CN109722034A - A kind of antistatic silicone rubber foamed material and preparation method thereof - Google Patents
A kind of antistatic silicone rubber foamed material and preparation method thereof Download PDFInfo
- Publication number
- CN109722034A CN109722034A CN201811517417.XA CN201811517417A CN109722034A CN 109722034 A CN109722034 A CN 109722034A CN 201811517417 A CN201811517417 A CN 201811517417A CN 109722034 A CN109722034 A CN 109722034A
- Authority
- CN
- China
- Prior art keywords
- parts
- agent
- antistatic
- silicone rubber
- polyethylene glycol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of antistatic silicone rubber foamed materials and preparation method thereof, the silicon rubber foam material mainly includes that following component raw material is made: 110 parts of raw-silastic continuously, 30~48 parts of filler, 2~10 parts of antistatic agent, 0~3 part of silane coupling agent, 1.5~12 parts of hydroxy silicon oil, 2~10 parts of solvent, 4~10 parts of foaming agent, 2~6 parts of blowing promotor, 0.1~0.5 part of release agent, 0.5~5 part of vulcanizing agent.The present invention also includes preparation method, antistatic agent solution and filler are first subjected to dispersion pretreatment, then pretreated filler and raw rubber, auxiliary agent etc. are kneaded, foaming agent then is added and vulcanizing agent mill is uniform, it is squeezed out or is pressed and molded, or can further post vulcanization molding.Antistatic effect is good after silicon rubber foam material vulcanization prepared by the present invention, and antistatic property is lasting and can free colour matching；Preparation method simply can yield.
Description
Technical field
The present invention relates to field of rubber materials, more particularly to a kind of antistatic silicone rubber foamed material and its preparation side
Method.
Background technique
Silicon rubber have good mechanical property, excellent gas permeability, physiological inertia, weatherability, heat resistance, cold resistance with
And electrical insulation capability etc., it is obtained in numerous areas such as automobile parts, electric power electrical apparatus, architectural engineering, medical instrument, daily necessities
Extensive utilization.Silicon rubber electrical insulation capability is good, and accumulation of static electricity can be generated when contacting or rubbing with other materials, especially deposits some
Have and easily causes great electrostatic hazard when using in the environment of fire hazard.Therefore excellent antistatic property and lasting silicon rubber
Material can be effectively avoided in use process because of insecurity caused by electrostatic.Silicon rubber foam material both maintains silicon rubber
Special performance has many advantages, such as lightweight, heat-insulated, flexibility and resilience simultaneously, plays damping in practical engineering application, fills out
The effects of filling sealing and noise reduction sound insulation.
Preparing antistatic silicone rubber foamed material mainly at present has the conductive Carbon Materials of addition, surface coating or interior addition surface
Activating agent and addition three kinds of methods of conductive metal or metal-oxide powder.Wherein, carbon black is unfavorable for silicone rubber products coloring
And keep clean processing environment, carbon nanotube and graphene higher cost；Surface coating or interior addition surfactant are most
Non-refractory or antistatic persistence are poor；The poor compatibility of addition conductive metal or metal oxide and silicon rubber leads to product capability
Performance is learned to decline to a great extent.Therefore the antistatic agent composition for being suitble to silicon rubber vulcanization system is selected, antistatic agent and silicon rubber are improved
Compatibility between glue guarantees that the lasting stability of antistatic effect is the critical problem of invention.
Summary of the invention
The purpose of the present invention is to provide a kind of antistatic silicone rubber foamed materials and preparation method thereof.For antistatic agent
Compatibility, dispersing uniformity and antistatic effect persistent problem in silicon rubber select high temperature resistant polyethers and imidazole salts
Reaction prepares high performance antistatic agent, by by antistatic agent with filler is well-mixed pre-processes, promote antistatic agent
Sufficiently adhere to filler surface, improves dispersibility and compatibility of the antistatic agent in silicon rubber, to make silicon rubber foam material
Material obtains the antistatic property effect of lasting stability.
The technical solution used in the present invention is:
A kind of antistatic silicone rubber foamed material, which is characterized in that include following raw material: silicon rubber according to the mass fraction
80~110 parts of raw rubber, 30~48 parts of filler, 2~10 parts of antistatic agent, 0~3 part of silane coupling agent, hydroxy silicon oil 1.5~12
Part, 2~10 parts of solvent, 4~10 parts of foaming agent, 2~6 parts of blowing promotor, 0.1~0.5 part of release agent, 0.5~5 part of vulcanizing agent.
Preferably, the antistatic agent is polyethylene glycol imidazolium ionic liquid, the polyethylene glycol imidazolium ion
The general structure of liquid are as follows:
Wherein X=Br, BF4, PF6, NO3, NO2, SbF6, ZnCl3, SnCl3, SO3, HSO3, H2PO4, CF3CO2, CF3SO3,
CH3SO3, C (CF3SO2)3, N (CF3SO2)2, N (FSO2)2, N (C2F5SO2)2, NTf2；n≥4；R be H or 1~4 carbon atom not
Saturation or saturated straight chain or branch chain alkyl.
It is further preferred that the preparation of the polyethylene glycol imidazolium ionic liquid formula (I) is the following steps are included: by imidazoles
It is reacted in microwave reactor with monochloro for polyethylene glycol, then by gained intermediate product polyethylene glycol imidazole radicals chlorate
It is dissolved into anhydrous second cyanogen solvent, is stirred at room temperature under nitrogen protection after addition coordination anion salt and completes ion-exchange reactions,
It is evaporated under reduced pressure solvent after being filtered to remove villaumite with diatomite again and obtains target product.
It is further preferred that the preparation of the polyethylene glycol imidazolium ionic liquid formula (II) is the following steps are included: by miaow
Azoles and both-end chlorinated polyethylene glycol are added in the reaction kettle containing dry toluene, and the lower reaction of argon gas protection generates rufous liquid
Body takes lower liquid to be washed with ether after cooling, the double imidazole radicals chlorates of polyethylene glycol is obtained after vacuum drying, finally by gained
The double imidazole radicals chlorates of polyethylene glycol are dissolved into anhydrous second cyanogen solvent, and room temperature is stirred under nitrogen protection after addition coordination anion salt
It mixes and completes ion-exchange reactions, then be evaporated under reduced pressure solvent after being filtered to remove villaumite with diatomite and obtain target product.
Preferably, the raw-silastic continuously is methyl vinyl silicon kautschuk, dimethyl silicone rubber raw rubber, methylbenzene
One of base vinylsiloxane rubber or multiple combinations.
Preferably, the filler is the combination of one or both of fume colloidal silica, precipitated silica.
Preferably, the silane coupling agent is vinyltrimethoxysilane, vinyltriethoxysilane, dimethyl
One of dimethoxysilane, hexamethyldisilazane or multiple combinations；The solvent be N-Methyl pyrrolidone, water,
One of methanol, methylene chloride, acetonitrile etc. or multiple combinations.
Preferably, the vulcanizing agent is benzoyl peroxide, cumyl peroxide, 2,4- dichloro benzoyl peroxide first
Acyl, two (t-butylperoxyisopropyl) benzene, bis- (tert-butyl peroxide) hexanes (bis 25 vulcanizing agent) of 2,5- dimethyl -2,5-
One of or multiple combinations.
Preferably, the release agent is one of calcium stearate, zinc stearate, barium stearate or multiple combinations；It is described
Foaming agent is one or both of dinitrosopentamethlyene tetramine (blowing agent H), azodicarbonamide (blowing agent AC) group
It closes；Blowing promotor is the combination of one or both of urea rouge, zinc oxide.
The preparation method of antistatic silicone rubber foamed material, which comprises the following steps:
(1) first antistatic agent is uniformly mixed with solvent, antistatic agent mixed solution is made；
(2) antistatic mixed solution is placed in high speed disperser with filler and is dispersed, room temperature is above for 24 hours spare；
(3) after raw-silastic continuously, hydroxy silicon oil, silane coupling agent, release agent being added in kneader, then step is added portionwise
Suddenly filler after (2) decentralized processing is mediated uniformly, and room temperature is kneaded 10~30min, be warming up to 110~130 DEG C be kneaded 20~
It discharges after 40min；
(4) foaming agent is added in above-mentioned steps (3) rubber compound on a mill and vulcanizing agent mill is uniform；
(5) extrusion molding or compression molding；
(6) post vulcanization.
As a preferred solution of the present invention, the relative molecular weight of the polyethylene glycol imidazolium ionic liquid be 400~
4000；The white carbon black BET method specific surface area is 50m2/ g or more, particularly preferred 100~300m2/g；The release agent is preferred
Zinc stearate, preferably 0.1~0.3 part of dosage；The foaming agent and the total dosage of auxiliary agent are preferably 6~12 parts.
The specific preparation step of antistatic silicone rubber foamed material:
(1) first antistatic agent is uniformly mixed with solvent, antistatic agent mixed solution is made；
(2) antistatic mixed solution and filler are placed in high speed disperser and disperse 30min, room temperature is above for 24 hours standby
With；
(3) after raw-silastic continuously, hydroxy silicon oil, silane coupling agent, release agent being added in kneader, then step is added portionwise
Suddenly the filler after (2) decentralized processing is mediated uniformly, and room temperature is kneaded 20min, is gone out after being warming up to 110~130 DEG C of mixing 30min
Material；
(4) foaming agent is added in above-mentioned steps (3) rubber compound on a mill and vulcanizing agent mill is uniform；
(5) extrusion molding or compression molding；
(6) post vulcanization.
The beneficial effects of the present invention are: antistatic agent used herein has polyoxyethylene ether and imidazole salt ionic liquid
The denominator of body antistatic agent, and be not easy for opposite small molecular ion liquid (such as -3 methyl tetrafluoro boron fluorate of 1- ethyl)
It is migrated from silicon rubber；Furthermore by being pre-processed to silicon rubber reinforced filling white carbon black, antistatic agent is evenly dispersed simultaneously
It is adsorbed on white carbon black surface, being subject to suitable calendering process preparation may be implemented the quasi- effect reached of the present invention: antistatic agent exists
Good dispersibility is obtained during mixing silicon rubber；It is formed using scatter-gather state of the pretreatment reinforced filling in silicon rubber
Conductive network is formed in microstructure；Improve compatibility of the antistatic agent in silicon rubber, weakens to a certain extent antistatic
Agent transfer ability guarantees the persistence of silicon rubber antistatic effect, enhances antistatic agent in silicon rubber foam material adaptability.This
Outside, preparation method of the present invention is simple, is produced on a large scale, and economic benefit is obvious.
Specific embodiment
Below by specific embodiment, the present invention is further explained, but the present invention is not limited only to this.Embodiment and comparative example
The antistatic silicone rubber foamed material volume resistivity measurement method of preparation is referring to GB/T 1410-2006 (solid insulating material
Volume resistivity and surface resistivity test method), it the results are shown in Table 1.
Heretofore described polyethylene glycol imidazole salts polymer ions liquid synthetic route following reaction formula (I), (II).Its
Middle X includes Br, BF4, PF6, NO3, NO2, SbF6, ZnCl3, SnCl3, SO3, HSO3, H2PO4, CF3CO2, CF3SO3, CH3SO3, C
(CF3SO2)3, N (CF3SO2)2, N (FSO2)2, N (C2F5SO2)2, NTf2；R includes the insatiable hunger and/or saturation of H or 1~4 carbon atom
Straight chain or branch chain alkyl；n≥4；Prepared polymer molecular weight is 400~4000.
Mainly there are two steps for polyethyleneglycol imidazolium ionic liquid (formula I), first by imidazoles and monochloro for poly- second two
Alcohol is reacted in microwave reactor, and gained intermediate product polyethylene glycol imidazole radicals chlorate is then dissolved into anhydrous second cyanogen
In solvent, it is stirred at room temperature under nitrogen protection after addition coordination anion salt and completes ion-exchange reactions for 24 hours, finally with diatomite mistake
It filters out vacuum distillation after villaumite and falls solvent and obtain target product.
Similarly, polyethylene glycol Neo Heliopan AP ionic liquid formula (II) also includes two steps, first by imidazoles and both-end
Chlorinated polyethylene glycol is added in the reaction kettle containing dry toluene, and the lower reaction of argon gas protection generates rufous liquid, after cooling
It takes lower liquid to be washed 3 times with ether, the double imidazole radicals chlorates of polyethylene glycol is obtained after vacuum drying, finally by the poly- second two of gained
The double imidazole radicals chlorates of alcohol are dissolved into anhydrous second cyanogen solvent, are stirred at room temperature for 24 hours under nitrogen protection after addition coordination anion salt
Complete carry out ion-exchange reactions is evaporated under reduced pressure solvent and obtains target product after being finally filtered to remove villaumite with diatomite.
In following embodiment of the present invention in polyethylene glycol imidazole radicals salt polymer ions liquid polyethylene glycol segment with its point
The form of son amount size indicates.
Embodiment 1
90 parts of methyl vinyl silicon kautschuk；10 parts of dimethyl silicone rubber raw rubber；BET method specific surface area 170m2/ g's
38 parts of fume colloidal silica；- 3 polyethylene glycol of 1- methyl (200) 6 parts of ionic liquid of tetrafluoroborate of list；2 parts of water, methanol 4
Part；1.5 parts of dimethyldimethoxysil,ne；2.2 parts of hydroxy silicon oil；0.3 part of zinc stearate；4 parts of blowing agent H, 2 parts of zinc oxide；
0.8 part of benzoyl peroxide, two 0.4 part of (t-butylperoxyisopropyl) benzene.
Specific step is as follows by the preparation process of the present embodiment antistatic silicone rubber foamed material:
(1) the single tetrafluoroborate ionic liquid of -3 polyethylene glycol of 1- methyl (200) is uniformly mixed with water and methanol,
Antistatic agent mixed solution is made；
(2) antistatic agent mixed solution is poured into fume colloidal silica and then disperses 30min, dispersion with high speed disperser
After the completion room temperature for 24 hours more than；
(3) methyl vinyl silicon kautschuk, dimethyl silicone rubber raw rubber, dimethylformamide dimethyl oxygroup are added in kneader
White carbon black after step (2) decentralized processing is added portionwise after silane, hydroxy silicon oil, zinc stearate is mediated uniformly, and room temperature is kneaded
20min discharges after being warming up to 120 DEG C of mixing 30min；
(4) blowing agent H, zinc oxide, benzoyl peroxide and two is added in above-mentioned steps (3) rubber compound on a mill
Mill is uniform after (t-butylperoxyisopropyl) benzene.
(5) it after being pressed and molded, carries out post vulcanization (180 DEG C, 2h).
Comparative example 1
90 parts of methyl vinyl silicon kautschuk；10 parts of dimethyl silicone rubber raw rubber；BET method specific surface area 170m2/ g's
38 parts of fume colloidal silica；- 3 polyethylene glycol of 1- methyl (200) 6 parts of ionic liquid of tetrafluoroborate of list；2 parts of water, methanol 4
Part；1.5 parts of dimethyldimethoxysil,ne；2.2 parts of hydroxy silicon oil；0.3 part of zinc stearate；4 parts of blowing agent H, 2 parts of zinc oxide；
0.8 part of benzoyl peroxide, two 0.4 part of (t-butylperoxyisopropyl) benzene.
This comparative example antistatic silicone rubber foam formulation is same as Example 1, but antistatic agent, solvent, fills out
Material, which is added directly into silicon rubber, to be kneaded, the specific steps are as follows:
(1) methyl vinyl silicon kautschuk, dimethyl silicone rubber raw rubber, dimethylformamide dimethyl oxygroup are added in kneader
The single tetrafluoroborate ionic liquid of silane, -3 polyethylene glycol of 1- methyl (200), water, methanol, hydroxy silicon oil, zinc stearate
After be added portionwise fume colloidal silica mediate uniformly, room temperature be kneaded 20min, discharge after being warming up to 120 DEG C of mixing 30min；
(2) blowing agent H, zinc oxide, benzoyl peroxide and two is added in above-mentioned steps (3) rubber compound on a mill
Mill is uniform after (t-butylperoxyisopropyl) benzene.
(3) it after being pressed and molded, carries out post vulcanization (180 DEG C, 2h)
Embodiment 2
100 parts of methyl vinyl silicon kautschuk；BET method specific surface area 200m230 parts of/g precipitated silica；1- second
- 3 polyethylene glycol of base (200) 5 parts of ionic liquid of tetrafluoroborate of list；5 parts of N-Methyl pyrrolidone；Vinyl trimethoxy
1.2 parts of silane；1.8 parts of hydroxy silicon oil；4 parts of blowing agent H, 2 parts of zinc oxide；0.1 part of zinc stearate, benzoyl peroxide 0.8
Part, two 0.4 part of (t-butylperoxyisopropyl) benzene.
Specific step is as follows by the preparation process of the present embodiment antistatic silicone rubber foamed material:
(1) the single tetrafluoroborate ionic liquid of -3 polyethylene glycol of 1- ethyl (200) and N-Methyl pyrrolidone is mixed
It closes uniformly, antistatic agent mixed solution is made；
(2) antistatic agent mixed solution is poured into fume colloidal silica and then disperses 30min, dispersion with high speed disperser
After the completion room temperature for 24 hours more than；
(3) methyl vinyl silicon kautschuk, dimethyl silicone rubber raw rubber, dimethylformamide dimethyl oxygroup are added in kneader
White carbon black after step (2) decentralized processing is added portionwise after silane, hydroxy silicon oil, zinc stearate is mediated uniformly, and room temperature is kneaded
20min discharges after being warming up to 110 DEG C of mixing 30min；
(4) blowing agent H, zinc oxide, benzoyl peroxide and two is added in above-mentioned steps (3) rubber compound on a mill
Mill is uniform after (t-butylperoxyisopropyl) benzene.
(5) it after being pressed and molded, carries out post vulcanization (200 DEG C, 2h).
Comparative example 2
100 parts of methyl vinyl silicon kautschuk；BET method specific surface area 200m230 parts of/g precipitated silica；1- second
5 parts of fluorate of -3 methyl tetrafluoro boron of base；5 parts of N-Methyl pyrrolidone；1.2 parts of vinyltrimethoxysilane；Hydroxy silicon oil 1.8
Part；4 parts of blowing agent H, 2 parts of zinc oxide；0.8 part of benzoyl peroxide, two 0.4 part of (t-butylperoxyisopropyl) benzene.
Specific step is as follows by the preparation process of this comparative example antistatic silicone rubber foamed material:
(1) -3 methyl tetrafluoro boron 5 parts of ionic liquids of fluorate of 1- ethyl are uniformly mixed with N-Methyl pyrrolidone, are made
Antistatic agent mixed solution；
(2) antistatic agent mixed solution is poured into fume colloidal silica and then disperses 30min, dispersion with high speed disperser
After the completion room temperature for 24 hours more than；
(3) methyl vinyl silicon kautschuk, dimethyl silicone rubber raw rubber, dimethylformamide dimethyl oxygroup are added in kneader
White carbon black after step (2) decentralized processing is added portionwise after silane, hydroxy silicon oil, zinc stearate is mediated uniformly, and room temperature is kneaded
20min discharges after being warming up to 110 DEG C of mixing 30min；
(4) blowing agent H, zinc oxide, benzoyl peroxide and two is added in above-mentioned steps (3) rubber compound on a mill
Mill is uniform after (t-butylperoxyisopropyl) benzene.
(5) it after being pressed and molded, carries out post vulcanization (200 DEG C, 2h).
Embodiment 3
100 parts of methyl phenyl vinyl silicone rubber raw rubber；BET method specific surface area 170m236 parts of/g precipitated silica；1-
- 3 polyethylene glycol of vinyl (200) 6 parts of ionic liquid of imidazoles trifluoromethanesulfonic acid of list；2 parts of water；2 parts of N-Methyl pyrrolidone；Two
2 parts of methyl dimethoxysilane；2 parts of hydroxy silicon oil；0.3 part of zinc stearate；5 parts of blowing agent AC；2 parts of urea rouge；Double two or five sulphur
1.5 parts of agent.
Specific step is as follows by the preparation process of the present embodiment antistatic silicone rubber foamed material:
(1) by the single imidazoles trifluoromethanesulfonic acid ionic liquid of -3 polyethylene glycol of 1- vinyl (200) and N- crassitude
Ketone and water are uniformly mixed, and antistatic agent mixed solution is made；
(2) antistatic mixed solution and precipitated silica are placed in high speed disperser and disperse 30min, room temperature
More than for 24 hours；
(3) methyl vinyl silicon kautschuk, dimethyldimethoxysil,ne, hydroxy silicon oil, hard is added in kneader
White carbon black after above-mentioned steps (2) decentralized processing is added portionwise after ester acid zinc is mediated uniformly, and room temperature is kneaded 20min, is warming up to 120
DEG C be kneaded 30min after discharge；
(4) it is uniform that blowing agent AC, urea rouge and double two or five mills is added in above-mentioned steps (3) rubber compound on a mill.
(5) it after being pressed and molded, carries out post vulcanization (200 DEG C, 2h).
Comparative example 3
100 parts of methyl phenyl vinyl silicone rubber raw rubber；BET method specific surface area 170m236 parts of/g precipitated silica；1-
- 36 parts of methylimidazole trifluoromethanesulfonic acid ionic liquid of vinyl；2 parts of water；2 parts of N-Methyl pyrrolidone；Dimethylformamide dimethyl oxygen
2 parts of base silane；2 parts of hydroxy silicon oil；0.3 part of zinc stearate；5 parts of blowing agent AC；2 parts of urea rouge；1.5 parts of bis 25 vulcanizing agent.
Specific step is as follows by the preparation process of this comparative example antistatic silicone rubber foamed material:
(1) -3 methylimidazole trifluoromethanesulfonic acid ionic liquid of 1- vinyl is mixed with N-Methyl pyrrolidone and water
It is even, antistatic agent mixed solution is made；
(2) antistatic mixed solution and precipitated silica are placed in high speed disperser and disperse 30min, room temperature
More than for 24 hours；
(3) methyl vinyl silicon kautschuk, dimethyldimethoxysil,ne, hydroxy silicon oil, hard is added in kneader
White carbon black after above-mentioned steps (2) decentralized processing is added portionwise after ester acid zinc is mediated uniformly, and room temperature is kneaded 20min, is warming up to 120
DEG C be kneaded 30min after discharge；
(4) it is uniform that blowing agent AC, urea rouge and double two or five mills is added in above-mentioned steps (3) rubber compound on a mill.
(5) it after being pressed and molded, carries out post vulcanization (200 DEG C, 2h).
Embodiment 4
100 parts of methyl vinyl silicon kautschuk；BET method specific surface area 300m230 parts of/g precipitated silica；1- third
6 parts of -3 polyethylene glycol of base (400) list tetrafluoroborate ionic liquid, 2 parts of water, 5 parts of methanol；Vinyltriethoxysilane
2 parts；1.8 parts of hydroxy silicon oil；2 parts of blowing agent H；6 parts of blowing agent AC；3 parts of urea rouge；0.3 part of zinc stearate；Benzoyl peroxide first
1 part of acyl, two 0.4 part of (t-butylperoxyisopropyl) benzene.
Specific step is as follows by the preparation process of the antistatic antistatic silicone rubber foamed material of the present embodiment:
(1) the single tetrafluoroborate ionic liquid of -3 polyethylene glycol of 1- propyl (400) is sufficiently mixed with first alcohol and water
Uniformly, antistatic agent mixed solution is made；
(2) antistatic mixed solution is added in precipitated silica and disperses 30min, room temperature in high speed disperser
It places more than for 24 hours；
(3) methyl vinyl silicon kautschuk, hydroxy silicon oil, vinyltriethoxysilane, hard is added in kneader
White carbon black after above-mentioned steps (2) decentralized processing is added portionwise after ester acid zinc, room temperature are kneaded 20min, are warming up to 130 DEG C of mixings
It discharges after 30min；
(4) blowing agent H, blowing agent AC, urea rouge, benzoyl peroxide first is added in above-mentioned steps (3) rubber compound on a mill
Acyl, two (t-butylperoxyisopropyl) benzene mills are uniform.
(5) extrusion molding carries out post vulcanization (185 DEG C, 2.5h).
Comparative example 4
100 parts of methyl vinyl silicon kautschuk；BET method specific surface area 200m230 parts of/g precipitated silica；1- third
- 36 parts of n-octyl tetrafluoroborate ionic liquid of base, 4 parts of N-Methyl pyrrolidone, 2 parts of methanol；Vinyl triethoxyl
2 parts of silane；1.8 parts of hydroxy silicon oil；2 parts of blowing agent H；6 parts of blowing agent AC；3 parts of urea rouge；0.3 part of zinc stearate；Peroxidating
1 part of benzoyl, two 0.4 part of (t-butylperoxyisopropyl) benzene.
Specific step is as follows by the preparation process of this comparative example antistatic silicone rubber foamed material:
(1) -3 n-octyl tetrafluoroborate ionic liquid of 1- propyl and first alcohol and water are sufficiently mixed uniformly, are made
Antistatic agent mixed solution；
(2) antistatic mixed solution is added in precipitated silica and disperses 30min, room temperature in high speed disperser
It places more than for 24 hours；
(3) methyl vinyl silicon kautschuk, hydroxy silicon oil, vinyltriethoxysilane, hard is added in kneader
White carbon black after above-mentioned steps (2) decentralized processing is added portionwise after ester acid zinc, room temperature are kneaded 20min, are warming up to 130 DEG C of mixings
It discharges after 30min；
(4) blowing agent H, blowing agent AC, urea rouge, benzoyl peroxide first is added in above-mentioned steps (3) rubber compound on a mill
Acyl, two (t-butylperoxyisopropyl) benzene mills are uniform.
(5) extrusion molding carries out post vulcanization (185 DEG C, 2.5h).
Embodiment 5
100 parts of methyl vinyl silicon kautschuk；BET method specific surface area 200m230 parts of/g precipitated silica；1- first
6 parts of the double tetrafluoroborate ionic liquids of -3 polyethylene glycol of base (200), 2 parts of water, 5 parts of methanol；Vinyltriethoxysilane
2 parts；1.8 parts of hydroxy silicon oil；2 parts of blowing agent H；6 parts of blowing agent AC；2 parts of urea rouge；0.3 part of zinc stearate；Benzoyl peroxide first
1 part of acyl, two 0.4 part of (t-butylperoxyisopropyl) benzene.
Specific step is as follows by the preparation process of the present embodiment antistatic silicone rubber foamed material:
(1) the double tetrafluoroborate ionic liquids of -3 polyethylene glycol of 1- methyl (200) are sufficiently mixed with first alcohol and water
Uniformly, antistatic agent mixed solution is made；
(2) antistatic mixed solution is added in precipitated silica and disperses 30min, room temperature in high speed disperser
It places more than for 24 hours；
(3) methyl vinyl silicon kautschuk, hydroxy silicon oil, vinyltriethoxysilane, hard is added in kneader
White carbon black after above-mentioned steps (2) decentralized processing is added portionwise after ester acid zinc, room temperature are kneaded 20min, are warming up to 130 DEG C of mixings
It discharges after 30min；
(4) blowing agent H, blowing agent AC, urea rouge, benzoyl peroxide first is added in above-mentioned steps (3) rubber compound on a mill
Acyl, two (t-butylperoxyisopropyl) benzene mills are uniform.
(5) extrusion molding, post vulcanization (185 DEG C, 2.5h).
Comparative example 5
100 parts of methyl vinyl silicon kautschuk；BET method specific surface area 300m230 parts of/g precipitated silica；1,6- bis-
6 parts of (3- hexyl imidazolium) hexylidene hexafluorophosphoric acid ionic liquid, 2 parts of water, 5 parts of methanol；2 parts of vinyltriethoxysilane；
1.8 parts of hydroxy silicon oil；2 parts of blowing agent H；6 parts of blowing agent AC；2 parts of urea rouge；0.3 part of zinc stearate；Benzoyl peroxide 1
Part, two 0.4 part of (t-butylperoxyisopropyl) benzene.
Specific step is as follows by the preparation process of this comparative example antistatic silicone rubber foamed material:
(1) (3- hexyl imidazolium) the hexylidene hexafluorophosphoric acid ionic liquid of 1,6- bis- and first alcohol and water are sufficiently mixed
It is even, antistatic agent mixed solution is made；
(2) antistatic mixed solution is added in precipitated silica and disperses 30min, room temperature in high speed disperser
It places more than for 24 hours；
(3) methyl vinyl silicon kautschuk, hydroxy silicon oil, vinyltriethoxysilane, hard is added in kneader
White carbon black after above-mentioned steps (2) decentralized processing is added portionwise after ester acid zinc, room temperature are kneaded 20min, are warming up to 130 DEG C of mixings
It discharges after 30min；
(4) blowing agent H, blowing agent AC, urea rouge, benzoyl peroxide first is added in above-mentioned steps (3) rubber compound on a mill
Acyl, two (t-butylperoxyisopropyl) benzene mills are uniform.
(5) extrusion molding, post vulcanization (185 DEG C, 2.5h).
Embodiment 6
80 parts of methyl vinyl silicon kautschuk；BET method specific surface area 200m215 parts of/g precipitated silica；BET method ratio
Surface area 200m215 parts of/g fume colloidal silica；- 3 polyethylene glycol of 1- ethyl (200) list tetrafluoroborate ionic liquid 2
Part；5 parts of methylene chloride；1.5 parts of hydroxy silicon oil；4 parts of blowing agent H, 2 parts of zinc oxide；0.1 part of barium stearate, peroxidating diisopropyl
0.5 part of benzene.
Specific step is as follows by the preparation process of the present embodiment antistatic silicone rubber foamed material:
(1) the single tetrafluoroborate ionic liquid of -3 polyethylene glycol of 1- ethyl (200) is uniformly mixed with methylene chloride,
Antistatic agent mixed solution is made；
(2) antistatic agent mixed solution is poured into fume colloidal silica and precipitated silica, then uses high speed dispersion
Machine disperse 30min, after the completion of dispersion room temperature for 24 hours more than；
(3) step is added portionwise after methyl vinyl silicon kautschuk, hydroxy silicon oil, barium stearate being added in kneader
(2) white carbon black after decentralized processing is mediated uniformly, and room temperature is kneaded 10min, is discharged after being warming up to 110 DEG C of mixing 40min；
(4) it is opened after blowing agent H, zinc oxide, cumyl peroxide being added in above-mentioned steps (3) rubber compound on a mill
Refining is uniform.
(5) it after being pressed and molded, carries out post vulcanization (200 DEG C, 2h).
Embodiment 7
110 parts of methyl vinyl silicon kautschuk；BET method specific surface area 200m224 parts of/g precipitated silica；BET method
Specific surface area 200m224 parts of/g fume colloidal silica；- 3 polyethylene glycol of 1- ethyl (200) list tetrafluoroborate ionic liquid
10 parts；5 parts of methylene chloride；5 parts of acetonitrile；9 parts of hydroxy silicon oil；3 parts of vinyltrimethoxysilane, vinyltriethoxysilane
3 parts, 3 parts of hexamethyldisilazane, 10 parts of blowing agent H, 3 parts of urea rouge, 3 parts of zinc oxide；0.4 part of calcium stearate, barium stearate
0.1 part, 4 parts of 2,4- dichlorobenzoperoxide.
Specific step is as follows by the preparation process of the present embodiment antistatic silicone rubber foamed material:
(1) the single tetrafluoroborate ionic liquid of -3 polyethylene glycol of 1- ethyl (200) and methylene chloride and acetonitrile is mixed
It closes uniformly, antistatic agent mixed solution is made；
(2) antistatic agent mixed solution is poured into fume colloidal silica and precipitated silica, then uses high speed dispersion
Machine disperse 30min, after the completion of dispersion room temperature for 24 hours more than；
(3) methyl vinyl silicon kautschuk, vinyltrimethoxysilane, three ethoxy of vinyl are added in kneader
After step (2) decentralized processing is added portionwise after base silane, hexamethyldisilazane, hydroxy silicon oil, calcium stearate, barium stearate
White carbon black is mediated uniformly, and room temperature is kneaded 30min, is discharged after being warming up to 130 DEG C of mixing 20min；
(4) blowing agent H, zinc oxide, urea rouge, 2,4- dichloro mistake is added in above-mentioned steps (3) rubber compound on a mill
Mill is uniform after Benzoyl Oxide.
(5) it after being pressed and molded, carries out post vulcanization (200 DEG C, 2h).
Embodiment 8
100 parts of methyl vinyl silicon kautschuk；BET method specific surface area 300m230 parts of/g precipitated silica；1- first
- 3 polyethylene glycol of base (400) 6 parts, 2 parts of methanol of ionic liquid of tetrafluoroborate of list；2 parts of vinyltriethoxysilane；Hydroxyl
12 parts of base silicone oil；2 parts of blowing agent H；6 parts of blowing agent AC；3 parts of urea rouge；0.3 part of zinc stearate；3 parts of benzoyl peroxide,
2,4- 2 parts of dichlorobenzoperoxides.
Specific step is as follows by the preparation process of the present embodiment antistatic silicone rubber foamed material:
(1) the single tetrafluoroborate ionic liquid of -3 polyethylene glycol of 1- methyl (400) and methanol are sufficiently mixed uniformly,
Antistatic agent mixed solution is made；
(2) antistatic mixed solution is added in precipitated silica and disperses 30min, room temperature in high speed disperser
It places more than for 24 hours；
(3) methyl vinyl silicon kautschuk, hydroxy silicon oil, vinyltriethoxysilane, hard is added in kneader
White carbon black after above-mentioned steps (2) decentralized processing is added portionwise after ester acid zinc, room temperature are kneaded 20min, are warming up to 120 DEG C of mixings
It discharges after 30min；
(4) blowing agent H, blowing agent AC, urea rouge, benzoyl peroxide first is added in above-mentioned steps (3) rubber compound on a mill
Acyl, 2,4- dichlorobenzoperoxide mill are uniform.
(5) extrusion molding carries out post vulcanization (185 DEG C, 2.5h).
Test data
The antistatic silicone rubber foamed material prepared to Examples 1 to 8 and comparative example 1~5 is tested, and test result is such as
Table 1.
Table 1.
In addition to the implementation, the antistatic agent that the present invention can also use are as follows: -3 polyethylene glycol of 1- allyl (200) is double
Limidazolium hexafluorophosphate ionic liquid, the double imidazoles hydrophosphate ionic liquids of -3 polyethylene glycol of 1- allyl (400), 1- methyl -3
Polyethylene glycol (800) list imidazoles trifluoromethanesulfonic acid ionic liquid, -3 polyethylene glycol of 1- butyl (200) double tetrafluoroborates
Ionic liquid, the double imidazoles hydrophosphate ionic liquids of -3 polyethylene glycol of 1- methyl (400), -3 polyethylene glycol of 1- allyl (400)
Double imidazoles cdicynanmide ionic liquids, the double imidazoles cdicynanmide ionic liquids of -3 polyethylene glycol of 1- allyl (400) etc..
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.
Claims (10)
1. a kind of antistatic silicone rubber foamed material, which is characterized in that according to the mass fraction, include following raw material: silicon rubber is raw
80~110 parts of glue, 30~48 parts of filler, 2~10 parts of antistatic agent, 0~3 part of silane coupling agent, 1.5~12 parts of hydroxy silicon oil,
2~10 parts of solvent, 4~10 parts of foaming agent, 2~6 parts of blowing promotor, 0.1~0.5 part of release agent, 0.5~5 part of vulcanizing agent.
2. a kind of antistatic silicone rubber foamed material according to claim 1, which is characterized in that the antistatic agent is
Polyethylene glycol imidazolium ionic liquid, the general structure of the polyethylene glycol imidazolium ionic liquid are as follows:
Wherein X=Br, BF4, PF6, NO3, NO2, SbF6, ZnCl3, SnCl3, SO3, HSO3, H2PO4, CF3CO2, CF3SO3, CH3SO3,
C(CF3SO2)3, N (CF3SO2)2, N (FSO2)2, N (C2F5SO2)2, NTf2；n≥4；R be H or 1~4 carbon atom insatiable hunger and/or
Saturated straight chain or branch chain alkyl.
3. a kind of antistatic silicone rubber foamed material according to claim 2, which is characterized in that the polyethylene glycol imidazoles
The preparation of ionic liquid formula (I) is the following steps are included: imidazoles and monochloro are carried out instead for polyethylene glycol in microwave reactor
It answers, then gained intermediate product polyethylene glycol imidazole radicals chlorate is dissolved into anhydrous second cyanogen solvent, coordination anion is added
It is stirred at room temperature under nitrogen protection after salt and completes ion-exchange reactions, then be evaporated under reduced pressure after being filtered to remove villaumite with diatomite molten
Agent obtains target product.
4. according to a kind of antistatic silicone rubber foamed material as claimed in claim 2, which is characterized in that the polyethylene glycol imidazole salts
The preparation of ionic liquid formula (II) is the following steps are included: being added to imidazoles and both-end chlorinated polyethylene glycol containing dry toluene
In reaction kettle, the lower reaction of argon gas protection generates rufous liquid, takes lower liquid to be washed with ether after cooling, after vacuum drying
To the double imidazole radicals chlorates of polyethylene glycol, the double imidazole radicals chlorates of gained polyethylene glycol are finally dissolved into anhydrous second cyanogen solvent
In, it is stirred at room temperature under nitrogen protection after addition coordination anion salt and completes ion-exchange reactions, then be filtered to remove chlorine with diatomite
It is evaporated under reduced pressure solvent after salt and obtains target product.
5. a kind of antistatic silicone rubber foamed material according to claim 1, which is characterized in that the raw-silastic continuously
For one of methyl vinyl silicon kautschuk, dimethyl silicone rubber raw rubber, methyl phenyl vinyl silicone rubber or a variety of groups
It closes.
6. a kind of antistatic silicone rubber foamed material according to claim 1, which is characterized in that the filler is gas phase
The combination of one or both of method white carbon black, precipitated silica.
7. a kind of antistatic silicone rubber foamed material according to claim 1, which is characterized in that the silane coupling agent
For in vinyltrimethoxysilane, vinyltriethoxysilane, dimethyldimethoxysil,ne, hexamethyldisilazane
One or more combinations；The solvent is one of N-Methyl pyrrolidone, water, methanol, methylene chloride, acetonitrile etc. or more
Kind combination.
8. a kind of antistatic silicone rubber foamed material according to claim 1, which is characterized in that the vulcanizing agent was
Benzoyl Oxide, cumyl peroxide, 2,4- dichlorobenzoperoxide, two (t-butylperoxyisopropyl) benzene, 2,5-
One of bis- (tert-butyl peroxide) hexanes (bis 25 vulcanizing agent) of dimethyl -2,5- or multiple combinations.
9. a kind of antistatic silicone rubber foamed material according to claim 1, which is characterized in that the release agent is hard ester
One of sour calcium, zinc stearate, barium stearate or multiple combinations；The foaming agent is dinitrosopentamethlyene tetramine, idol
The combination of one or both of nitrogen diformamide；Blowing promotor is the combination of one or both of urea rouge, zinc oxide.
10. the preparation method of any one of the described antistatic silicone rubber foamed material of claim 1~9, which is characterized in that including with
Lower step:
(1) first antistatic agent is uniformly mixed with solvent, antistatic agent mixed solution is made；
(2) antistatic mixed solution is placed in high speed disperser with filler and is dispersed, room temperature is above for 24 hours spare；
(3) after raw-silastic continuously, hydroxy silicon oil, silane coupling agent, release agent being added in kneader, then step is added portionwise
(2) filler after decentralized processing is mediated uniformly, and room temperature is kneaded 10~30min, is warming up to 110~130 DEG C of 20~40min of mixing
After discharge；
(4) foaming agent is added in above-mentioned steps (3) rubber compound on a mill and vulcanizing agent mill is uniform；
(5) extrusion molding or compression molding；
(6) post vulcanization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811517417.XA CN109722034A (en) | 2018-12-12 | 2018-12-12 | A kind of antistatic silicone rubber foamed material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811517417.XA CN109722034A (en) | 2018-12-12 | 2018-12-12 | A kind of antistatic silicone rubber foamed material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109722034A true CN109722034A (en) | 2019-05-07 |
Family
ID=66295307
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811517417.XA Pending CN109722034A (en) | 2018-12-12 | 2018-12-12 | A kind of antistatic silicone rubber foamed material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109722034A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375390A (en) * | 2020-10-26 | 2021-02-19 | 东莞怡力精密制造有限公司 | Antistatic silicon rubber material and preparation method thereof |
| CN112457672A (en) * | 2020-11-27 | 2021-03-09 | 合肥艺光高分子材料科技有限公司 | Antistatic foamed silica gel plate composition and foamed silica gel plate production method |
| CN113337118A (en) * | 2021-04-30 | 2021-09-03 | 深圳市飞荣达科技股份有限公司 | Permanent antistatic silica gel and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120038648A (en) * | 2010-10-14 | 2012-04-24 | 한문정 | Antistatic coating composition having matting effect and anti-static property using ionic liquid modified expanded perlite |
| CN105086470A (en) * | 2015-09-11 | 2015-11-25 | 深圳市新纶科技股份有限公司 | Antistatic silicon rubber and preparation method thereof |
| CN105261786A (en) * | 2015-10-09 | 2016-01-20 | 上海应用技术学院 | Novel ionic liquid and preparation method thereof |
| CN106566259A (en) * | 2016-11-07 | 2017-04-19 | 山东非金属材料研究所 | Silicone rubber foaming material and preparation method thereof |
| CN108624063A (en) * | 2018-05-28 | 2018-10-09 | 广东聚合科技股份有限公司 | Sulphurated siliastic and preparation method thereof |
-
2018
- 2018-12-12 CN CN201811517417.XA patent/CN109722034A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120038648A (en) * | 2010-10-14 | 2012-04-24 | 한문정 | Antistatic coating composition having matting effect and anti-static property using ionic liquid modified expanded perlite |
| CN105086470A (en) * | 2015-09-11 | 2015-11-25 | 深圳市新纶科技股份有限公司 | Antistatic silicon rubber and preparation method thereof |
| CN105261786A (en) * | 2015-10-09 | 2016-01-20 | 上海应用技术学院 | Novel ionic liquid and preparation method thereof |
| CN106566259A (en) * | 2016-11-07 | 2017-04-19 | 山东非金属材料研究所 | Silicone rubber foaming material and preparation method thereof |
| CN108624063A (en) * | 2018-05-28 | 2018-10-09 | 广东聚合科技股份有限公司 | Sulphurated siliastic and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 孔萍，等: "《塑料材料》", 31 July 2017, 广东高等教育出版社 * |
| 张凯,等: "抗静电硅橡胶泡沫材料的研制", 《绝缘材料》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112375390A (en) * | 2020-10-26 | 2021-02-19 | 东莞怡力精密制造有限公司 | Antistatic silicon rubber material and preparation method thereof |
| CN112457672A (en) * | 2020-11-27 | 2021-03-09 | 合肥艺光高分子材料科技有限公司 | Antistatic foamed silica gel plate composition and foamed silica gel plate production method |
| CN113337118A (en) * | 2021-04-30 | 2021-09-03 | 深圳市飞荣达科技股份有限公司 | Permanent antistatic silica gel and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105086470B (en) | A kind of antistatic silicone rubber and preparation method thereof | |
| CN109722034A (en) | A kind of antistatic silicone rubber foamed material and preparation method thereof | |
| CN104974530B (en) | A kind of high-performance anti creepage trace silicon rubber and preparation method thereof | |
| CN102010600B (en) | Conductive liquid silicon rubber-based adhesive and preparation method for composition thereof | |
| KR101949224B1 (en) | Composition | |
| CN110300772B (en) | Polyoxazolidinones and process for their preparation | |
| Zhang et al. | Ion conductive characteristics of cross-linked network polysiloxane-based solid polymer electrolytes | |
| KR20150100675A (en) | Polyolefin-based cable compound formulation for improved foamability and enhanced processability | |
| EP3275937B1 (en) | Polyether-based polymer composition | |
| US4801622A (en) | Curable and foamable organopolysiloxane composition | |
| CN109627580A (en) | A kind of light color permanent anti-static modified polypropylene material and preparation method thereof | |
| CN107629190A (en) | Solar insulated water tank modified polyurethane insulation material | |
| CN110922762A (en) | High-conductivity silica gel composition based on conductive powder wet modification technology | |
| CN104844785B (en) | A kind of cationic polymer, preparation method and anion-exchange membrane, preparation method | |
| CN111171687A (en) | Flame-retardant polyurea coating and preparation method thereof | |
| TWI601788B (en) | Thermosetting silicone rubber composition | |
| JPH1192751A (en) | Antistatic agent having excellent heat resistance used for resin, and antistatic resin composition | |
| CN108624063A (en) | Sulphurated siliastic and preparation method thereof | |
| JP2017155399A (en) | Conductive polymer aqueous solution with which fiber is to be impregnated | |
| CN111117209A (en) | Preparation method of polyurethane flame-retardant antistatic composite material | |
| CN108299783A (en) | A kind of high-strength anti-flaming CABLE MATERIALS and preparation method thereof | |
| JP2752904B2 (en) | Method for producing conductive silicone rubber sponge | |
| Lu et al. | The surface modification by carboxyl ionic liquid for mesoporous silica and the preparation of composite polymer electrolyte with the modified mesoporous silica | |
| CN103937031B (en) | Modified zinc borate and preparation method thereof | |
| KR20190026133A (en) | Anion-exchange membrane based on aminated poly(tyrene-ethylene-butylene-styrene) copolymer and manufacturing method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 528400 Torch Development Zone, Guangdong, Zhongshan Province, No. two, No. 1, Jiangxi Road Applicant after: Guangdong poly Technology Co.,Ltd. Address before: 528400 Torch Development Zone, Guangdong, Zhongshan Province, No. two, No. 1, Jiangxi Road Applicant before: Guangdong Polysil Technology Co.,Ltd. |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190507 |