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Abstract
The invention belongs to technical field of material, and in particular to a kind of preparation method of conductive seal agent.Nano graphite flakes are during acrylonitrile and butadiene copolymer form nitrile rubber in the present invention, since there are active reaction points in nano-graphite lamella, the cross-linking reaction of rubber can be caused, greatly reduce the mobility of nitrile rubber segment, the nitrile rubber of high conductivity can check the influence of electromagnetic field of high frequency in the interlayer filling of conductive seal agent, so that interference field is formed vortex inside conductive seal agent and generates reflection on conductive seal agent surface, reach shield effectiveness, and the high copper powder of magnetic conductivity is added, improves effectiveness；It is squeezed out to obtain starch fillers with extruder after sweet potato flour, glycerol and water are mixed high speed dispersion, improve the adhesion strength of sealant, the low temperature flexibility of soybean protein lotion is preferable simultaneously, can have preferable sealing performance at low ambient temperatures, enhance conductive seal agent elasticity and toughness, has broad application prospects.
Description
Technical field
The invention belongs to technical field of material, and in particular to a kind of preparation method of conductive seal agent.
Background technique
Polysulfide sealant is because of its good processing performance, excellent oil resistivity, water resistance, low air penetrability, weatherability, resistance toization
Medium is good, and shock resistance, anti-vibration have good adhesive property to metal, nonmetallic etc., in Aeronautics and Astronautics, ship, build
It builds, the industries such as automobile, electronic apparatus are widely applied.The density size of sealant influences aircraft entirety in aircraft industry
Weight, and then its cruising ability is had an impact, even the loss of weight in aircraft industry in terms of g is all meaningful, simultaneously
Sealant uses temperature requirement also higher than conventional sealant.
Polysulfide sealant is that filler and auxiliary agent appropriate is added, passes through metal oxide using liquid polysulfide rubber as host agent
And the multicomponent sealing material of peroxide cure.With the development of technology and the requirement of application environment is higher, in addition to intrinsic
Other functions of sealing performance, polysulfide sealant also constantly enhance.But reinforced filling used in existing polysulfide sealant and
The density of curing agent is higher, and the sealant density after leading to vulcanization is generally in 1.5g/cm3 or more；Simultaneously because polysulfide itself
Structure is thermo-labile, and thermal degradation occurs at high temperature for the bonding site not contacted with air, be in thick fluid, cause bonding and it is close
Envelope failure.Existing sealant performance is also undesirable in terms of low-density and resistance to thermal degradation.
Conductive seal agent conduct has both conduction and quickly grows with sealing binding function polymer composite, and research achievement is wide
It is general to be used to eliminate electrostatic, electromagnetic shielding and other various electric power application fields.Currently, the report in relation to conductive seal agent is mostly to have
Machine silicon rubber is that matrix is studied, but due to the defect of organic silicon rubber itself, is limited its scope of application, especially existed
Organosilicon is easily swollen in resistance to oil environment, is unable to satisfy requirement.
Polysulfide sealant is and to be equipped with filler auxiliary agent appropriate using liquid polysulfide rubber as main base, passes through metal oxygen
The multicomponent sealing material of compound and peroxide cure.Due to its good water resistance, low-permeable, weatherability, chemically-resistant
Medium is good, shock resistance, anti-vibration, and has good adhesive property to metal, nonmetallic etc., in aerospace, electronics electricity
The industries such as device are widely applied.But liquid polysulfide rubber is due to its molecule feature, poor with common conductive metal powder compatibility, because
This, conductive seal agent resistivity obtained is high or even is not available.
Silicon rubber is that main chain is alternately arranged by silicon and oxygen atom, and the rubber there are two organic group is usually connected on silicon atom.
Silicon rubber has excellent high-low temperature resistant (- 60 DEG C~260 DEG C) performance, and special silicon rubber uses temperature up to 300 DEG C or more,
Simultaneously there is excellent weatherability, physiological inertia, electrical insulation capability and gas permeability etc., aerospace, electronics, medical instrument with
The every field such as automobile are all applied widely, and played an important role in national economy.
Silicon rubber can be divided into condensed type and add-on type by reaction type, can be divided into one-component and bi-component by manner of formulation,
Temperature when by reaction can be divided into room temperature vulcanized and high temperature vulcanized type again.Single-component room temperature vulcanized type silicon rubber is due to packaging letter
Single, the easy to use and very wide advantage of application range, has been widely used, but the oil resistant of silicon rubber in sealant field
Property, solvent resistance etc. are poor.It is used to meet silicon rubber in the occasion that engine, gear-box etc. are contacted with oil, it is necessary to try
Improve the oil resistance of silicon rubber.There are mainly two types of modes for the oil resistance of raising silicon rubber at present: first is that in point of silicon rubber
Introduced in subchain fluorine-containing group (such as trifluoro propyl), but this method higher cost, can only the demands such as aerospace compared with
Few field uses, it is difficult to widely apply in the industry；Second is that the filler of various oil resistivitys is added in formula to improve silicon rubber
The oil resistance of glue sealant, second method is relatively easy, economical, is currently used main method.
Sealant exists at present: the problems such as volume resistivity is higher, effectiveness is poor, sticky general.
Therefore, inventing the excellent sealant of one kind has positive effect to field of material technology.
Summary of the invention
Present invention mainly solves the technical issues of, electromagnetic screen higher for the general volume resistivity of current sealant material
It is poor to cover effect, viscoplasticity declines after sealant adds conductive filler, can reduce sealant and be bonded and sealed the defect of effect, mention
A kind of preparation method of conductive seal agent is supplied.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of conductive seal agent, it is characterised in that specific preparation step are as follows:
Starch fillers, soybean protein lotion, polyurethane foam, lactic acid bacteria powder are placed in sealed fermenter, controlled at 40
~50 DEG C, 3~5 days are stood, the filtering removal isolated fermentation filter residue of filtrate mixes fermentation filter residue, copper powder, mixing rubber material
Conjunction is transferred in foaming machine pressurization of foaming, and to the ammonium hydroxide that azodicarbonamide is added in foaming machine, mass fraction is 20%, discharges
After be cut into particle and obtain conductive seal agent；
The specific preparation step of the mixing rubber material are as follows:
(1) acrylonitrile and butadiene is added in three-necked flask, the sodium hydroxide that mass fraction is 5% is added into three-necked flask
Solution, polyvinyl alcohol, the nano graphite flakes water slurry that mass fraction is 40%, start blender, with 80~90r/min revolving speed
After 10~15min of stirring and emulsifying, potassium peroxydisulfate is added, is heated to 45~48 DEG C, 3~4h of insulation reaction obtains conductive fourth
Nitrile rubber；
(2) 40~45g acrylic acid and copolymer-maleic anhydride are added equipped with 100~120mL mass fraction is 30~40% acetone
In the beaker of solution, 80~85 DEG C are heated to, 60~70g bentonite is added to beaker, is cooled to room temperature and obtains bentonite
Bentonite suspension is placed in supercentrifuge by suspension, is centrifuged 15~17min with the revolving speed of 3100~3800r/min, is gone
Except upper liquid, lamella bentonite is obtained, lamella bentonite is placed in baking oven, is heated to 80~90 DEG C, dry 3~4h,
Obtain modified alta-mud；
(3) Conductive NBR is placed in double roll mill, is plasticated 2~3 times, then conductive butyronitrile is added into double roll mill
Modified alta-mud, the 20~25g white carbon black of rubber quality 5~8%, mixing are plasticated 2~3 times, are discharged, are obtained mixing rubber material；
The specific preparation step of the mixing rubber material are as follows:
(1) 4 ︰ 1 of sweet potato flour, glycerol and water 7 ︰ in mass ratio is mixed, is placed in high speed disperser with 3000~3500r/min's
Revolving speed disperses 10~15min and obtains starch fillers, pours into double screw extruder, and extrusion obtains starch fillers；
(2) 200~220mL distilled water is added into the four-hole boiling flask with blender, reflux condenser, is with mass fraction
40% sodium hydroxide solution adjusts pH, is heated to 90~100 DEG C to four-hole boiling flask, and 60~70g soy meal, heat preservation is added
After handling 50~55min, 10~12g phenol is added into four-hole boiling flask, is cooled to 70~75 DEG C, 15~20min of isothermal holding,
Continue that 20~25mL formaldehyde is added into four-hole boiling flask, react 1~2h, cooled to room temperature obtains soybean protein lotion.
According to parts by weight, 10~15 parts of starch fillers, 10~18 parts of soybean protein lotions, 20~35 parts of polyurethane foams
Foam, 5~10 parts of lactic acid bacteria powders, 70~80 parts of fermentation filter residues, 40~50 parts of copper powders, 30~35 parts of mixing rubber material, 8~10 parts of idols
The ammonium hydroxide that nitrogen diformamide, 50~60 parts of mass fractions are 20%.
The temperature that foaming machine is controlled in foaming process is 150 DEG C~180 DEG C, and blow pressure is 4~5MPa.
Each raw material of Conductive NBR is prepared in the specific preparation step (1) of the mixing rubber material, in parts by weight
Meter, including 80~90 parts of acrylonitrile, 90~110 parts of butadiene, the sodium hydroxide solution that 100~120 parts of mass fractions are 5%, 30
Nano graphite flakes water slurry, 1~3 part of potassium peroxydisulfate of~40 parts of polyvinyl alcohol, 100~120 parts of mass fractions for 40%.
Acrylic acid used in the specific preparation step (2) of the mixing rubber material and the preferred horse of copolymer-maleic anhydride
Carry out 3 ︰ 1 of mass ratio of acid anhydrides and acrylic acid.
Plasticating in the specific preparation step (3) of the mixing rubber material and shortening the preceding roll temperature of middle double roll mill into is 45
~55 DEG C, rear roll temperature is 40~50 DEG C, and roll spacing is 8~10mm.
Sweet potato flour, 7 ︰ of glycerol and water mixing mass ratio, 4 ︰ 1 in the specific preparation step (1) of the mixing rubber material.
The ginseng of double screw extruder when extrusion prepares starch fillers in the specific preparation step (1) of the mixing rubber material
Number are as follows: head temperature is 230~250 DEG C, and screw speed is 160~180r/min, and feed rate is 50~75g/min.
Sodium hydroxide solution adjusts flask before heat temperature raising is handled in the specific preparation step (2) of the mixing rubber material
Middle reaction system pH is 9~10.
The beneficial effects of the present invention are:
(1) nano graphite flakes are during acrylonitrile and butadiene copolymer form nitrile rubber in the present invention, due to nano-graphite
There are active reaction point in lamella, the cross-linking reaction of rubber can be caused, under emulsion blending, graphite flake layer reaches in rubber matrix
Nano-dispersed is arrived, while there are also certain intercalation configurations to exist, potential active site and rubber molecule on nano-graphite lamella
It has occurred and adequately contacts and autovulcanization thus has occurred, cause nano-graphite lamella fully dispersed in rubber, and can break
The insulation crystalline region of bad rubber forms conductive network, improves nitrile rubber electric conductivity, due to the fine dispersion and stone of nano-graphite
Polar functional group on ink sheet layer and the polar interaction between the group of rubber, cause interface strong between graphite and matrix
In conjunction with, greatly reduce the mobility of nitrile rubber segment, plasticate during be added modified alta-mud can be intercalation into rubber
In, biggish hysteresis loss can be generated in stress, improve the resilience performance of conductive seal agent, the nitrile rubber of high conductivity
The influence of electromagnetic field of high frequency can be checked in the interlayer filling of conductive seal agent, interference field is made to form whirlpool inside conductive seal agent
It flows and generates reflection on conductive seal agent surface, weaken influence of the interference field to elaxtic seal, reach shield effectiveness, and
The high copper powder of magnetic conductivity is added, increases eddy current effect, improves effectiveness；
(2) it is squeezed out to obtain starch fillers with extruder after sweet potato flour, glycerol and water being mixed high speed dispersion, be matched by raw material of paper pulp
Mixed powder is made, finally by the fermenting raw materials such as starch fillers, soybean protein lotion, lactic acid bacteria powder, isolated fermentation filter
Fermentation filter residue, copper powder, mixing rubber material mixed foaming are obtained conductive seal agent by slag, and prepared soybean protein lotion can be with
Polyurethane foam further occurrence cross-linking reaction improves the adhesion strength of sealant, while the low temperature of soybean protein lotion is soft
Toughness is preferable, can have preferable sealing performance at low ambient temperatures, during the fermentation, the grape decomposed by starch fillers
Sugar ferments in foamed polyurethane hole and rubber layer generates lactic acid, and lactic acid polymerize between hole generates polylactic acid, prepared
The stronger polylactic acid of toughness and paper fiber are filled in conductive seal agent, enhances conductive seal agent elasticity and toughness, are had wide
Wealthy application prospect.
Specific embodiment
According to parts by weight, 80~90 parts of acrylonitrile and 90~110 parts of butadiene are added in three-necked flask, are burnt to three mouthfuls
Sodium hydroxide solution, 30~40 parts of polyvinyl alcohol, 100~120 parts of quality that 100~120 parts of mass fractions are 5% are added in bottle
The nano graphite flakes water slurry that score is 40% starts blender, with 80~90r/min revolving speed stirring and emulsifying, 10~15min
Afterwards, 1~3 part of potassium peroxydisulfate is added, is heated to 45~48 DEG C, 3~4h of insulation reaction obtains Conductive NBR；By 40
The beaker equipped with 100~120mL mass fraction for 30~40% acetone solns is added in~45g acrylic acid and maleic anhydride acid copolymer
In, 80~85 DEG C are heated to, 60~70g bentonite is added to beaker, is cooled to room temperature and obtains bentonite suspension, it will be swollen
Moisten native suspension to be placed in supercentrifuge, 15~17min is centrifuged with the revolving speed of 3100~3800r/min, upper liquid is removed, obtains
To lamella bentonite, lamella bentonite is placed in baking oven, is heated to 80~90 DEG C, dry 3~4h obtains bentone
Soil；Conductive NBR is placed in double roll mill, is 45~55 DEG C in preceding roll temperature, rear roll temperature is 40~50 DEG C, roller
Away to plasticate under conditions of 8~10mm 2~3 times, then the modification of Conductive NBR quality 5~8% is added into double roll mill
Bentonite, 20~25g white carbon black, mixing are plasticated 2~3 times, are discharged, are obtained mixing rubber material；Sweet potato flour, glycerol and water are pressed into matter
Amount is mixed than 7 ︰, 4 ︰ 1, is placed in high speed disperser and is dispersed 10~15min with the revolving speed of 3000~3500r/min and obtain starch to fill out
Material, is poured into double screw extruder, and control head temperature is 230~250 DEG C, and screw speed is 160~180r/min, feeding speed
Rate is 50~75g/min, and extrusion obtains starch fillers；To with blender, reflux condenser four-hole boiling flask in be added 200~
220mL distilled water adjusts pH to 9~10 with the sodium hydroxide solution that mass fraction is 40%, is heated to 90 to four-hole boiling flask
~100 DEG C, 60~70g soy meal is added, after 50~55min of isothermal holding, 10~12g phenol, drop are added into four-hole boiling flask
Temperature continues that 20~25mL formaldehyde is added into four-hole boiling flask, reacts 1~2h to 70~75 DEG C, 15~20min of isothermal holding, from
It is so cooled to room temperature, obtains soybean protein lotion；According to parts by weight, by 10~15 parts of starch fillers, 10~18 portions of soybean eggs
Virgin's milk liquid, 20~35 parts of polyurethane foams, 5~10 parts of lactic acid bacteria powders are placed in sealed fermenter, controlled at 40~50 DEG C,
Stand 3~5 days, filtering removal the isolated fermentation filter residue of filtrate, by 70~80 parts of fermentation filter residues, 40~50 parts of copper powders, 30~
The mixing of 35 mixing rubber material is transferred in foaming machine pressurization of foaming, and 8~10 parts of azodicarbonamides, 50 is added to foaming machine
The ammonium hydroxide that~60 parts of mass fractions are 20%, the temperature for controlling foaming machine is 150 DEG C~180 DEG C, and blow pressure is 4~5MPa, out
It is cut into particle after material and obtains conductive seal agent.
The preparation of Conductive NBR:
According to parts by weight, 80 parts of acrylonitrile and 90 parts of butadiene are added in three-necked flask, 100 parts is added into three-necked flask
The nano graphite flakes aqueous suspension that sodium hydroxide solution that mass fraction is 5%, 30 parts of polyvinyl alcohol, 100 parts of mass fractions are 40%
Liquid, starting blender are added 1 part of potassium peroxydisulfate after 80r/min revolving speed stirring and emulsifying 10min, are heated to 45 DEG C, protect
Temperature reaction 3h, obtains Conductive NBR；
The preparation of modified alta-mud: it is 30% the third that 40g acrylic acid and maleic anhydride acid copolymer, which are added equipped with 100mL mass fraction,
In the beaker of ketone solution, 80 DEG C are heated to, 60g bentonite is added to beaker, is cooled to room temperature and obtains bentonite suspension,
Bentonite suspension is placed in supercentrifuge, 15min is centrifuged with the revolving speed of 3100r/min, upper liquid is removed, obtains lamella
Lamella bentonite is placed in baking oven by bentonite, is heated to 80 DEG C, and dry 3h obtains modified alta-mud；
The preparation of mixing rubber material: Conductive NBR is placed in double roll mill, is 45 DEG C in preceding roll temperature, rear roll temperature
It is 40 DEG C, roll spacing is plasticated 2 times under conditions of being 8mm, then the modification of Conductive NBR quality 5% is added into double roll mill
Bentonite, 20g white carbon black, mixing are plasticated 2 times, are discharged, are obtained mixing rubber material；
The preparation of starch fillers:
4 ︰ 1 of sweet potato flour, glycerol and water 7 ︰ in mass ratio is mixed, is placed in high speed disperser and is dispersed with the revolving speed of 3000r/min
10min obtains starch fillers, pours into double screw extruder, and control head temperature is 230 DEG C, screw speed 160r/min,
Feed rate is 50g/min, and extrusion obtains starch fillers；
The preparation of soybean protein lotion:
200mL distilled water is added into the four-hole boiling flask with blender, reflux condenser, the hydrogen-oxygen for being 40% with mass fraction
Change sodium solution and adjust pH to 9,90 DEG C is heated to four-hole boiling flask, is added 60g soy meal, after isothermal holding 50min, Xiang Si
10g phenol is added in mouth flask, is cooled to 70 DEG C, isothermal holding 15min, continues that 20mL formaldehyde is added into four-hole boiling flask, instead
1h is answered, cooled to room temperature obtains soybean protein lotion；
The preparation of conductive seal agent:
According to parts by weight, 10 parts of starch fillers, 10 parts of soybean protein lotions, 20 parts of polyurethane foams, 5 parts of lactic acid bacteria powders are set
In sealed fermenter, controlled at 40 DEG C, 3 days are stood, the filtering removal isolated fermentation filter residue of filtrate ferments 70 parts
Filter residue, 40 parts of copper powders, the mixing of 30 mixing rubber material are transferred in foaming machine pressurization of foaming, and 8 parts of azos two are added to foaming machine
The ammonium hydroxide that formamide, 50 parts of mass fractions are 20%, the temperature for controlling foaming machine is 150 DEG C, blow pressure 4MPa, after discharging
It is cut into particle and obtains conductive seal agent.
The preparation of Conductive NBR: according to parts by weight, three-necked flask is added in 85 parts of acrylonitrile and 100 parts of butadiene
In, sodium hydroxide solution, the 35 parts of polyvinyl alcohol, 110 parts of mass fractions that 110 parts of mass fractions are 5% are added into three-necked flask
For 40% nano graphite flakes water slurry, starts blender and 2 parts of mistakes are added after 85r/min revolving speed stirring and emulsifying 12.5min
Potassium sulfate, is heated to 46.5 DEG C, and insulation reaction 3.5h obtains Conductive NBR；
The preparation of modified alta-mud:
40~45g acrylic acid and maleic anhydride acid copolymer are added to the beaker equipped with 110mL mass fraction for 35% acetone soln
In, 82.5 DEG C are heated to, 65g bentonite is added to beaker, is cooled to room temperature and obtains bentonite suspension, bentonite is hanged
Supernatant liquid is placed in supercentrifuge, is centrifuged 16min with the revolving speed of 3450r/min, is removed upper liquid, obtain lamella bentonite, will
Lamella bentonite is placed in baking oven, is heated to 85 DEG C, and dry 3.5h obtains modified alta-mud；
The preparation of mixing rubber material:
Conductive NBR is placed in double roll mill, is 50 DEG C in preceding roll temperature, rear roll temperature is 45 DEG C, roll spacing 9mm
Under conditions of plasticate 2.5 times, then into double roll mill be added Conductive NBR quality 6.5% modified alta-mud, 22.5g
White carbon black, mixing are plasticated 2.5 times, are discharged, are obtained mixing rubber material；
The preparation of starch fillers:
4 ︰ 1 of sweet potato flour, glycerol and water 7 ︰ in mass ratio is mixed, is placed in high speed disperser and is dispersed with the revolving speed of 3250r/min
12.5min obtains starch fillers, pours into double screw extruder, and control head temperature is 240 DEG C, screw speed 170r/
Min, feed rate 62.5g/min, extrusion obtain starch fillers；
The preparation of soybean protein lotion:
210mL distilled water is added into the four-hole boiling flask with blender, reflux condenser, the hydrogen-oxygen for being 40% with mass fraction
Change sodium solution and adjust pH to 9.5,95 DEG C is heated to four-hole boiling flask, is added 65g soy meal, after isothermal holding 52.5min,
11g phenol is added into four-hole boiling flask, is cooled to 72.5 DEG C, isothermal holding 17.5min, continues to be added into four-hole boiling flask
22.5mL formaldehyde, reacts 1.5h, and cooled to room temperature obtains soybean protein lotion；
The preparation of conductive seal agent:
According to parts by weight, by 12.5 parts of starch fillers, 14 parts of soybean protein lotions, 27.5 parts of polyurethane foams, 7.5 parts of lactic acid
Bacterium powder is placed in sealed fermenter, controlled at 45 DEG C, stands 4 days, the filtering removal isolated fermentation filter residue of filtrate, by 75
Part fermentation filter residue, 45 parts of copper powders, 32.5 mixing rubber material mixing, be transferred in foaming machine foam pressurization, and to foaming machine be added 9
The ammonium hydroxide that part azodicarbonamide, 55 parts of mass fractions are 20%, the temperature for controlling foaming machine is 165 DEG C, and blow pressure is
4.5MPa is cut into particle and obtains conductive seal agent after discharging.
The preparation of Conductive NBR: according to parts by weight, three-necked flask is added in 90 parts of acrylonitrile and 110 parts of butadiene
In, sodium hydroxide solution, the 40 parts of polyvinyl alcohol, 120 parts of mass fractions that 120 parts of mass fractions are 5% are added into three-necked flask
For 40% nano graphite flakes water slurry, starts blender and 3 parts of over cures are added after 90r/min revolving speed stirring and emulsifying 15min
Sour potassium, is heated to 48 DEG C, and insulation reaction 4h obtains Conductive NBR；
The preparation of modified alta-mud:
It is to add in the beaker of 40% acetone soln equipped with 120mL mass fraction that 45g acrylic acid and maleic anhydride acid copolymer, which are added,
Heat is warming up to 85 DEG C, and 70g bentonite is added to beaker, is cooled to room temperature and obtains bentonite suspension, bentonite suspension is set
In supercentrifuge, 17min is centrifuged with the revolving speed of 3800r/min, upper liquid is removed, obtains lamella bentonite, lamella is swollen
Profit soil is placed in baking oven, is heated to 90 DEG C, and dry 4h obtains modified alta-mud；
The preparation of mixing rubber material:
Conductive NBR is placed in double roll mill, is 55 DEG C in preceding roll temperature, rear roll temperature is 50 DEG C, roll spacing 10mm
Under conditions of plasticate 3 times, then into double roll mill be added Conductive NBR quality 8% modified alta-mud, 25g white carbon black,
Mixing is plasticated 3 times, is discharged, is obtained mixing rubber material；
The preparation of starch fillers:
4 ︰ 1 of sweet potato flour, glycerol and water 7 ︰ in mass ratio is mixed, is placed in high speed disperser and is dispersed with the revolving speed of 3500r/min
15min obtains starch fillers, pours into double screw extruder, and control head temperature is 250 DEG C, screw speed 180r/min,
Feed rate is 75g/min, and extrusion obtains starch fillers；
The preparation of soybean protein lotion:
220mL distilled water is added into the four-hole boiling flask with blender, reflux condenser, the hydrogen-oxygen for being 40% with mass fraction
Change sodium solution and adjust pH to 10,100 DEG C is heated to four-hole boiling flask, is added 0g soy meal, after isothermal holding 55min, to
12g phenol is added in four-hole boiling flask, is cooled to 75 DEG C, isothermal holding 20min, continues that 25mL formaldehyde is added into four-hole boiling flask,
2h is reacted, cooled to room temperature obtains soybean protein lotion；
The preparation of conductive seal agent:
According to parts by weight, by 15 parts of starch fillers, 18 parts of soybean protein lotions, 35 parts of polyurethane foams, 10 parts of lactic acid bacteria powders
It is placed in sealed fermenter, controlled at 50 DEG C, stands 5 days, the filtering removal isolated fermentation filter residue of filtrate sends out 80 parts
Ferment filter residue, 50 parts of copper powders, the mixing of 35 mixing rubber material are transferred in foaming machine pressurization of foaming, and 10 parts of idols are added to foaming machine
The ammonium hydroxide that nitrogen diformamide, 60 parts of mass fractions are 20%, the temperature for controlling foaming machine is 180 DEG C, blow pressure 5MPa, out
It is cut into particle after material and obtains conductive seal agent.
Comparative example 1 and the preparation method of example 1 are essentially identical, have only the difference is that lacking mixing rubber material.
Comparative example 2 and the preparation method of example 1 are essentially identical, have only the difference is that lacking soybean protein lotion.
The sealant of 3 company, Beijing of comparative example production.
Performance detection is carried out to the sealant in the present invention and comparative example respectively, testing result is as shown in table 1:
Detection method:
Volume resistivity is detected referring to the standard of GB/T 15662.
Tensile strength is detected referring to the standard of GB 7124-2008.
Elongation at break is detected referring to the standard of GB/T 32369-2015.
1 sealant performance measurement result of table
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Volume resistivity (Ω cm) | 1.87 | 1.59 | 1.01 | 3.87 | 3.62 | 3.01 |
| Tensile strength (MPa) | 2.98 | 3.21 | 3.42 | 0.67 | 1.23 | 1.78 |
| Elongation at break (%) | 92 | 95 | 97 | 75 | 79 | 83 |
By table 1, it can be seen that conductive seal agent volume resistivity prepared by the present invention is lower, effectiveness is preferable, draws
It is preferable to stretch intensity, elongation at break is excellent, improves envelope agent to a certain extent and is bonded and sealed effect, has broad application prospects.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of conductive seal agent, it is characterised in that specific preparation step are as follows:
Starch fillers, soybean protein lotion, polyurethane foam, lactic acid bacteria powder are placed in sealed fermenter, controlled at 40
~50 DEG C, 3~5 days are stood, the filtering removal isolated fermentation filter residue of filtrate mixes fermentation filter residue, copper powder, mixing rubber material
Conjunction is transferred in foaming machine pressurization of foaming, and to the ammonium hydroxide that azodicarbonamide is added in foaming machine, mass fraction is 20%, discharges
After be cut into particle and obtain conductive seal agent；
The specific preparation step of the mixing rubber material are as follows:
(1) acrylonitrile and butadiene is added in three-necked flask, the sodium hydroxide that mass fraction is 5% is added into three-necked flask
Solution, polyvinyl alcohol, the nano graphite flakes water slurry that mass fraction is 40%, start blender, with 80~90r/min revolving speed
After 10~15min of stirring and emulsifying, potassium peroxydisulfate is added, is heated to 45~48 DEG C, 3~4h of insulation reaction obtains conductive fourth
Nitrile rubber；
(2) 40~45g acrylic acid and copolymer-maleic anhydride are added equipped with 100~120mL mass fraction is 30~40% acetone
In the beaker of solution, 80~85 DEG C are heated to, 60~70g bentonite is added to beaker, is cooled to room temperature and obtains bentonite
Bentonite suspension is placed in supercentrifuge by suspension, is centrifuged 15~17min with the revolving speed of 3100~3800r/min, is gone
Except upper liquid, lamella bentonite is obtained, lamella bentonite is placed in baking oven, is heated to 80~90 DEG C, dry 3~4h,
Obtain modified alta-mud；
(3) Conductive NBR is placed in double roll mill, is plasticated 2~3 times, then conductive butyronitrile is added into double roll mill
Modified alta-mud, the 20~25g white carbon black of rubber quality 5~8%, mixing are plasticated 2~3 times, are discharged, are obtained mixing rubber material；
The specific preparation step of the mixing rubber material are as follows:
(1) 4 ︰ 1 of sweet potato flour, glycerol and water 7 ︰ in mass ratio is mixed, is placed in high speed disperser with 3000~3500r/min's
Revolving speed disperses 10~15min and obtains starch fillers, pours into double screw extruder, and extrusion obtains starch fillers；
(2) 200~220mL distilled water is added into the four-hole boiling flask with blender, reflux condenser, is with mass fraction
40% sodium hydroxide solution adjusts pH, is heated to 90~100 DEG C to four-hole boiling flask, and 60~70g soy meal, heat preservation is added
After handling 50~55min, 10~12g phenol is added into four-hole boiling flask, is cooled to 70~75 DEG C, 15~20min of isothermal holding,
Continue that 20~25mL formaldehyde is added into four-hole boiling flask, react 1~2h, cooled to room temperature obtains soybean protein lotion.
2. a kind of preparation method of conductive seal agent according to claim 1, it is characterised in that: according to parts by weight, 10
~15 parts of starch fillers, 10~18 parts of soybean protein lotions, 20~35 parts of polyurethane foams, 5~10 parts of lactic acid bacteria powders, 70~80
Part fermentation filter residue, 40~50 parts of copper powders, 30~35 parts of mixing rubber material, 8~10 parts of azodicarbonamides, 50~60 parts of quality point
The ammonium hydroxide that number is 20%.
3. a kind of preparation method of conductive seal agent according to claim 1, it is characterised in that: control hair in foaming process
The temperature of bubble machine is 150 DEG C~180 DEG C, and blow pressure is 4~5MPa.
4. a kind of preparation method of conductive seal agent according to claim 1, it is characterised in that: the mixing rubber material
Specific preparation step (1) in prepare each raw material of Conductive NBR, according to parts by weight, including 80~90 parts of acrylonitrile, 90
~110 parts of butadiene, the sodium hydroxide solution that 100~120 parts of mass fractions are 5%, 30~40 parts of polyvinyl alcohol, 100~120
Nano graphite flakes water slurry, 1~3 part potassium peroxydisulfate of part mass fraction for 40%.
5. a kind of preparation method of conductive seal agent according to claim 1, it is characterised in that: the mixing rubber material
Specific preparation step (2) used in acrylic acid and the preferred maleic anhydride of copolymer-maleic anhydride and acrylic acid 3 ︰ of mass ratio
1。
6. a kind of preparation method of conductive seal agent according to claim 1, it is characterised in that: the mixing rubber material
Specific preparation step (3) in plasticate shorten into middle double roll mill preceding roll temperature be 45~55 DEG C, rear roll temperature be 40~50
DEG C, roll spacing is 8~10mm.
7. a kind of preparation method of conductive seal agent according to claim 1, it is characterised in that: the mixing rubber material
Specific preparation step (1) in sweet potato flour, 7 ︰ of glycerol and water mixing mass ratio, 4 ︰ 1.
8. a kind of preparation method of conductive seal agent according to claim 1, it is characterised in that: the mixing rubber material
Specific preparation step (1) in extrusion double screw extruder when preparing starch fillers parameter are as follows: head temperature is 230~250
DEG C, screw speed is 160~180r/min, and feed rate is 50~75g/min.
9. a kind of preparation method of conductive seal agent according to claim 1, it is characterised in that: the mixing rubber material
Specific preparation step (2) in heat temperature raising handle before sodium hydroxide solution adjust flask in reaction system pH be 9~10.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1149895A (en) * | 1997-04-30 | 1999-02-23 | Yokohama Rubber Co Ltd:The | Production of rubber composition containing modified carbon black for rubber reinforcement |
| CN107325748A (en) * | 2017-06-02 | 2017-11-07 | 中国航发北京航空材料研究院 | It is capable of bi-component electrically conductive organosilicon sealant of doped graphene and preparation method thereof |
| CN108659393A (en) * | 2018-05-15 | 2018-10-16 | 王雪峰 | A kind of preparation method of sealing electromagnetic shielding elastic material |
-
2019
- 2019-04-30 CN CN201910362120.9A patent/CN110041554A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1149895A (en) * | 1997-04-30 | 1999-02-23 | Yokohama Rubber Co Ltd:The | Production of rubber composition containing modified carbon black for rubber reinforcement |
| CN107325748A (en) * | 2017-06-02 | 2017-11-07 | 中国航发北京航空材料研究院 | It is capable of bi-component electrically conductive organosilicon sealant of doped graphene and preparation method thereof |
| CN108659393A (en) * | 2018-05-15 | 2018-10-16 | 王雪峰 | A kind of preparation method of sealing electromagnetic shielding elastic material |
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Application publication date: 20190723 |