CN117801513A - Preparation method of multifunctional conductive rubber - Google Patents
Preparation method of multifunctional conductive rubber Download PDFInfo
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- CN117801513A CN117801513A CN202311213681.5A CN202311213681A CN117801513A CN 117801513 A CN117801513 A CN 117801513A CN 202311213681 A CN202311213681 A CN 202311213681A CN 117801513 A CN117801513 A CN 117801513A
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- 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
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Abstract
The invention provides a preparation method of multifunctional conductive rubber, which comprises the steps of modifying nylon fiber, catalytically activating, and chemically plating cobalt-tungsten-phosphorus alloy to obtain conductive nylon composite fiber; adding the conductive nylon composite fiber into a mixed solution of polymethyl vinyl siloxane, epoxy acrylate, carbomer resin, 1, 6-hexanediol diacrylate, hydroxyethyl methacrylate, tripropylene glycol and acrylic ester, pentaerythritol triacrylate and benzoin methyl ether, mixing, vulcanizing and obtaining the multifunctional conductive rubber. The multifunctional conductive rubber material prepared by the technical scheme has the comprehensive performances of electrothermal conversion, electromagnetic shielding, mechanical sensing and temperature sensing, and is excellent in performance index, which is a technical effect which cannot be realized by other conductive rubber materials.
Description
Technical Field
The invention relates to the technical field of electronic materials, in particular to a preparation method of multifunctional conductive rubber.
Background
Conductive rubber can be divided into two main types, namely structural type and composite type according to different structures and preparation methods. The structural conductive rubber is formed by chemical or electrochemical doping of a polymer with conjugated pi bonds, and has conductive groups or ions, and meanwhile, the whole molecular chain has good flexibility. The composite conductive rubber is obtained by blending conductive filler and rubber, and the conductivity of the composite conductive rubber depends on the conductivity of the conductive filler and the distribution condition of the conductive filler in the rubber. The conductive performance and mechanical performance of the composite conductive rubber can be changed by changing the amount and the type of the filler, so that the use requirements in different environments are met.
Xu Ting et al investigated the effect of silver-plated nickel powder volume fraction on silver-plated nickel powder/silicone rubber highly conductive composite material properties. The results show that: as the volume fraction of the silver-plated nickel powder is increased, the Shore A hardness of the composite material is increased, the stretch-break elongation is rapidly reduced, the volume resistivity is reduced, and an obvious percolation phenomenon occurs; when the volume fraction of the silver-plated nickel powder is 0.44, the composite material has good conductive stability and excellent electromagnetic shielding effectiveness, but has poor electrochemical corrosion resistance (rubber industry, 2018, 65:866). Sun Xilu and the like use methyl vinyl silicone rubber as a base rubber and white carbon black and the like as fillers to prepare heat vulcanized (HTV) silicone rubber. The influence of the amount of manganese acrylate and cerium acrylate on the performance of HTV silicone rubber is studied. The results show that as the amount of acrylate increases, the tensile strength of the silicone rubber increases up to about 11MPa, the elongation at break increases, the tear strength increases and then decreases, and the hardness decreases gradually. Wherein, the improvement effect of the manganese acrylate on the elongation at break and the tearing strength is better than that of cerium acrylate, and when the manganese acrylate is used in an amount of 4 parts, the tearing strength of the silicon rubber is as high as 43.47kN/m. The rubber processability analysis and the transmission electron microscope result show that the acrylate can obviously improve the dispersibility of the white carbon black. HTV silicone rubber (silicone material, 2018, 32:442) with high tensile and tear strength can be obtained with a small addition of acrylate. Li Yankui and the like research the influence of the two-stage vulcanization process on the performance of the aluminum silver-plated conductive rubber, and find that the influence of the non-pressure two-stage vulcanization process on the tensile strength and the elongation after break of the conductive rubber is smaller, and the use requirement of the mechanical property of the product is still met. The pressureless two-stage vulcanization process hardly influences the distribution of filler particles, can greatly improve the crosslinking density of the conductive rubber matrix, greatly reduces the number of oxidation channels, achieves the effect of slowing down the aging of the silicon rubber matrix, and improves the conductivity stability of the conductive rubber. The pressureless two-stage vulcanization process can remarkably improve the conductive stability of the conductive rubber, and the electromagnetic shielding effectiveness is more than 90dB at 500MHz and 1GHz frequency points (Yunnan chemical industry, 2019, 46:142). Ge Tiejun, etc.: the electrothermal paint is prepared by taking carbon crystal as filler and polyvinyl alcohol glue as base material, and the electrothermal film of carbon crystal Polycarbonate (PC) is prepared by printing. The influence of the grid structure on the electrothermal conversion efficiency of the PC electrothermal film is explored, and the mechanism of the PC electrothermal film is researched from the angles of volume resistivity, heating temperature, dielectric constant and microstructure. The results show that: compared with a PC electrothermal film with a planar structure, a thin-layer micro-capacitance structure is formed between a carbon crystal electrothermal coating and a grid of the carbon crystal PC electrothermal film with the grid structure, and the PC electrothermal film has higher heating temperature, lower volume resistivity and larger dielectric constant; the electrothermal conversion efficiency of the carbon crystal PC electrothermal film with the grid structure is 87.4 percent (modern plastic processing application, 2019,31 (3): 1).
In summary, conductive rubbers are various in variety and various in performance, but most of them have single functions, so that it is difficult to satisfy the multifunctional requirements. The multifunctional conductive rubber prepared by the invention has excellent electric heat conversion, electromagnetic shielding, mechanical sensing and temperature sensing performances, is unusual in the field of conductive rubber, and has great application value in the field of aerospace with high requirements on material performance integration level.
Disclosure of Invention
The invention aims to provide a preparation method of multifunctional conductive rubber, which aims to solve the problems that the existing conductive rubber has single function and is difficult to meet the multifunctional requirement.
In order to solve the technical problems, the technical scheme of the invention is as follows: the preparation method of the multifunctional conductive rubber comprises the following steps:
s1, placing 15-20 g of nylon 66 fiber into 50ml of acetone solution, adding 1-2 ml of 3-aminopropyl trimethoxy silane, 1-2 g of dodecyl trimethyl ammonium bromide and 1-2 ml of water, stirring at room temperature for 3 hours, filtering, placing the solid in an oven, and heating at 120 ℃ for 30 minutes to obtain modified nylon fiber;
s2, placing 15-20 g of the modified nylon fiber into 100ml of nano gold aqueous solution with gold concentration of 0.05% -0.1%, standing for 3 hours, and filtering to obtain gold activated nylon fiber;
s3, adding 3-4 g of cobalt dichloride, 3-4 g of sodium tungstate, 2-3 g of sodium hypophosphite, 6-8 g of sodium citrate, 5-6 g of ammonium chloride and 6-8 ml of 25% ammonia water into 100ml of water to obtain cobalt-tungsten-phosphorus electroless plating solution;
s4, placing 8-10 g Jin Huohua nylon fibers in 100ml of the cobalt-tungsten-phosphorus electroless plating solution, heating to 90 ℃, standing for 3 hours, and filtering to obtain cobalt-tungsten-phosphorus coated nylon fibers;
s5, mixing 8-10 g of the cobalt tungsten phosphorus coated nylon fiber, 8-10 g of polymethyl vinyl siloxane, 1-1.2 g of epoxy acrylate, 1-1.6 g of carbomer resin, 1-1.4 g of 1, 6-hexanediol diacrylate, 1-1.4 g of hydroxyethyl methacrylate, 2-2.8 g of tripropylene glycol acrylate, 0.8-1 g of pentaerythritol triacrylate and 0.4-0.6 g of benzoin methyl ether to obtain a nylon silicone rubber mixture;
s6, mixing 25-30 g of the nylon silicone rubber mixture into a film with the thickness of 1.8mm, vulcanizing the film at 200 ℃ for 120 minutes, and cooling to obtain the multifunctional conductive rubber.
Further, the prepared multifunctional guideThe electrothermal conversion efficiency of the electric rubber is 97.8-99.1%, the electromagnetic shielding efficiency in the wave band of 30-1500 MHz is 68-79 dB, the stress strain sensing sensitivity is 8.7-9.6, and the temperature sensing sensitivity is-1.8X10 -2 ～-1.2×10 -2 K -1 。
The preparation method of the multifunctional conductive rubber provided by the invention has the beneficial effects that:
1) The novel conductive rubber material prepared by the invention has comprehensive properties of electrothermal conversion, electromagnetic shielding, mechanical sensing and temperature sensing, and is excellent in performance index, which is a technical effect which cannot be realized by other conductive rubber materials.
2) In terms of how to prepare conductive rubber with excellent comprehensive properties (electric heat conversion, electromagnetic shielding, mechanical sensing and temperature sensing), no document can provide experimental guidance or theoretical teaching at present, and the invention is creative from nothing to nothing.
3) At present, no theory or experiment shows that the conductive rubber with excellent single performance has excellent comprehensive performance; the general knowledge of the person skilled in the art is: the preparation method and the technical effects produced by the preparation method have uniqueness, namely the technical effects are obvious.
Detailed Description
The preparation method of the multifunctional conductive rubber provided by the invention is further described in detail below by combining specific examples. Advantages and features of the invention will become more apparent from the following description and from the claims.
Example 1
15g of nylon 66 fiber was placed in 50ml of acetone solution, 1ml of 3-aminopropyl trimethoxysilane, 1g of dodecyl trimethyl ammonium bromide, and 1ml of water were added, stirred at room temperature for 3 hours, filtered, and the solid was placed in an oven and heated at 120℃for 30 minutes to obtain a modified nylon fiber.
15g of modified nylon fiber is placed in 100ml of nano gold aqueous solution with gold concentration of 0.05 percent, placed for 3 hours and filtered, thus obtaining the gold activated nylon fiber.
3g of cobalt dichloride, 3g of sodium tungstate, 2g of sodium hypophosphite, 6g of sodium citrate, 5g of ammonium chloride and 6ml of ammonia water with the concentration of 25% are added into 100ml of water to obtain cobalt tungsten phosphorus chemical plating solution.
8g Jin Huohua nylon fiber is placed in 100ml cobalt tungsten phosphorus chemical plating solution, heated to 90 ℃, placed for 3 hours and filtered, and the cobalt tungsten phosphorus coated nylon fiber is obtained.
8g of cobalt tungsten phosphorus coated nylon fiber, 8g of polymethyl vinyl siloxane, 1g of epoxy acrylate, 1g of carbomer resin, 1g of 1, 6-hexanediol diacrylate, 1g of hydroxyethyl methacrylate, 2g of tripropylene glycol and acrylate, 0.8g of pentaerythritol triacrylate and 0.4g of benzoin methyl ether were mixed to obtain a nylon silicone rubber mixture.
25g of nylon silicone rubber mixture was mixed into a 1.8mm thick film, and the film was vulcanized at 200℃for 120 minutes, cooled, and used as a multifunctional conductive rubber.
Reference (modern plastic processing application, 2019,31 (3): 1), the electrothermal conversion efficiency of the multifunctional conductive rubber is 97.8%, the electromagnetic shielding effectiveness of the multifunctional conductive rubber in the wave band of 30-1500 MHz is 68-79 dB as measured by the national standard GB/T30142-2013 planar electromagnetic shielding material shielding effectiveness measuring method, the stress strain sensing sensitivity of the multifunctional conductive rubber is 9.6 as measured by reference (Journal of Materials Chemistry A,2018, 6:16556), and the temperature sensing sensitivity of the multifunctional conductive rubber is-1.8x10 as measured by reference (Advanced Healthcare Materials,2018, 7:1800074) -2 K -1 。
Example 2
20g of nylon 66 fiber was placed in 50ml of acetone solution, 2ml of 3-aminopropyl trimethoxysilane, 2g of dodecyl trimethyl ammonium bromide and 2ml of water were added, stirred at room temperature for 3 hours, filtered, and the solid was placed in an oven and heated at 120 ℃ for 30 minutes to obtain a modified nylon fiber.
20g of modified nylon fiber is placed in 100ml of nano gold aqueous solution with gold concentration of 0.1 percent, placed for 3 hours and filtered, thus obtaining the gold activated nylon fiber.
Adding 4g of cobalt dichloride, 4g of sodium tungstate, 3g of sodium hypophosphite, 8g of sodium citrate, 6g of ammonium chloride and 8ml of 25% ammonia water into 100ml of water to obtain cobalt tungsten phosphorus chemical plating solution.
10g Jin Huohua nylon fiber is placed in 100ml cobalt tungsten phosphorus chemical plating solution, heated to 90 ℃, placed for 3 hours and filtered, and the cobalt tungsten phosphorus coated nylon fiber is obtained.
10g of cobalt tungsten phosphorus coated nylon fiber, 10g of polymethyl vinyl siloxane, 1.2g of epoxy acrylate, 1.6g of carbomer resin, 1.4g of 1, 6-hexanediol diacrylate, 1.4g of hydroxyethyl methacrylate, 2.8g of tripropylene glycol and acrylate, 1g of pentaerythritol triacrylate and 0.6g of benzoin methyl ether are mixed to obtain a nylon silicone rubber mixture.
30g of nylon silicone rubber mixture is mixed into a film with the thickness of 1.8mm, and the film is vulcanized for 120 minutes at the temperature of 200 ℃, and is cooled to obtain the multifunctional conductive rubber.
Reference (modern plastic processing application, 2019,31 (3): 1), the electrothermal conversion efficiency of the multifunctional conductive rubber is 99.1%, the electromagnetic shielding effectiveness of the multifunctional conductive rubber in the wave band of 30-1500 MHz is 68-79 dB as measured by the national standard GB/T30142-2013 planar electromagnetic shielding material shielding effectiveness measuring method, the stress strain sensing sensitivity of the multifunctional conductive rubber is 8.7 as measured by reference (Journal of Materials Chemistry A,2018, 6:16556), and the temperature sensing sensitivity of the multifunctional conductive rubber is-1.2x10 as measured by reference (Advanced Healthcare Materials,2018, 7:1800074) -2 K -1 。
Example 3
18g of nylon 66 fiber was placed in 50ml of acetone solution, 1.52ml of 3-aminopropyl trimethoxysilane, 1.2g of dodecyl trimethyl ammonium bromide, and 1.2ml of water were added, stirred at room temperature for 3 hours, filtered, and the solid was placed in an oven and heated at 120℃for 30 minutes to obtain a modified nylon fiber.
18g of modified nylon fiber is placed in 100ml of nano gold aqueous solution with gold concentration of 0.1 percent, placed for 3 hours and filtered, thus obtaining the gold activated nylon fiber.
3.4g of cobalt dichloride, 3.4g of sodium tungstate, 2.3g of sodium hypophosphite, 6.8g of sodium citrate, 5.6g of ammonium chloride and 6.8ml of ammonia water with the concentration of 25% are added into 100ml of water to obtain cobalt tungsten phosphorus chemical plating solution.
9g Jin Huohua nylon fiber is placed in 100ml cobalt tungsten phosphorus chemical plating solution, heated to 90 ℃, placed for 3 hours and filtered, and the cobalt tungsten phosphorus coated nylon fiber is obtained.
9g of cobalt tungsten phosphorus coated nylon fiber, 9g of polymethyl vinyl siloxane, 1.2g of epoxy acrylate, 1.6g of carbomer resin, 1g of 1, 6-hexanediol diacrylate, 1g of hydroxyethyl methacrylate, 2g of tripropylene glycol and acrylate, 1g of pentaerythritol triacrylate and 0.4g of benzoin methyl ether are mixed to obtain a nylon silicone rubber mixture.
28g of nylon silicone rubber mixture is mixed into a film with the thickness of 1.8mm, and the film is vulcanized for 120 minutes at 200 ℃, and cooled to obtain the multifunctional conductive rubber.
Reference (modern plastic processing application, 2019,31 (3): 1), the electrothermal conversion efficiency of the multifunctional conductive rubber is 98.9%, the electromagnetic shielding effectiveness of the multifunctional conductive rubber in the wave band of 30-1500 MHz is 68-79 dB, the stress strain sensing sensitivity of the multifunctional conductive rubber is 8.9, and the temperature sensing sensitivity of the multifunctional conductive rubber is-1.4x10, which is measured by reference (Journal of Materials Chemistry A,2018, 6:16556) and reference (Advanced Healthcare Materials,2018, 7:1800074) -2 K -1 。
Example 4
20g of nylon 66 fiber was placed in 50ml of acetone solution, 2ml of 3-aminopropyl trimethoxysilane, 1g of dodecyl trimethyl ammonium bromide and 2ml of water were added, stirred at room temperature for 3 hours, filtered, and the solid was placed in an oven and heated at 120 ℃ for 30 minutes to obtain a modified nylon fiber.
20g of modified nylon fiber is placed in 100ml of nano gold aqueous solution with gold concentration of 0.05 percent, placed for 3 hours and filtered, thus obtaining the gold activated nylon fiber.
3g of cobalt dichloride, 4g of sodium tungstate, 3g of sodium hypophosphite, 6g of sodium citrate, 6g of ammonium chloride and 6ml of 25% ammonia water are added into 100ml of water to obtain cobalt tungsten phosphorus chemical plating solution.
8g Jin Huohua nylon fiber is placed in 100ml cobalt tungsten phosphorus chemical plating solution, heated to 90 ℃, placed for 3 hours and filtered, and the cobalt tungsten phosphorus coated nylon fiber is obtained.
8g of cobalt tungsten phosphorus coated nylon fiber, 10g of polymethyl vinyl siloxane, 1g of epoxy acrylate, 1.6g of carbomer resin, 1g of 1, 6-hexanediol diacrylate, 1.4g of hydroxyethyl methacrylate, 2g of tripropylene glycol and acrylate, 1g of pentaerythritol triacrylate and 0.6g of benzoin methyl ether were mixed to obtain a nylon silicone rubber mixture.
25g of nylon silicone rubber mixture was mixed into a 1.8mm thick film, and the film was vulcanized at 200℃for 120 minutes, cooled, and used as a multifunctional conductive rubber.
Reference (modern plastic processing application, 2019,31 (3): 1), the electrothermal conversion efficiency of the multifunctional conductive rubber is 98.6%, the electromagnetic shielding effectiveness of the multifunctional conductive rubber in the wave band of 30-1500 MHz is 68-79 dB, the stress strain sensing sensitivity of the multifunctional conductive rubber is 9.3, and the temperature sensing sensitivity of the multifunctional conductive rubber is-1.5X10, measured by reference (Journal of Materials Chemistry A,2018, 6:16556), measured by reference (Advanced Healthcare Materials,2018, 7:1800074), measured by reference (national standard) GB/T30142-2013) planar electromagnetic shielding material shielding effectiveness measuring method -2 K -1 。
What is not described in detail in this specification is prior art known to those skilled in the art. It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (2)
1. The preparation method of the multifunctional conductive rubber is characterized by comprising the following steps of:
s1, placing 15-20 g of nylon 66 fiber into 50ml of acetone solution, adding 1-2 ml of 3-aminopropyl trimethoxy silane, 1-2 g of dodecyl trimethyl ammonium bromide and 1-2 ml of water, stirring at room temperature for 3 hours, filtering, placing the solid in an oven, and heating at 120 ℃ for 30 minutes to obtain modified nylon fiber;
s2, placing 15-20 g of the modified nylon fiber into 100ml of nano gold aqueous solution with gold concentration of 0.05% -0.1%, standing for 3 hours, and filtering to obtain gold activated nylon fiber;
s3, adding 3-4 g of cobalt dichloride, 3-4 g of sodium tungstate, 2-3 g of sodium hypophosphite, 6-8 g of sodium citrate, 5-6 g of ammonium chloride and 6-8 ml of 25% ammonia water into 100ml of water to obtain cobalt-tungsten-phosphorus electroless plating solution;
s4, placing 8-10 g Jin Huohua nylon fibers in 100ml of the cobalt-tungsten-phosphorus electroless plating solution, heating to 90 ℃, standing for 3 hours, and filtering to obtain cobalt-tungsten-phosphorus coated nylon fibers;
s5, mixing 8-10 g of the cobalt tungsten phosphorus coated nylon fiber, 8-10 g of polymethyl vinyl siloxane, 1-1.2 g of epoxy acrylate, 1-1.6 g of carbomer resin, 1-1.4 g of 1, 6-hexanediol diacrylate, 1-1.4 g of hydroxyethyl methacrylate, 2-2.8 g of tripropylene glycol acrylate, 0.8-1 g of pentaerythritol triacrylate and 0.4-0.6 g of benzoin methyl ether to obtain a nylon silicone rubber mixture;
s6, mixing 25-30 g of the nylon silicone rubber mixture into a film with the thickness of 1.8mm, vulcanizing the film at 200 ℃ for 120 minutes, and cooling to obtain the multifunctional conductive rubber.
2. The multifunctional conductive rubber is characterized in that the electrothermal conversion efficiency of the prepared multifunctional conductive rubber is 97.8-99.1%, the electromagnetic shielding efficiency in the wave band of 30-1500 MHz is 68-79 dB, the stress strain sensing sensitivity is 8.7-9.6, and the temperature sensing sensitivity is-1.8x10 -2 ～-1.2×10 -2 K -1 。
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