CN112646377A - Conductive silicone rubber for electromagnetic shielding and preparation method thereof - Google Patents
Conductive silicone rubber for electromagnetic shielding and preparation method thereof Download PDFInfo
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- CN112646377A CN112646377A CN202011556627.7A CN202011556627A CN112646377A CN 112646377 A CN112646377 A CN 112646377A CN 202011556627 A CN202011556627 A CN 202011556627A CN 112646377 A CN112646377 A CN 112646377A
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 128
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011231 conductive filler Substances 0.000 claims abstract description 62
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000007822 coupling agent Substances 0.000 claims abstract description 50
- 239000000463 material Substances 0.000 claims abstract description 46
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 37
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 34
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 23
- 229920002545 silicone oil Polymers 0.000 claims abstract description 21
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 17
- 239000004014 plasticizer Substances 0.000 claims abstract description 17
- 239000004595 color masterbatch Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 229920001971 elastomer Polymers 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 25
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 16
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- 229920005560 fluorosilicone rubber Polymers 0.000 claims description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 8
- 229920002554 vinyl polymer Polymers 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical group C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 5
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical group CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical group CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000003365 glass fiber Substances 0.000 claims description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical group [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 2
- 150000003376 silicon Chemical class 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 7
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- -1 methyl vinyl Chemical group 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000003712 anti-aging effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The application relates to the technical field of electromagnetic shielding materials, and provides conductive silicone rubber for electromagnetic shielding and a preparation method thereof. The raw materials of the conductive silicone rubber for electromagnetic shielding comprise: 100 parts of silicon rubber, 300 parts of conductive filler 250-containing silica, 6-8 parts of fumed silica, 4-16 parts of coupling agent, 20-30 parts of color master batch, 2-4 parts of cross-linking agent, 4-6 parts of hydroxyl silicone oil, 2-4 parts of plasticizer, 1-3 parts of vulcanizing agent and 0-1 part of release agent. In the formula, each 100 parts of silicone rubber is compounded with more than 200 parts of conductive filler, and simultaneously, 4-16 parts of coupling agent and 6-8 parts of fumed silica are added, so that the synergistic effect of the raw materials ensures the excellent conductivity and aging resistance of the conductive silicone rubber, effectively enhances the magnetic conductivity of the material, and improves the mechanical property of the material to a certain extent, so that the good strength and toughness of the material can meet the application requirements of the material.
Description
Technical Field
The application belongs to the technical field of electromagnetic shielding materials, and particularly relates to conductive silicone rubber for electromagnetic shielding and a preparation method thereof.
Background
With the rapid development of the electronic information era and the technological progress, electronic products are more and more widely used. Many wireless communication devices and electronic devices inevitably bring a lot of electromagnetic pollution due to electromagnetic leakage, and the problem of electromagnetic interference mainly includes the following points: 1. affecting the normal operation of the electronic equipment; 2. electromagnetic information leakage; 3. electromagnetic environmental pollution. In order to solve these problems, the use of electromagnetic shielding materials can be effectively suppressed, and thus, the development of electromagnetic shielding materials having good electromagnetic shielding properties has been the focus of research by those skilled in the art.
The conductive silicone rubber is one of common electromagnetic shielding materials, and is an elastomer which is prepared by filling a certain amount of conductive filler, pigment filler and other additives into silicone rubber by taking the silicone rubber as a base material, uniformly dispersing and then crosslinking through a certain chemical reaction. However, due to the difference in polarity, there is poor interface compatibility between the silicone rubber and the filler, which results in a limited increase in the electromagnetic shielding performance and mechanical properties of the conductive silicone rubber.
Disclosure of Invention
The application aims to provide the conductive silicone rubber for electromagnetic shielding, and aims to solve the problem that poor interface compatibility exists between silicone rubber and a filler in an existing conductive silicone rubber system, so that the increase degree of the electromagnetic shielding performance and the mechanical performance of the conductive silicone rubber is limited.
Further, the application also provides a preparation method of the conductive silicone rubber for electromagnetic shielding.
The technical scheme adopted by the application is as follows:
in a first aspect, the present application provides an electromagnetic shielding conductive silicone rubber, which comprises the following raw materials in parts by weight:
the conductive silicone rubber for electromagnetic shielding is prepared from silicone rubber, conductive filler, fumed silica, a coupling agent, a color master, a cross-linking agent, hydroxyl silicone oil, a plasticizer, a vulcanizing agent and a release agent, wherein each 100 parts of silicone rubber is compounded with more than 200 parts of conductive filler, and simultaneously 4-16 parts of the coupling agent and 6-8 parts of fumed silica are added.
In a second aspect, the present application provides a method for preparing a conductive silicone rubber for electromagnetic shielding, comprising the following steps:
the conductive silicone rubber for electromagnetic shielding is prepared from the following raw materials: silicon rubber, conductive filler, fumed silica, a coupling agent, color master batch, a cross-linking agent, hydroxyl silicone oil, a plasticizer, a vulcanizing agent and a release agent;
reacting the conductive filler with a portion of the coupling agent to form a modified conductive filler;
reacting the fumed silica with the rest of the coupling agent to form modified fumed silica;
mixing the silicon rubber, the modified fumed silica and the modified conductive filler to obtain a first rubber material;
mixing the first rubber material with the color master, the hydroxyl silicone oil, the plasticizer and the release agent to obtain a second rubber material;
and mixing the second rubber compound with the cross-linking agent and the vulcanizing agent.
According to the preparation method provided by the application, the conductive filler and the fumed silica respectively react with the coupling agent to perform surface modification before mixing, so that the interface compatibility of the conductive filler and the fumed silica with the silicone rubber is effectively improved, the using amount of the conductive filler compounded with the silicone rubber is obviously increased, the magnetic conductivity of the conductive silicone rubber is effectively enhanced, and the material has good electromagnetic shielding performance from 200KHz to 10GHz frequency bands; in addition, the mechanical property of the material is improved to a certain extent, so that the material has good strength, toughness, wear resistance and ageing resistance, and can meet the application requirements of the material. The method is simple, is simple and convenient to operate, and can realize large-scale preparation of the conductive silicone rubber for electromagnetic shielding.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application more clearly apparent, the present application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.
The terms "first", "second" and "first" are used for descriptive purposes only and are used for distinguishing purposes such as substances from one another, and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated, and features defined as "first" and "second" may explicitly or implicitly include one or more such features.
The embodiment of the application provides conductive silicone rubber for electromagnetic shielding, which comprises the following components in parts by weight:
the conductive silicone rubber for electromagnetic shielding provided by the embodiment of the application takes silicone rubber, conductive filler, fumed silica, a coupling agent, color master, a cross-linking agent, hydroxyl silicone oil, a plasticizer, a vulcanizing agent and a release agent as raw materials, more than 200 parts of conductive filler is compounded in every 100 parts of silicone rubber, and 4-16 parts of coupling agent and 6-8 parts of fumed silica are added at the same time, and the raw materials have synergistic effect, so that the excellent conductive performance and aging resistance of the conductive silicone rubber are ensured, the magnetic conductivity of the material is effectively enhanced, the material has good electromagnetic shielding performance from a 200KHz frequency band to a 10GHz frequency band, the conductive silicone rubber can be applied to the field of electromagnetic compatibility (EMC), the mechanical property of the material is improved to a certain extent, and the good strength and toughness of the material can meet the application requirements of the material.
Particularly, the silicon rubber is used as a substrate, and good mechanical property and weather resistance are provided for the conductive silicon rubber.
In some embodiments, the silicone rubber is a mixture of methyl vinyl silicone rubber and fluorosilicone rubber, and the weight of the fluorosilicone rubber is 0-50% of the total mass of the silicone rubber. The natural silicon rubber has generally poor ageing resistance, and the methyl vinyl silicon rubber and the fluorosilicone rubber are mixed in proportion, so that the anti-aging silicon rubber has excellent ageing resistance and conductivity, can meet various application requirements of the conductive silicon rubber, is favorable for reducing cost and improving processability.
In order to further improve the mechanical property and the weather resistance of the conductive silicone rubber, the applicant further optimizes the specific composition of the silicone rubber. In one embodiment, the silicone rubber is composed of methyl vinyl silicone rubber having a vinyl content of 0.03% to 0.06% and methyl vinyl silicone rubber having a vinyl content of 0.13% to 0.2%. In another embodiment, the silicone rubber is composed of methyl vinyl silicone rubber having a vinyl content of 0.03% to 0.06% and fluorinated silicone rubber. In yet another embodiment, the silicone rubber is a methyl vinyl silicone rubber having a vinyl content of 0.03% to 0.06%. By adjusting the silicone rubber to be the specific composition, the conductive silicone rubber has optimal mechanical properties and weather resistance, and is favorable for further improving the interface compatibility of the silicone rubber with the conductive filler and the fumed silica, so that the electromagnetic shielding performance of the material is improved.
The conductive filler provides conductive performance and magnetic conductivity for the conductive silicone rubber, and on the basis of 100 parts of the silicone rubber, the amount of the conductive filler is 250-300 parts, specifically 250 parts, 260 parts, 270 parts, 280 parts, 290 parts or 300 parts.
In some embodiments, the conductive filler is selected from at least one of silver-plated aluminum powder, silver-plated copper powder, silver-plated nickel powder, silver-plated glass fiber, and silver particles. The conductive fillers have good conductive performance and magnetic conductivity, have good mixing performance with silicon rubber, particularly methyl vinyl silicone rubber and fluorine silicone rubber, and are beneficial to improving the filling amount of the conductive fillers in the silicon rubber, so that the electromagnetic performance of the conductive silicon rubber is further improved. In a further embodiment, the conductive filler is silver-plated aluminum powder, the average particle size of the silver-plated aluminum powder is 35-45 μm, the silver-plated aluminum powder is aluminum powder with a silver layer plated on the surface, the aluminum powder is composed of aluminum and carbon, and the aluminum accounts for 75-85% by weight. The conductive filler is filled in silicon rubber, particularly methyl vinyl silicon rubber and fluorine silicon rubber, so that the conductive silicon rubber has excellent electromagnetic performance.
The fumed silica is used for improving the mechanical strength, the wear resistance and the aging resistance of the conductive silicone rubber, and the fumed silica has good adsorption capacity, so that the uniform mixing degree of all raw materials in the formula can be improved to a certain degree. Based on 100 parts of silicon rubber, the amount of the fumed silica is 6-8 parts, specifically 6 parts, 6.5 parts, 7 parts, 7.5 parts or 8 parts.
The coupling agent is used for modifying the conductive filler and the fumed silica so as to improve the interface compatibility of the silicone rubber with the conductive filler and the fumed silica, so that the using amount of the conductive filler can be obviously increased to more than 250 parts, and the electromagnetic performance of the conductive silicone rubber is enhanced. The amount of the coupling agent is 4-16 parts, specifically 4 parts, 6 parts, 8 parts, 10 parts, 12 parts, 14 parts or 16 parts, based on 100 parts of the silicone rubber.
In some embodiments, the coupling agent is vinyltriethoxysilane. The coupling agent has good reactivity with the conductive filler and the fumed silica, and is beneficial to improving the electromagnetic property of the conductive silicone rubber. In a specific embodiment, the coupling agent is selected as coupling agent A151.
The color master batch is used for adjusting the color of the conductive silicone rubber, and the amount of the color master batch is 20-30 parts on the basis of 100 parts of the silicone rubber, specifically 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts or 30 parts. The type of the color masterbatch can be flexibly adjusted according to the application requirements of the prepared conductive silicone rubber, and the embodiment of the application is not particularly limited.
The hydroxyl silicone oil is used as a structure control agent for forming the conductive silicone rubber, and the dosage of the hydroxyl silicone oil is 4-6 parts, specifically 4 parts, 4.5 parts, 5 parts, 5.5 parts or 6 parts on the basis of 100 parts of the dosage of the silicone rubber. In some embodiments, the hydroxy silicone oil has a hydroxyl content of 6% to 8%. The hydroxyl silicone oil has good compatibility with silicone rubber, particularly methyl vinyl silicone rubber and fluorine silicone rubber, and is beneficial to further improving the product performance.
The cross-linking agent, the plasticizer, the vulcanizing agent and the release agent are used as auxiliary agents for forming the conductive silicone rubber, so that the processing performance of the conductive silicone rubber is improved on the premise of ensuring the conductivity and the excellent anti-aging performance of the conductive silicone rubber. Based on 100 parts of the silicon rubber, 2-4 parts of a cross-linking agent, specifically 2 parts, 2.5 parts, 3 parts, 3.5 parts or 4 parts; 2-4 parts of a plasticizer, specifically 2 parts, 2.5 parts, 3 parts, 3.5 parts or 4 parts; 1-3 parts of vulcanizing agent, specifically 1 part, 1.5 parts, 2 parts, 2.5 parts or 3 parts; 0-1 part of release agent, specifically 0.2 part, 0.5 part, 0.7 part, 0.9 part or 1 part. In some embodiments, the coupling agent is vinyltriethoxysilane, the crosslinking agent is triallyl isocyanurate, the vulcanizing agent is bis-penta, the release agent is zinc stearate, and the plasticizer is acetyl tributyl citrate. Thus, the processing performance of the conductive silicone rubber is improved to the maximum extent, and the excellent conductive performance of the material is kept.
In order to prepare the conductive silicone rubber for electromagnetic shielding, the embodiment of the application provides a preparation method of the conductive silicone rubber for electromagnetic shielding, and the preparation method comprises the following steps:
s01, providing raw materials according to the conductive silicone rubber for electromagnetic shielding: silicon rubber, conductive filler, fumed silica, a coupling agent, color master batch, a cross-linking agent, hydroxyl silicone oil, a plasticizer, a vulcanizing agent and a release agent;
s02, reacting the conductive filler with a part of coupling agent to form modified conductive filler;
s03, reacting the fumed silica with the residual coupling agent to form modified fumed silica;
s04, mixing the silicon rubber, the modified fumed silica and the modified conductive filler to obtain a first rubber material;
s05, mixing the first rubber material with color master, hydroxyl silicone oil, a plasticizer and a release agent to obtain a second rubber material;
and S06, mixing the second rubber compound with a crosslinking agent and a vulcanizing agent.
According to the preparation method provided by the embodiment of the application, the conductive filler and the fumed silica are respectively reacted with the coupling agent to carry out surface modification before mixing, so that the interface compatibility of the conductive filler and the fumed silica with the silicone rubber is effectively improved, the using amount of the conductive filler compounded with the silicone rubber is obviously increased, the magnetic conductivity of the conductive silicone rubber is effectively enhanced, and the material has good electromagnetic shielding performance from 200KHz to 10GHz frequency bands; in addition, the mechanical property of the material is improved to a certain extent, so that the material has good strength, toughness, wear resistance and ageing resistance, and can meet the application requirements of the material. The method is simple, is simple and convenient to operate, and can realize large-scale preparation of the conductive silicone rubber for electromagnetic shielding.
The types, the amounts and the effects of the silicone rubber, the conductive filler, the fumed silica, the coupling agent, the color master, the crosslinking agent, the hydroxyl silicone oil, the plasticizer, the vulcanizing agent and the release agent in the step S01 are basically the same as those described above, and are not repeated here for saving space.
In step S02, the conductive filler and a portion of the coupling agent are reacted so that the coupling agent surface modifies the conductive filler to obtain a modified conductive filler.
In some embodiments, the step of reacting fumed silica and a portion of the coupling agent comprises: stirring at 1000 and 1500rpm for 1-5 min. In the specific embodiment, fumed silica and part of the coupling agent are stirred for 3min at 1200rpm in a high-speed planetary stirrer.
In step S03, the fumed silica and the remaining coupling agent are reacted to modify the fumed silica on the surface of the coupling agent, so as to obtain the modified fumed silica.
In some embodiments, the step of reacting the electrically conductive filler and the remaining coupling agent comprises: stirring at 1000 and 1500rpm for 1-5 min. In a specific example, the conductive filler and the remaining coupling agent were stirred in a high speed planetary mixer at 1200rpm for 3 min.
In some embodiments, the weight ratio of the coupling agent in the step of reacting fumed silica and a portion of the coupling agent to the coupling agent in the step of reacting the conductive filler and the remaining coupling agent is (4-6): (8-10).
In step S04, the silicone rubber, the modified fumed silica, and the modified conductive filler are mixed, so that the modified fumed silica and the modified conductive filler are fully and uniformly filled in the silicone rubber.
In order to promote more uniform filling of the modified fumed silica and the modified conductive filler in the silicone rubber, preferably, the modified fumed silica and the modified conductive filler are mixed with the silicone rubber in sequence. In some embodiments, the modified fumed silica is added to the silicone rubber in batches and mixed for 10min at a rotating speed of 10-15rpm, and then the modified conductive filler is added in batches and mixed for 10min at a rotating speed of 10-15 rpm.
The mixing may be carried out by conventional mixing techniques in the art, such as in some embodiments, in an open mill.
In step S05, the first rubber compound is mixed with the color masterbatch, the hydroxyl silicone oil, the plasticizer, and the release agent, so that the color masterbatch, the hydroxyl silicone oil, the plasticizer, and the release agent are uniformly dispersed in the first rubber compound.
In some embodiments, the primary compound is mixed with color masterbatch, hydroxyl silicone oil, plasticizer, and mold release agent in an open mill for 10min at 12-15 rpm.
In step S06, the second compound is mixed with the crosslinking agent and the vulcanizing agent so that the crosslinking agent and the vulcanizing agent are uniformly dispersed in the second compound and simultaneously undergo a vulcanization reaction, thereby obtaining the conductive silicone rubber for electromagnetic shielding.
In some examples, the secondary compound is mixed with the crosslinking agent and the vulcanizing agent in an open mill at 12-15rpm for 10min at room temperature.
The practice of the present invention is illustrated by the following examples.
Example 1
The embodiment provides a conductive silicone rubber for electromagnetic shielding, and a preparation method thereof comprises the following steps:
1) preparing materials according to the formula in the table 1;
TABLE 1
2) Stirring the fumed silica and 3 parts of the coupling agent A151 in a high-speed planetary stirrer at 1200rpm for 3min, taking out, and drying in an oven at 100 ℃ for 10min to obtain modified fumed silica;
3) stirring the conductive filler and 9 parts of coupling agent in a high-speed planetary stirrer at 1200rpm for 3min, taking out, and drying in an oven at 100 ℃ for 10min to obtain a modified conductive filler;
4) plasticating methyl vinyl raw rubber 110-8s and fluorosilicone rubber FSR8430-U in an open mill, adding modified fumed silica in batches, mixing for 10min at a rotating speed of 13rpm, adding modified conductive filler in batches, and mixing for 10min at a rotating speed of 12rpm to obtain a first rubber material;
5) mixing the first rubber material, hydroxyl silicone oil, ATBC and a release agent in an open mill at a rotating speed of 14rpm for 10min to obtain a second rubber material;
6) the second compound was mixed with TAIC and Bidao in an open mill at 15rpm for 10min at room temperature.
Example 2
The embodiment provides a conductive silicone rubber for electromagnetic shielding, and a preparation method thereof comprises the following steps:
1) preparing materials according to the formula in the table 2;
TABLE 2
2) Stirring the fumed silica and 4 parts of the coupling agent A151 in a high-speed planetary stirrer at 1200rpm for 3min, taking out, and drying in an oven at 100 ℃ for 10min to obtain modified fumed silica;
3) stirring the conductive filler and 9 parts of coupling agent in a high-speed planetary stirrer at 1200rpm for 3min, taking out, and drying in an oven at 100 ℃ for 10min to obtain a modified conductive filler;
4) plasticating methyl vinyl raw rubber 110-8s and methyl vinyl silicone rubber 110-2s in an open mill, adding modified fumed silica in batches, mixing for 10min at the rotating speed of 12rpm, adding modified conductive filler in batches, and mixing for 10min at the rotating speed of 13rpm to obtain a first rubber material;
5) mixing the first rubber material, hydroxyl silicone oil, ATBC and a release agent in an open mill at a rotating speed of 15rpm for 10min to obtain a second rubber material;
6) the secondary mix was mixed with TAIC, Bingwu in an open mill at 14rpm for 10min at room temperature.
Example 3
The embodiment provides a conductive silicone rubber for electromagnetic shielding, and a preparation method thereof comprises the following steps:
1) preparing materials according to the formula in the table 3;
TABLE 3
2) Stirring the fumed silica and 6 parts of the coupling agent A151 in a high-speed planetary stirrer at 1200rpm for 3min, taking out, and drying in an oven at 100 ℃ for 10min to obtain modified fumed silica;
3) stirring the conductive filler and 9 parts of coupling agent in a high-speed planetary stirrer at 1200rpm for 3min, taking out, and drying in an oven at 100 ℃ for 10min to obtain a modified conductive filler;
4) adding 110-8s of methyl vinyl raw rubber into an open mill, adding modified fumed silica in batches, mixing for 10min at the rotating speed of 13rpm, adding modified conductive filler in batches, and mixing for 10min at the rotating speed of 13rpm to obtain a first rubber material;
5) mixing the first rubber material, hydroxyl silicone oil, ATBC and a release agent in an open mill at a rotating speed of 15rpm for 10min to obtain a second rubber material;
6) the secondary mix was mixed with TAIC and Bidao in an open mill at 13rpm for 10min at room temperature.
The conductive silicone rubber for electromagnetic shielding prepared in examples 1 to 3 was subjected to performance tests, and table 4 shows the test results.
TABLE 4
| Item | Test standard | Example 1 | Example 2 | Example 3 |
| Hardness (Shao's A) | GBT 531.1-2008 | 67 | 65 | 64 |
| Elongation/percent | GBT 528-1998 | 120 | 144 | 153 |
| Tensile strength/Mpa | GBT 528-1998 | 2 | 1.83 | 1.58 |
| Volume resistivity/ohm | GB/T11210-1989 | 0.003 | 0.0032 | 0.0035 |
| Damp-heat (double 85)/h | GB/T15905-1995 | ＞1000 | ＞1000 | ＞1000 |
| High and low temperature (-40 deg.C to 105 deg.C)/times | GB/T15905-1995 | ＞600 | ＞600 | ＞600 |
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. The conductive silicone rubber for electromagnetic shielding is characterized by comprising the following raw materials in parts by weight:
2. the conductive silicone rubber for electromagnetic shielding according to claim 1, wherein the silicone rubber is a mixture of methyl vinyl silicone rubber and fluorosilicone rubber, and the weight of the fluorosilicone rubber is 0 to 50% of the total mass of the silicone rubber.
3. The conductive silicone rubber for electromagnetic shielding according to claim 2, wherein the silicone rubber is composed of a methyl vinyl silicone rubber having a vinyl content of 0.03% to 0.06% and a methyl vinyl silicone rubber having a vinyl content of 0.13% to 0.2%; or
The silicon rubber consists of methyl vinyl silicon rubber with the vinyl content of 0.03 to 0.06 percent and fluorinated silicon rubber; or
The silicon rubber is methyl vinyl silicon rubber with the vinyl content of 0.03-0.06%.
4. The conductive silicone rubber for electromagnetic shielding according to claim 1, wherein the conductive filler is at least one selected from the group consisting of silver-plated aluminum powder, silver-plated copper powder, silver-plated nickel powder, silver-plated glass fiber, and silver particles.
5. The conductive silicone rubber for electromagnetic shielding according to claim 4, wherein the conductive filler is silver-plated aluminum powder, the average particle size of the silver-plated aluminum powder is 35-45 μm, the silver-plated aluminum powder is aluminum powder coated with a silver layer on the surface, the aluminum powder is composed of aluminum and carbon, and the aluminum accounts for 75-85 wt%.
6. The conductive silicone rubber for electromagnetic shielding according to any one of claims 1 to 5, wherein the hydroxyl silicone oil has a hydroxyl group content of 6% to 8%; and/or
The coupling agent is vinyl triethoxysilane; and/or
The cross-linking agent is triallyl isocyanurate; and/or
The vulcanizing agent is bis-di-penta; and/or
The release agent is zinc stearate; and/or
The plasticizer is acetyl tributyl citrate.
7. The preparation method of the conductive silicone rubber for electromagnetic shielding is characterized by comprising the following steps:
the conductive silicone rubber for electromagnetic shielding according to any one of claims 1 to 6, providing raw materials: silicon rubber, conductive filler, fumed silica, a coupling agent, color master batch, a cross-linking agent, hydroxyl silicone oil, a plasticizer, a vulcanizing agent and a release agent;
reacting the conductive filler with a portion of the coupling agent to form a modified conductive filler;
reacting the fumed silica with the rest of the coupling agent to form modified fumed silica;
mixing the silicon rubber, the modified fumed silica and the modified conductive filler to obtain a first rubber material;
mixing the first rubber material with the color master, the hydroxyl silicone oil, the plasticizer and the release agent to obtain a second rubber material;
and mixing the second rubber compound with the cross-linking agent and the vulcanizing agent.
8. The method of claim 7, wherein the step of reacting the fumed silica and a portion of the coupling agent comprises: stirring at 1500rpm of 1000-; and/or
The step of reacting the conductive filler and the remaining coupling agent comprises: stirring at 1000 and 1500rpm for 1-5 min.
9. The method according to claim 7, wherein the weight ratio of the coupling agent in the step of reacting the fumed silica with a portion of the coupling agent to the coupling agent in the step of reacting the conductive filler with the remainder of the coupling agent is (4-6): (8-10).
10. The method of claim 7, wherein the mixing is performed in an open mill.
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