CN103351839A - Single-component deamination-type high-conductivity silicone rubber and preparation method thereof - Google Patents
Single-component deamination-type high-conductivity silicone rubber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses single-component deamination-type high-conductivity silicone rubber and a preparation method thereof. The single-component deamination-type high-conductivity silicone rubber comprises organosilicon base polymers, reinforcement filler, conductive filler, thixotropic agents, plasticizer, crosslinking agents, coupling agents, catalysts, solvent and performance assistant. The preparation method comprises the following steps: firstly performing dehydration to the fillers; then performing planetary stirring to enable a mixture to uniformly dispersed; removing air; packaging in a sealed manner; obtaining the single-component deamination-type high-conductivity silicone rubber. The single-component deamination-type high-conductivity silicone rubber prepared through the preparation method has the advantages of simple curing way, favorable adhesion and simple preparation, is suitable for the operation of a glue dispenser, and is applicable to shielding adhesion in mobile phone base stations, communications and the military industrial field.
Description
Technical field
The present invention relates to a kind of rubber and preparation method thereof, be specifically related to a kind of single component and take off amine type high-conductivity silicon rubber and preparation method thereof.
Background technology
Conductivity silicon rubber is to add electroconductive stuffing in the sizing material of silicon rubber at present, mainly contains carbon black, graphite, metal-powder, alloy, metal oxide, fiber etc.Can add separately, also can be used.
Each class of electronic devices widespread use of high speed development along with modern science and technology, its hertzian wave highlights electronics and people's healthy impact, therefore electromagnetic wave shielding device is widely used in various electronic more, stability and the accuracy requirement of its electromagnetic shielding are also more and more higher, especially stricter, perfect for the shielding requirements of high-precision military project, Aerospace Electronic Equipments, arise at the historic moment as the conductive silicon rubber with good shielding properties.
Main curing system mainly is divided into single component and two-pack, hot setting and self-vulcanizing at present.
As the electric silica gel rubber combination, CN102276988 discloses a kind of single component Ni-C filled-type FIP hot sulfurization high-conductivity silicon rubber and preparation method thereof, it comprises the dimethyl siloxane that 52.5-62.5 part contains the ethenyl blocking of white carbon black, 37.5-47.5 part low viscosity ethenyl blocking dimethyl siloxane, 195-210 part Ni-C conductive filler material.
As the electric silica gel rubber adhesive, CN102807838 discloses a kind of bicomponent normal temperature addition curing electroconductive binder and preparation method thereof, and it comprises the base mateiral of 100 weight parts and the conductive particle of 100-8000 part.
Two kinds of conductive rubbers more than speaking of, a kind of is the two-pack addition curing, has certain part of limitation, namely can not normally solidify after touching the compound that contains N, S, P, Sn, Pb etc.Another kind is bi-component package, is not easy to the point gum machine operation, and often mixing is inhomogeneous on the mixed gluing equipment of a lot of two-packs, needs debugging, and waste is a lot.
For conductive silicon rubber, curing mode is simple, i.e. self-vulcanizing; Easy to operate, be fit to machine point glue, i.e. single-component package; Solidified nature is good, not affected by contactant, and namely catalyzer can not poisoned; The conductive silicon rubber that cementability is good is that a difficult point, particularly single component are taken off amine type conductive resin and rarely had report always.
Summary of the invention
The object of the invention is to, provide a kind of single component to take off amine type high-conductivity silicon rubber and preparation method thereof, to overcome the existing above-mentioned shortcoming and defect of prior art, filled up the blank in interior market.
The technical problem that will solve required for the present invention can be achieved through the following technical solutions:
As a first aspect of the present invention, single component is taken off amine type high-conductivity silicon rubber, it is characterized in that, according to the mass fraction, comprising: conductive resin intermediate, conductive filler material, amido linking agent, coupling agent, catalysts and solvents comprise following component:
The conduction intermediate of 20-50 part,
The conductive filler material of 30-70 part,
0.05-1 the amido linking agent of part,
0.01-1 the coupling agent of part,
0.01-1 part catalyzer,
5-20 part solvent;
Wherein, the conductive resin intermediate comprises:
The organosilicon base polymer of 10-40 part,
The softening agent of 0-2 part,
The reinforced filling of 10-40 part,
The thixotropic agent of 0-2 part,
The performance auxiliary agent of 0-1 part.
Further, described organosilicon base polymer is any one or the combination in hydroxyl-terminated injecting two methyl siloxane, trimethoxy end-blocking polydimethylsiloxane, triethoxy end-blocking polydimethylsiloxane, vinyl-dimethyl oxygen base end-blocking polydimethylsiloxane, divinyl methoxyl group end-blocking polydimethylsiloxane, vinyl diethoxy end-blocking polydimethylsiloxane, the divinyl oxyethyl group end-blocking polydimethylsiloxane, and its basic structure is shown below:
Further, described softening agent is any one or the combination in methyl-silicone oil, hexamethyl cyclotrisiloxane, the octamethylcyclotetrasiloxane.
Further, described reinforced filling is nano-calcium carbonate, silicon powder, MQ resin, carbon black, white carbon black, any one in the mica powder or combination.
Further, described thixotropic agent is the polymeric amide thixotropic agent, carbon black, white carbon black, polyoxyethylene glycol, pure aluminium silicate, hydrogenated castor oil, any one in the organobentonite or combination.
Further, described performance auxiliary agent is any one or the combination in hexamethyldisilazane, vinyltrimethoxy silane, isocyanates silane coupling agent, oxazole alkanes coupling agent, black slurry, the titanium dioxide.
Further, described conductive filler material is any one or the combination in aluminium powder, silver powder, copper powder, bronze, nickel powder, silver coated aluminum powder, silver-coated copper powder, silver coated nickel powder, nickel bag graphite, the graphitized carbon black.
Further, described amido linking agent is any one or the combination in methyl tricyclohexyltin amine base silane, vinyl tricyclohexyltin amine base silane, methyl three (methyl-propyl) amino containing silane, vinyl three (methyl-propyl) amino containing silane, methyl three positive definite amino containing silanes, vinyl three positive definite amino containing silanes, the methyl tri-isopropyl amine base silane.
Further, described coupling agent agent is any one or combination of γ-aminopropyl triethoxysilane, N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-aminopropyltrimethoxysilane, gamma-methyl allyl acyloxypropyl trimethoxysilane.
Further, described catalyzer is any one in dibutyltin diacetate, oxalic acid dioctyl tin, two sad dibutyl tins, stannous octoate, tin acetate, dibutyl tin laurate and the organic tin compound.
Further, described solvent is any one in acetone, butanone, toluene, dimethylbenzene, sherwood oil, hexamethyl cyclotrisiloxane, octamethylcyclotetrasiloxane, methylene dichloride, the tetrahydrofuran (THF).
As a second aspect of the present invention, single component is taken off the preparation method of amine type high-conductivity silicon rubber, it is characterized in that, may further comprise the steps:
(1) first with the 70 ℃ of baking 24 hours in vacuum drying oven of reinforced filling and conductive filler material;
(2) after then order adds organosilicon base polymer, softening agent, reinforced filling, thixotropic agent, performance auxiliary agent in the twin shaft planet stirring still in order, blend is 10～15 minutes under vacuum protection, then be warmed up to 100～120 ℃ of lower vacuum protection blend 1 hour, the vacuum protection borehole cooling namely obtains the conductive resin intermediate to room temperature;
(3) add conductive filler material after intermediate is cooled to room temperature, blend is 20～30 minutes under vacuum protection, then adds amido linking agent, coupling agent, catalyzer, vacuum stirring 20 minutes,
(4) add at last solvent, vacuum stirring packed and namely gets single component and take off amine type high-conductivity silicon rubber in 5 minutes.
Beneficial effect of the present invention:
The single component of the present invention preparation is taken off amine type high-conductivity silicon rubber, have that curing mode is simple, convenience point glue machine operation, bonding good, prepare simple advantage.
The shielding of product suitable cellular base station, communication and the military industry field of the present invention's preparation is bonding, especially relates to conduction is required higher field, and perhaps requirement has the communication apparatus of the performance of electromagnetic shielding.
Embodiment
Below in conjunction with specific embodiment, the present invention is done progressive explanation.Should be understood that following examples are only for explanation the present invention but not for limiting scope of the present invention.
Embodiment 1
Single component is taken off the prescription of amine type high-conductivity silicon rubber, calculates according to parts by weight, comprises following component:
The conductive resin intermediate:
10 parts hydroxyl-terminated injecting two methyl siloxane
0.3 the dimethyl silicone oil of part
12 parts nano-calcium carbonate
0.03 the white carbon black of part
0.02 the hexamethyldisilazane of part
Single component is taken off amine type high-conductivity silicon rubber:
21 parts conduction intermediate
68 parts silver-plated nickel powder
0.08 the methyl tricyclohexyltin amine base silane of part
0.01 the γ-aminopropyl triethoxysilane of part
0.01 part dibutyl tin laurate
10.9 part sherwood oil
Obtain tensile strength greater than 2.0MPa, unit elongation is greater than 50%, and Shao A hardness is 71, and volume specific resistance is that the single component of 6.7m Ω .cm is taken off amine type high-conductivity silicon rubber.
Embodiment 2
Single component is taken off the prescription of amine type high-conductivity silicon rubber, calculates according to parts by weight, comprises following component:
The conductive resin intermediate:
15 parts hydroxyl-terminated injecting two methyl siloxane
0.1 the octamethylcyclotetrasiloxane of part
10 parts silicon powder
0.03 the white carbon black of part
0.02 the vinyltrimethoxy silane of part
Single component is taken off amine type high-conductivity silicon rubber:
32 parts conduction intermediate
54 parts nickel bag graphite
0.08 methyl three (methyl-propyl) amino containing silane of part
0.01 the γ-aminopropyl triethoxysilane of part
0.01 part dibutyl tin laurate
13.9 part toluene
Obtain tensile strength greater than 1.5MPa, unit elongation is greater than 150%, and Shao A hardness is 60, and volume specific resistance is that the single component of 15m Ω .cm is taken off amine type high-conductivity silicon rubber.
Embodiment 3
Single component is taken off the prescription of amine type high-conductivity silicon rubber, calculates according to parts by weight, comprises following component:
The conductive resin intermediate:
20 parts trimethoxy end-blocking polydimethylsiloxane
1 part dimethyl silicone oil
18 parts nano-calcium carbonate
0.8 the white carbon black of part
0.02 the hexamethyldisilazane of part
Single component is taken off amine type high-conductivity silicon rubber:
20 parts conduction intermediate
65 parts silver-plated copper powder
0.1 the methyl tricyclohexyltin amine base silane of part
0.01 the γ-aminopropyl triethoxysilane of part
0.01 part tin acetate
14.88 part dimethylbenzene
Obtain tensile strength greater than 1.8MPa, unit elongation is greater than 70%, and Shao A hardness is 68, and volume specific resistance is that the single component of 7.8m Ω .cm is taken off amine type high-conductivity silicon rubber.
Embodiment 4
Single component is taken off the prescription of amine type high-conductivity silicon rubber, calculates according to parts by weight, comprises following component:
The conductive resin intermediate:
14 parts hydroxyl-terminated injecting two methyl siloxane
0.3 the dimethyl silicone oil of part
10 parts nano-calcium carbonate
0.03 the white carbon black of part
0.02 the titanium dioxide of part
Single component is taken off amine type high-conductivity silicon rubber:
30 parts conduction intermediate
58 parts silver powder
0.08 methyl three (methyl-propyl) amino containing silane of part
0.01 the γ-aminopropyl triethoxysilane of part
0.01 part dibutyl tin laurate
11.9 part dimethylbenzene
Obtain tensile strength greater than 1.6MPa, unit elongation is greater than 80%, and Shao A hardness is 70, and volume specific resistance is that the single component of 5.3m Ω .cm is taken off amine type high-conductivity silicon rubber.
Comparative Examples 1
Single-component de-alcoholized conductive silicon rubber:
100 parts hydroxyl-terminated injecting two methyl siloxane
20 parts nano-calcium carbonate
330 parts silver-plated copper powder
3 parts vinyltrimethoxy silane
5 parts methyl triethoxy base silane
1 part N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane
3 parts tetrabutyl titanate
62 parts of dimethylbenzene
Obtain tensile strength greater than 1.1MPa, unit elongation is greater than 30%, and Shao A hardness is 75, and volume specific resistance is that the single component of 9.6m Ω .cm is taken off amine type high-conductivity silicon rubber.
Comparative Examples 2
The bi-component addition type conductive silicon rubber:
Conductive resin first component:
50 parts vinyl silicone oil (viscosity 1000cps)
5 parts containing hydrogen silicone oil (hydrogen content 0.3%)
155 parts silver powder
20 parts of silicon powders
30 parts sherwood oil
Conductive resin second component:
50 parts vinyl silicone oil (viscosity 1000cps)
5 parts containing hydrogen silicone oil (hydrogen content 0.3%)
175 parts silver powder
1.1 the platinum catalyst of part
30 parts sherwood oil
Blending ratio first component: second component=1:1
Obtain tensile strength greater than 0.3MPa, unit elongation is greater than 20%, and Shao A hardness is 74, and volume specific resistance is the bi-component addition type conductive silicon rubber of 3.6m Ω .cm.
To embodiment 1, embodiment 2, embodiment 3, embodiment 4, Comparative Examples 1, Comparative Examples 2, adopt testing method, tested its performance.
Volume specific resistance ASTM D991.
Anti-poisoning testing method:
(1) with the room temperature spontaneous curing in plastic cup of a conductive resin part, another part is coated on the wiring board of solder joint, self-vulcanizing 7 days;
(2) test its hardness with Shao A sclerometer behind the completion of cure;
(3) consistent if in hardness that solder joint solidifies and plastic cup, solidify hardness, illustrate and do not poison; If do not solidify or poorer than solidifying the anti-toxic of the obvious explanation on the low side of hardness in the plastic cup.
The peel test force method:
(1) conductive resin evenly is coated on the wide plastics film of two 1cm self-vulcanizing 7 days;
The plastics film two ends that (2) will glue conductive resin are fixed on the digital display puller system maximum pull that testing film is broken.
The result is as shown in table 1.
The detection of table 1 product
As can be seen from Table 1, use cementability of the present invention good, contact with wiring board and do not poison.Preferred prescription is embodiment 1.
The present invention compared with prior art, electroconductibility, capability of electromagnetic shielding are excellent, cementability is good, cost is moderate, the shielding that is fit to cellular base station, communication and military industry field is bonding.
More than the specific embodiment of the present invention is illustrated, but the present invention is as limit, only otherwise break away from aim of the present invention, the present invention can also have various variations.
Claims (12)
1. a single component is taken off amine type high-conductivity silicon rubber, it is characterized in that, according to the mass fraction, comprising: conductive resin intermediate, conductive filler material, amido linking agent, coupling agent, catalysts and solvents comprise following component:
The conduction intermediate of 20-50 part,
The conductive filler material of 30-70 part,
0.05-1 the amido linking agent of part,
0.01-1 the coupling agent of part,
0.01-1 part catalyzer,
5-20 part solvent;
Wherein, the conductive resin intermediate comprises:
The organosilicon base polymer of 10-40 part,
The softening agent of 0-2 part,
The reinforced filling of 10-40 part,
The thixotropic agent of 0-2 part,
The performance auxiliary agent of 0-1 part.
2. single component according to claim 1 is taken off amine type high-conductivity silicon rubber, it is characterized in that: described organosilicon base polymer is any one or the combination in hydroxyl-terminated injecting two methyl siloxane, trimethoxy end-blocking polydimethylsiloxane, triethoxy end-blocking polydimethylsiloxane, vinyl-dimethyl oxygen base end-blocking polydimethylsiloxane, divinyl methoxyl group end-blocking polydimethylsiloxane, vinyl diethoxy end-blocking polydimethylsiloxane, the divinyl oxyethyl group end-blocking polydimethylsiloxane, and its basic structure is shown below:
3. single component according to claim 1 is taken off amine type high-conductivity silicon rubber, it is characterized in that: described softening agent is any one or the combination in methyl-silicone oil, hexamethyl cyclotrisiloxane, the octamethylcyclotetrasiloxane.
4. single component according to claim 1 is taken off amine type high-conductivity silicon rubber, it is characterized in that: described reinforced filling is nano-calcium carbonate, silicon powder, MQ resin, carbon black, white carbon black, any one in the mica powder or combination.
5. single component according to claim 1 is taken off amine type high-conductivity silicon rubber, it is characterized in that: described thixotropic agent is the polymeric amide thixotropic agent, carbon black, white carbon black, polyoxyethylene glycol, pure aluminium silicate, hydrogenated castor oil, any one in the organobentonite or combination.
6. single component according to claim 1 is taken off amine type high-conductivity silicon rubber, it is characterized in that: described performance auxiliary agent is any one or the combination in hexamethyldisilazane, vinyltrimethoxy silane, isocyanates silane coupling agent, oxazole alkanes coupling agent, black slurry, the titanium dioxide.
7. single component according to claim 1 is taken off amine type high-conductivity silicon rubber, it is characterized in that: described conductive filler material is any one or the combination in aluminium powder, silver powder, copper powder, bronze, nickel powder, silver coated aluminum powder, silver-coated copper powder, silver coated nickel powder, nickel bag graphite, the graphitized carbon black.
8. single component according to claim 1 is taken off amine type high-conductivity silicon rubber, it is characterized in that: described amido linking agent is any one or the combination in methyl tricyclohexyltin amine base silane, vinyl tricyclohexyltin amine base silane, methyl three (methyl-propyl) amino containing silane, vinyl three (methyl-propyl) amino containing silane, methyl three positive definite amino containing silanes, vinyl three positive definite amino containing silanes, the methyl tri-isopropyl amine base silane.
9. single component according to claim 1 is taken off amine type high-conductivity silicon rubber, it is characterized in that: described coupling agent agent is any one or combination of γ-aminopropyl triethoxysilane, N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-aminopropyltrimethoxysilane, gamma-methyl allyl acyloxypropyl trimethoxysilane.
10. single component according to claim 1 is taken off amine type high-conductivity silicon rubber, it is characterized in that: described catalyzer is any one in dibutyltin diacetate, oxalic acid dioctyl tin, two sad dibutyl tins, stannous octoate, tin acetate, dibutyl tin laurate and the organic tin compound.
11. single component according to claim 1 is taken off amine type high-conductivity silicon rubber, it is characterized in that: described solvent is any one in acetone, butanone, toluene, dimethylbenzene, sherwood oil, hexamethyl cyclotrisiloxane, octamethylcyclotetrasiloxane, methylene dichloride, the tetrahydrofuran (THF).
12. a single component as claimed in claim 1 is taken off the preparation method of amine type high-conductivity silicon rubber, it is characterized in that, may further comprise the steps:
(1) first with the 70 ℃ of baking 24 hours in vacuum drying oven of reinforced filling and conductive filler material;
(2) after then order adds organosilicon base polymer, softening agent, reinforced filling, thixotropic agent, performance auxiliary agent in the twin shaft planet stirring still in order, blend is 10～15 minutes under vacuum protection, then be warmed up to 100～120 ℃ of lower vacuum protection blend 1 hour, the vacuum protection borehole cooling namely obtains the conductive resin intermediate to room temperature;
(3) add conductive filler material after intermediate is cooled to room temperature, blend is 20～30 minutes under vacuum protection, then adds amido linking agent, coupling agent, catalyzer, vacuum stirring 20 minutes,
(4) add at last solvent, vacuum stirring packed and namely gets single component and take off amine type high-conductivity silicon rubber in 5 minutes.
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| CN105176481A (en) * | 2015-10-08 | 2015-12-23 | 中国航空工业集团公司北京航空材料研究院 | High-conductivity organosilicone sealant based on single-component room temperature curing condensation and preparation method of high-conductivity organosilicone sealant |
| CN107880429A (en) * | 2013-12-25 | 2018-04-06 | 江苏亨通线缆科技有限公司 | The communications cable with function of shielding |
| CN108624055A (en) * | 2018-04-13 | 2018-10-09 | 苏州佳值电子工业有限公司 | Antistatic silica gel and use for electronic products gasket based on electrostatic protection |
| CN108641668A (en) * | 2018-05-31 | 2018-10-12 | 苏州瑞力博新材科技有限公司 | A kind of low silver content condensed type organic silicon conducting resinl and preparation method thereof |
| CN112708392A (en) * | 2020-12-25 | 2021-04-27 | 深圳德邦界面材料有限公司 | Low-volatility high-shielding silver-nickel conductive adhesive and preparation method thereof |
| CN112852342A (en) * | 2021-01-08 | 2021-05-28 | 深圳市维美德材料科技有限公司 | Super-soft conductive adhesive for 5G frequency spectrum and preparation method thereof |
| CN112940673A (en) * | 2021-03-05 | 2021-06-11 | 上海锐朗光电材料有限公司 | Single-component dealcoholized organosilicon conductive adhesive and preparation method thereof |
| CN114805426A (en) * | 2022-01-07 | 2022-07-29 | 山东硅科新材料有限公司 | Modified vinyl silane and preparation method and application thereof |
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| CN107880429A (en) * | 2013-12-25 | 2018-04-06 | 江苏亨通线缆科技有限公司 | The communications cable with function of shielding |
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| CN108624055A (en) * | 2018-04-13 | 2018-10-09 | 苏州佳值电子工业有限公司 | Antistatic silica gel and use for electronic products gasket based on electrostatic protection |
| CN108641668A (en) * | 2018-05-31 | 2018-10-12 | 苏州瑞力博新材科技有限公司 | A kind of low silver content condensed type organic silicon conducting resinl and preparation method thereof |
| CN108641668B (en) * | 2018-05-31 | 2020-11-20 | 苏州瑞力博新材科技有限公司 | Low-silver-content condensed type organic silicon conductive adhesive and preparation method thereof |
| CN112708392A (en) * | 2020-12-25 | 2021-04-27 | 深圳德邦界面材料有限公司 | Low-volatility high-shielding silver-nickel conductive adhesive and preparation method thereof |
| CN112852342A (en) * | 2021-01-08 | 2021-05-28 | 深圳市维美德材料科技有限公司 | Super-soft conductive adhesive for 5G frequency spectrum and preparation method thereof |
| CN112940673A (en) * | 2021-03-05 | 2021-06-11 | 上海锐朗光电材料有限公司 | Single-component dealcoholized organosilicon conductive adhesive and preparation method thereof |
| CN114805426A (en) * | 2022-01-07 | 2022-07-29 | 山东硅科新材料有限公司 | Modified vinyl silane and preparation method and application thereof |
| CN114805426B (en) * | 2022-01-07 | 2024-03-19 | 山东硅科新材料有限公司 | Modified vinyl silane and preparation method and application thereof |
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Application publication date: 20131016 |