CN114685976B - High-toughness conductive nylon material and preparation method thereof - Google Patents
High-toughness conductive nylon material and preparation method thereof Download PDFInfo
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- CN114685976B CN114685976B CN202210453034.0A CN202210453034A CN114685976B CN 114685976 B CN114685976 B CN 114685976B CN 202210453034 A CN202210453034 A CN 202210453034A CN 114685976 B CN114685976 B CN 114685976B
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- 239000000463 material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000004677 Nylon Substances 0.000 title claims abstract description 31
- 229920001778 nylon Polymers 0.000 title claims abstract description 31
- 239000011231 conductive filler Substances 0.000 claims abstract description 50
- 229920002292 Nylon 6 Polymers 0.000 claims abstract description 31
- 238000001746 injection moulding Methods 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 21
- 229920013636 polyphenyl ether polymer Polymers 0.000 claims abstract description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 16
- 229920001971 elastomer Polymers 0.000 claims abstract description 16
- 239000000806 elastomer Substances 0.000 claims abstract description 16
- 229920001910 maleic anhydride grafted polyolefin Polymers 0.000 claims abstract description 16
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 16
- 239000011029 spinel Substances 0.000 claims abstract description 16
- 238000001125 extrusion Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000002023 wood Substances 0.000 claims description 60
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 23
- 239000002042 Silver nanowire Substances 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 20
- 150000001721 carbon Chemical class 0.000 claims description 20
- 229910052799 carbon Inorganic materials 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 20
- 238000002791 soaking Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000009835 boiling Methods 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 14
- 229920002488 Hemicellulose Polymers 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 10
- 229920005610 lignin Polymers 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 10
- 239000010875 treated wood Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000012360 testing method Methods 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- 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
- C08K2201/011—Nanostructured additives
-
- 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
- C08K2201/016—Additives defined by their aspect ratio
-
- 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
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
Abstract
The invention provides a preparation method of a high-toughness conductive nylon material. Comprises the following components: nylon 6, polyphenyl ether, maleic anhydride grafted polyolefin elastomer, conductive filler and magnesia-alumina spinel whisker; the conductive filler is silver-doped 3D conductive filler. S1: all raw materials were placed in a vacuum oven and left to dry overnight; s2: putting the mixture into a single screw extruder, and carrying out melt extrusion and blending twice; s3: and (5) carrying out injection molding on the extruded particles in an injection molding machine to obtain the composite material. The silver-doped 3D conductive filler has high porosity, low density, large specific surface area, excellent compressibility and conductivity, so that the silver-doped 3D conductive filler has more advantages in conductivity and toughness; the addition of the magnesia-alumina spinel whisker can obviously inhibit the chain extension reaction of the maleic anhydride grafted polyolefin elastomer and nylon 6, reduce the viscosity of the nylon 6/polyphenyl ether composite material and improve the toughness of the material.
Description
Technical Field
The invention relates to the field of plastic materials, in particular to a high-toughness conductive nylon material and a preparation method thereof.
Background
Nylon 6 is an aliphatic linear macromolecule H- [ NH (CH) 2 )XCO] n -OH, the linear chain being mainly methylene (-CH 2), the individual segments being linked together mainly by amide bonds, the molecular configuration being planar zigzag. The molecular and crystal structures of nylon 6 determine its properties and product performance. Because of the existence of a large number of strong polar amide groups in the nylon 6 molecule, the nylon 6 molecule has excellent hygroscopicity compared with common chemical fibers, and can promote the nylon 6 macromolecule to be in a more easily-promoted stateWhen the nylon 6 is arranged, hydrogen bonds are formed among macromolecular chains, so that the bonding force among nylon 6 molecular chains is improved, the mobility of the nylon 6 molecular chains is reduced, and the arrangement among the nylon 6 molecular chains is more regular, so that the nylon 6 is a thermoplastic semi-crystalline polycondensate. Nylon 6 is translucent and has many applications due to its ease of processing, excellent mechanical properties and chemical resistance, including self-lubricating gears, bearings, fibers and a wide variety of commercial products. When the nylon material is applied to logistics equipment, the antistatic performance and the toughness are required to be simultaneously considered. In the modification process of nylon materials, a large amount of conductive components are required to be added, and generally, conductive media such as carbon fibers, carbon nanotubes, conductive carbon black and the like are adopted, but the toughness of the materials is obviously reduced, so that the problem to be solved is that the toughness is not influenced or is less influenced in the colleagues for improving the conductivity of the materials.
Disclosure of Invention
The technical problems to be solved are as follows: the invention aims to provide a high-toughness conductive nylon material and a preparation method thereof, and the silver-doped 3D conductive filler has high porosity, low density, large specific surface area, excellent compressibility and conductivity, so that the silver-doped 3D conductive filler has more advantages in conductivity and toughness; the addition of the magnesia-alumina spinel whisker can obviously inhibit the chain extension reaction of the maleic anhydride grafted polyolefin elastomer and nylon 6, reduce the viscosity of the nylon 6/polyphenyl ether composite material and improve the toughness of the material.
The technical scheme is as follows: the high-toughness conductive nylon material comprises the following components: 50 parts of nylon 6, 40-45 parts of polyphenyl ether, 2-3 parts of maleic anhydride grafted polyolefin elastomer, 10-15 parts of conductive filler and 2-5 parts of magnesia alumina spinel whisker;
the conductive filler is silver-doped 3D conductive filler.
Further, the grain diameter of the silver-doped 3D conductive filler is less than or equal to 74 mu m.
Further, the diameter of the magnesia-alumina spinel whisker is 1-8 mu m, and the length-diameter ratio is 20.
Further, the preparation method of the silver-doped 3D conductive filler comprises the following steps:
(1) Preparing 2.5mol/L NaOH and 0.4mol/L Na 2 SO 3 MixingBoiling the liquid at 170 ℃;
(2) Weighing square wood blocks with side length of 3cm, and placing the square wood blocks into the mixed solution for 6 hours to carry out lignin removal and hemicellulose treatment;
(3) Taking out the wood block, and cleaning the wood block to be neutral by boiled deionized water;
(4) Configuring 3mol/L H 2 O 2 Placing the cleaned wood block into boiling H 2 O 2 2h in the middle;
(5) Taking out the wood block, washing with deionized water, and freeze-drying for 12h;
(6) Directly annealing the chemically treated wood blocks in argon at 400-600 ℃ to obtain carbon sponge;
(7) Soaking the carbon sponge in 50% phosphoric acid for 1-2h, drying, and drying in a vacuum oven to obtain a modified carbon sponge;
(8) Preparing silver nanowire ethanol solution, and soaking the silver nanowire ethanol solution into the modified carbon sponge by using a pulse vacuum method for 10-15min;
(9) Taking out, and putting into a baking oven for baking;
(10) And crushing to obtain the silver-doped 3D conductive filler.
Further, the mass concentration of the silver nanowire ethanol solution is 0.1-0.2mg/mL.
Further, the pulse vacuum condition is room temperature condition, and the vacuum degree is 0.08MPa.
The preparation method of the high-toughness conductive nylon material comprises the following preparation steps:
s1: all raw materials were placed in a vacuum oven and left to dry overnight;
s2: putting the mixture into a single screw extruder, carrying out melt extrusion and blending twice, wherein the temperature of the screw is set to 265/270/270/270 ℃, and the rotating speed of the screw is set to 80rpm;
s3: and (5) carrying out injection molding on the extruded particles in an injection molding machine to obtain the composite material.
Further, the injection temperature in the step S3 is set to 255/260/270/270/270 ℃ and the mold temperature is set to 80 ℃.
The beneficial effects are that:
1. according to the invention, the silver-doped 3D conductive filler can be selectively dispersed in the nylon 6 and polyphenyl ether composite, the maleic anhydride grafted polyolefin elastomer can act with the silver-doped 3D conductive filler, the distance between silver-doped 3D conductive filler layers is increased, and meanwhile, the dispersion of the silver-doped 3D conductive filler in the nylon 6 and polyphenyl ether composite is improved, so that the generation of agglomerates is avoided.
2. According to the invention, the maleic anhydride grafted polyolefin elastomer can improve the interfacial binding force of the nylon 6 and the polyphenyl ether, reduce the size of the dispersed phase polyphenyl ether, and the addition of the silver-doped 3D conductive filler can prevent the polyphenyl ether from coalescence, so that the size of the polyphenyl ether phase is reduced.
3. The addition of the magnesia-alumina spinel whisker in the invention can obviously inhibit the chain extension reaction of the maleic anhydride grafted polyolefin elastomer and nylon 6, reduce the viscosity of the nylon 6/polyphenyl ether composite material and improve the toughness of the material.
4. The silver-doped 3D conductive filler has high porosity, low density, large specific surface area, excellent compressibility and conductivity, and has more advantages in conductivity and toughness.
5. The silver nanowire is adopted as the conductive matrix, and compared with a carbon material, the metal material has more excellent conductive performance.
Detailed Description
The invention provides a high-toughness conductive nylon material and a preparation method thereof, and the invention is further described in detail by matching with examples in order to make the purposes, technical schemes and effects of the invention clearer and more definite. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The high-toughness conductive nylon material comprises the following components: 50 parts of nylon 6, 40 parts of polyphenyl ether, 2 parts of maleic anhydride grafted polyolefin elastomer, 10 parts of silver-doped 3D conductive filler with the particle size of 58-74 mu m, 2 parts of magnesia alumina spinel whisker with the diameter of 1-8 mu m and the length-diameter ratio of 20.
The preparation method of the silver-doped 3D conductive filler comprises the following steps:
(1) Preparing 2.5mol/L NaOH and 0.4mol/L Na 2 SO 3 Boiling the mixed solution at 170 ℃;
(2) Weighing square wood blocks with side length of 3cm, and placing the square wood blocks into the mixed solution for 6 hours to carry out lignin removal and hemicellulose treatment;
(3) Taking out the wood block, and cleaning the wood block to be neutral by boiled deionized water;
(4) Configuring 3mol/L H 2 O 2 Placing the cleaned wood block into boiling H 2 O 2 2h in the middle;
(5) Taking out the wood block, washing with deionized water, and freeze-drying for 12h;
(6) Directly annealing the chemically treated wood blocks in argon at 400 ℃ to obtain carbon sponge;
(7) Soaking the carbon sponge in 50% phosphoric acid for 1h, drying, and then putting into a vacuum oven for drying to obtain a modified carbon sponge;
(8) Preparing silver nanowire ethanol solution with the mass concentration of 0.1mg/mL, soaking the silver nanowire ethanol solution into the modified carbon sponge by using a pulse vacuum method under the room temperature condition, wherein the vacuum degree is 0.08MPa, and the treatment time is 10min;
(9) Taking out, and putting into a baking oven for baking;
(10) And crushing to obtain the silver-doped 3D conductive filler.
The preparation method of the high-toughness conductive nylon material comprises the following preparation steps:
s1: all raw materials were placed in a vacuum oven and left to dry overnight;
s2: putting the mixture into a single screw extruder, carrying out melt extrusion and blending twice, wherein the temperature of the screw is set to 265/270/270/270 ℃, and the rotating speed of the screw is set to 80rpm;
s3: and (3) carrying out injection molding on the extruded particles in an injection molding machine to obtain the composite material, wherein the injection molding temperature is 255/260/270/270/270 ℃ and the mold temperature is 80 ℃.
Example 2
The high-toughness conductive nylon material comprises the following components: 50 parts of nylon 6, 41 parts of polyphenyl ether, 2 parts of maleic anhydride grafted polyolefin elastomer, 11 parts of silver-doped 3D conductive filler with the particle size of 48-58 mu m, and 2 parts of magnesia alumina spinel whisker with the diameter of 1-8 mu m and the length-diameter ratio of 20.
The preparation method of the silver-doped 3D conductive filler comprises the following steps:
(1) Preparing 2.5mol/L NaOH and 0.4mol/L Na 2 SO 3 Boiling the mixed solution at 170 ℃;
(2) Weighing square wood blocks with side length of 3cm, and placing the square wood blocks into the mixed solution for 6 hours to carry out lignin removal and hemicellulose treatment;
(3) Taking out the wood block, and cleaning the wood block to be neutral by boiled deionized water;
(4) Configuring 3mol/L H 2 O 2 Placing the cleaned wood block into boiling H 2 O 2 2h in the middle;
(5) Taking out the wood block, washing with deionized water, and freeze-drying for 12h;
(6) Directly annealing the chemically treated wood blocks in argon at 450 ℃ to obtain carbon sponge;
(7) Soaking the carbon sponge in 50% phosphoric acid for 1h, drying, and then putting into a vacuum oven for drying to obtain a modified carbon sponge;
(8) Preparing silver nanowire ethanol solution with the mass concentration of 0.1mg/mL, soaking the silver nanowire ethanol solution into the modified carbon sponge by using a pulse vacuum method under the room temperature condition, wherein the vacuum degree is 0.08MPa, and the treatment time is 11min;
(9) Taking out, and putting into a baking oven for baking;
(10) And crushing to obtain the silver-doped 3D conductive filler.
The preparation method of the high-toughness conductive nylon material comprises the following preparation steps:
s1: all raw materials were placed in a vacuum oven and left to dry overnight;
s2: putting the mixture into a single screw extruder, carrying out melt extrusion and blending twice, wherein the temperature of the screw is set to 265/270/270/270 ℃, and the rotating speed of the screw is set to 80rpm;
s3: and (3) carrying out injection molding on the extruded particles in an injection molding machine to obtain the composite material, wherein the injection molding temperature is 255/260/270/270/270 ℃ and the mold temperature is 80 ℃.
Example 3
The high-toughness conductive nylon material comprises the following components: 50 parts of nylon 6, 42 parts of polyphenyl ether, 2.5 parts of maleic anhydride grafted polyolefin elastomer, 12 parts of silver-doped 3D conductive filler with the particle size of 38-48 mu m, 3 parts of magnesia alumina spinel whisker with the diameter of 1-8 mu m and the length-diameter ratio of 20.
The preparation method of the silver-doped 3D conductive filler comprises the following steps:
(1) Preparing 2.5mol/L NaOH and 0.4mol/L Na 2 SO 3 Boiling the mixed solution at 170 ℃;
(2) Weighing square wood blocks with side length of 3cm, and placing the square wood blocks into the mixed solution for 6 hours to carry out lignin removal and hemicellulose treatment;
(3) Taking out the wood block, and cleaning the wood block to be neutral by boiled deionized water;
(4) Configuring 3mol/L H 2 O 2 Placing the cleaned wood block into boiling H 2 O 2 2h in the middle;
(5) Taking out the wood block, washing with deionized water, and freeze-drying for 12h;
(6) Directly annealing the chemically treated wood blocks in argon at 500 ℃ to obtain carbon sponge;
(7) Soaking the carbon sponge in 50% phosphoric acid for 1.5h, drying, and then putting into a vacuum oven for drying to obtain a modified carbon sponge;
(8) Preparing silver nanowire ethanol solution with the mass concentration of 0.15mg/mL, soaking the silver nanowire ethanol solution into the modified carbon sponge by using a pulse vacuum method under the room temperature condition, wherein the vacuum degree is 0.08MPa, and the treatment time is 12min;
(9) Taking out, and putting into a baking oven for baking;
(10) And crushing to obtain the silver-doped 3D conductive filler.
The preparation method of the high-toughness conductive nylon material comprises the following preparation steps:
s1: all raw materials were placed in a vacuum oven and left to dry overnight;
s2: putting the mixture into a single screw extruder, carrying out melt extrusion and blending twice, wherein the temperature of the screw is set to 265/270/270/270 ℃, and the rotating speed of the screw is set to 80rpm;
s3: and (3) carrying out injection molding on the extruded particles in an injection molding machine to obtain the composite material, wherein the injection molding temperature is 255/260/270/270/270 ℃ and the mold temperature is 80 ℃.
Example 4
The high-toughness conductive nylon material comprises the following components: 50 parts of nylon 6, 43 parts of polyphenyl ether, 2.5 parts of maleic anhydride grafted polyolefin elastomer, 13 parts of silver-doped 3D conductive filler with the particle size of 25-38 mu m, 3 parts of magnesia alumina spinel whisker with the diameter of 1-8 mu m and the length-diameter ratio of 20.
The preparation method of the silver-doped 3D conductive filler comprises the following steps:
(1) Preparing 2.5mol/L NaOH and 0.4mol/L Na 2 SO 3 Boiling the mixed solution at 170 ℃;
(2) Weighing square wood blocks with side length of 3cm, and placing the square wood blocks into the mixed solution for 6 hours to carry out lignin removal and hemicellulose treatment;
(3) Taking out the wood block, and cleaning the wood block to be neutral by boiled deionized water;
(4) Configuring 3mol/L H 2 O 2 Placing the cleaned wood block into boiling H 2 O 2 2h in the middle;
(5) Taking out the wood block, washing with deionized water, and freeze-drying for 12h;
(6) Directly annealing the chemically treated wood blocks in argon at 500 ℃ to obtain carbon sponge;
(7) Soaking the carbon sponge in 50% phosphoric acid for 1.5h, drying, and then putting into a vacuum oven for drying to obtain a modified carbon sponge;
(8) Preparing silver nanowire ethanol solution with the mass concentration of 0.15mg/mL, soaking the silver nanowire ethanol solution into the modified carbon sponge by using a pulse vacuum method under the room temperature condition, wherein the vacuum degree is 0.08MPa, and the treatment time is 13min;
(9) Taking out, and putting into a baking oven for baking;
(10) And crushing to obtain the silver-doped 3D conductive filler.
The preparation method of the high-toughness conductive nylon material comprises the following preparation steps:
s1: all raw materials were placed in a vacuum oven and left to dry overnight;
s2: putting the mixture into a single screw extruder, carrying out melt extrusion and blending twice, wherein the temperature of the screw is set to 265/270/270/270 ℃, and the rotating speed of the screw is set to 80rpm;
s3: and (3) carrying out injection molding on the extruded particles in an injection molding machine to obtain the composite material, wherein the injection molding temperature is 255/260/270/270/270 ℃ and the mold temperature is 80 ℃.
Example 5
The high-toughness conductive nylon material comprises the following components: 50 parts of nylon 6, 44 parts of polyphenyl ether, 3 parts of maleic anhydride grafted polyolefin elastomer, 14 parts of silver-doped 3D conductive filler with the particle size of 18-25 mu m, and 4 parts of magnesia alumina spinel whisker with the diameter of 1-8 mu m and the length-diameter ratio of 20.
The preparation method of the silver-doped 3D conductive filler comprises the following steps:
(1) Preparing 2.5mol/L NaOH and 0.4mol/L Na 2 SO 3 Boiling the mixed solution at 170 ℃;
(2) Weighing square wood blocks with side length of 3cm, and placing the square wood blocks into the mixed solution for 6 hours to carry out lignin removal and hemicellulose treatment;
(3) Taking out the wood block, and cleaning the wood block to be neutral by boiled deionized water;
(4) Configuring 3mol/L H 2 O 2 Placing the cleaned wood block into boiling H 2 O 2 2h in the middle;
(5) Taking out the wood block, washing with deionized water, and freeze-drying for 12h;
(6) Directly annealing the chemically treated wood blocks in argon at 550 ℃ to obtain carbon sponge;
(7) Soaking the carbon sponge in 50% phosphoric acid for 2h, drying, and then putting into a vacuum oven for drying to obtain a modified carbon sponge;
(8) Preparing silver nanowire ethanol solution with the mass concentration of 0.2mg/mL, soaking the silver nanowire ethanol solution into the modified carbon sponge by using a pulse vacuum method under the room temperature condition, wherein the vacuum degree is 0.08MPa, and the treatment time is 14min;
(9) Taking out, and putting into a baking oven for baking;
(10) And crushing to obtain the silver-doped 3D conductive filler.
The preparation method of the high-toughness conductive nylon material comprises the following preparation steps:
s1: all raw materials were placed in a vacuum oven and left to dry overnight;
s2: putting the mixture into a single screw extruder, carrying out melt extrusion and blending twice, wherein the temperature of the screw is set to 265/270/270/270 ℃, and the rotating speed of the screw is set to 80rpm;
s3: and (3) carrying out injection molding on the extruded particles in an injection molding machine to obtain the composite material, wherein the injection molding temperature is 255/260/270/270/270 ℃ and the mold temperature is 80 ℃.
Example 6
The high-toughness conductive nylon material comprises the following components: 50 parts of nylon 6, 45 parts of polyphenyl ether, 3 parts of maleic anhydride grafted polyolefin elastomer, 15 parts of silver-doped 3D conductive filler with the particle size of 13-18 mu m, and 5 parts of magnesia alumina spinel whisker with the diameter of 1-8 mu m and the length-diameter ratio of 20.
The preparation method of the silver-doped 3D conductive filler comprises the following steps:
(1) Preparing 2.5mol/L NaOH and 0.4mol/L Na 2 SO 3 Boiling the mixed solution at 170 ℃;
(2) Weighing square wood blocks with side length of 3cm, and placing the square wood blocks into the mixed solution for 6 hours to carry out lignin removal and hemicellulose treatment;
(3) Taking out the wood block, and cleaning the wood block to be neutral by boiled deionized water;
(4) Configuring 3mol/L H 2 O 2 Placing the cleaned wood block into boiling H 2 O 2 2h in the middle;
(5) Taking out the wood block, washing with deionized water, and freeze-drying for 12h;
(6) Directly annealing the chemically treated wood blocks in argon at 600 ℃ to obtain carbon sponge;
(7) Soaking the carbon sponge in 50% phosphoric acid for 2h, drying, and then putting into a vacuum oven for drying to obtain a modified carbon sponge;
(8) Preparing silver nanowire ethanol solution with the mass concentration of 0.2mg/mL, soaking the silver nanowire ethanol solution into the modified carbon sponge by using a pulse vacuum method under the room temperature condition, wherein the vacuum degree is 0.08MPa, and the treatment time is 15min;
(9) Taking out, and putting into a baking oven for baking;
(10) And crushing to obtain the silver-doped 3D conductive filler.
The preparation method of the high-toughness conductive nylon material comprises the following preparation steps:
s1: all raw materials were placed in a vacuum oven and left to dry overnight;
s2: putting the mixture into a single screw extruder, carrying out melt extrusion and blending twice, wherein the temperature of the screw is set to 265/270/270/270 ℃, and the rotating speed of the screw is set to 80rpm;
s3: and (3) carrying out injection molding on the extruded particles in an injection molding machine to obtain the composite material, wherein the injection molding temperature is 255/260/270/270/270 ℃ and the mold temperature is 80 ℃.
Comparative example 1
The difference between this example and example 6 is that the particle size of the silver-doped 3D conductive filler is different, specifically:
the high-toughness conductive nylon material comprises the following components: 50 parts of nylon 6, 45 parts of polyphenyl ether, 3 parts of maleic anhydride grafted polyolefin elastomer, 15 parts of silver-doped 3D conductive filler with the particle size of 13-74 mu m, and 5 parts of magnesia alumina spinel whisker with the diameter of 1-8 mu m and the length-diameter ratio of 20.
The preparation method of the silver-doped 3D conductive filler comprises the following steps:
(1) Preparing 2.5mol/L NaOH and 0.4mol/L Na 2 SO 3 Boiling the mixed solution at 170 ℃;
(2) Weighing square wood blocks with side length of 3cm, and placing the square wood blocks into the mixed solution for 6 hours to carry out lignin removal and hemicellulose treatment;
(3) Taking out the wood block, and cleaning the wood block to be neutral by boiled deionized water;
(4) Configuring 3mol/L H 2 O 2 Placing the cleaned wood block into boiling H 2 O 2 2h in the middle;
(5) Taking out the wood block, washing with deionized water, and freeze-drying for 12h;
(6) Directly annealing the chemically treated wood blocks in argon at 600 ℃ to obtain carbon sponge;
(7) Soaking the carbon sponge in 50% phosphoric acid for 2h, drying, and then putting into a vacuum oven for drying to obtain a modified carbon sponge;
(8) Preparing silver nanowire ethanol solution with the mass concentration of 0.2mg/mL, soaking the silver nanowire ethanol solution into the modified carbon sponge by using a pulse vacuum method under the room temperature condition, wherein the vacuum degree is 0.08MPa, and the treatment time is 15min;
(9) Taking out, and putting into a baking oven for baking;
(10) And crushing to obtain the silver-doped 3D conductive filler.
The preparation method of the high-toughness conductive nylon material comprises the following preparation steps:
s1: all raw materials were placed in a vacuum oven and left to dry overnight;
s2: putting the mixture into a single screw extruder, carrying out melt extrusion and blending twice, wherein the temperature of the screw is set to 265/270/270/270 ℃, and the rotating speed of the screw is set to 80rpm;
s3: and (3) carrying out injection molding on the extruded particles in an injection molding machine to obtain the composite material, wherein the injection molding temperature is 255/260/270/270/270 ℃ and the mold temperature is 80 ℃.
Comparative example 2
This example differs from example 6 in that it does not contain magnesia alumina spinel whiskers, in particular:
the high-toughness conductive nylon material comprises the following components: 50 parts of nylon 6, 45 parts of polyphenyl ether, 3 parts of maleic anhydride grafted polyolefin elastomer and 15 parts of silver-doped 3D conductive filler with the particle size of 13-18 mu m.
The preparation method of the silver-doped 3D conductive filler comprises the following steps:
(1) Preparing 2.5mol/L NaOH and 0.4mol/L Na 2 SO 3 Boiling the mixed solution at 170 ℃;
(2) Weighing square wood blocks with side length of 3cm, and placing the square wood blocks into the mixed solution for 6 hours to carry out lignin removal and hemicellulose treatment;
(3) Taking out the wood block, and cleaning the wood block to be neutral by boiled deionized water;
(4) Configuring 3mol/L H 2 O 2 Placing the cleaned wood block into boiling H 2 O 2 2h in the middle;
(5) Taking out the wood block, washing with deionized water, and freeze-drying for 12h;
(6) Directly annealing the chemically treated wood blocks in argon at 600 ℃ to obtain carbon sponge;
(7) Soaking the carbon sponge in 50% phosphoric acid for 2h, drying, and then putting into a vacuum oven for drying to obtain a modified carbon sponge;
(8) Preparing silver nanowire ethanol solution with the mass concentration of 0.2mg/mL, soaking the silver nanowire ethanol solution into the modified carbon sponge by using a pulse vacuum method under the room temperature condition, wherein the vacuum degree is 0.08MPa, and the treatment time is 15min;
(9) Taking out, and putting into a baking oven for baking;
(10) And crushing to obtain the silver-doped 3D conductive filler.
The preparation method of the high-toughness conductive nylon material comprises the following preparation steps:
s1: all raw materials were placed in a vacuum oven and left to dry overnight;
s2: putting the mixture into a single screw extruder, carrying out melt extrusion and blending twice, wherein the temperature of the screw is set to 265/270/270/270 ℃, and the rotating speed of the screw is set to 80rpm;
s3: and (3) carrying out injection molding on the extruded particles in an injection molding machine to obtain the composite material, wherein the injection molding temperature is 255/260/270/270/270 ℃ and the mold temperature is 80 ℃.
Tensile property test: the tensile properties of the samples were determined using a universal material tester and were carried out at room temperature according to the GB/T16421-1996 standard, the dumbbell-shaped samples having dimensions of 75X 4X 2mm 3 The stretching rate was 10mm/min.
HDT test: the HDT of the sample was measured using a heat distortion/Vicat tester, according to GB/T1634.1-2019, the sample size being 80X 10X 4mm 2 The initial temperature is 20 ℃, the temperature rising rate is 120 ℃/h, and the test pressure is 1.8MPa. Testing the notch impact strength of the cantilever beam: the sample was tested for notched Izod impact strength using a pendulum impact machine, performed at room temperature according to GB/T1843-2008 standard, using a 4J pendulum, with an initial sample size of 80X 10X 4mm 3 V-shaped notch with depth of 2mm.
Table 1 characterization of mechanical properties of the example materials
Volume resistivity test: the measurement was carried out according to GB/T1410-2006 standard.
Table 2 characterization of the conductivity properties of the example materials
Claims (5)
1. The high-toughness conductive nylon material is characterized by comprising the following components: 50 parts of nylon 6, 40-45 parts of polyphenyl ether, 2-3 parts of maleic anhydride grafted polyolefin elastomer, 10-15 parts of conductive filler and 2-5 parts of magnesia alumina spinel whisker;
the conductive filler is silver-doped 3D conductive filler, the particle size of the silver-doped 3D conductive filler is 13-18 mu m, and the preparation method of the silver-doped 3D conductive filler comprises the following steps:
(1) Preparing 2.5mol/L NaOH and 0.4mol/L Na 2 SO 3 Boiling the mixed solution at 170 ℃;
(2) Weighing square wood blocks with side length of 3cm, and placing the square wood blocks into the mixed solution for 6 hours to carry out lignin removal and hemicellulose treatment;
(3) Taking out the wood block, and cleaning the wood block to be neutral by boiled deionized water;
(4) Configuring 3mol/L H 2 O 2 Placing the cleaned wood block into boiling H 2 O 2 2h in the middle;
(5) Taking out the wood block, washing with deionized water, and freeze-drying for 12h;
(6) Directly annealing the chemically treated wood blocks in argon at 400-600 ℃ to obtain carbon sponge;
(7) Soaking the carbon sponge in 50% phosphoric acid for 1-2h, drying, and drying in a vacuum oven to obtain a modified carbon sponge;
(8) Preparing silver nanowire ethanol solution, and soaking the silver nanowire ethanol solution into the modified carbon sponge by using a pulse vacuum method for 10-15min;
(9) Taking out, and putting into a baking oven for baking;
(10) Crushing to obtain silver-doped 3D conductive filler;
the diameter of the magnesia-alumina spinel whisker is 1-8 mu m, and the length-diameter ratio is 20.
2. The high-toughness conductive nylon material according to claim 1, wherein the mass concentration of the silver nanowire ethanol solution is 0.1-0.2mg/mL.
3. The high-toughness conductive nylon material according to claim 1, wherein the pulsed vacuum process is performed at room temperature and the vacuum degree is 0.08MPa.
4. The method for preparing the high-toughness conductive nylon material according to claim 1, wherein the preparation steps are as follows:
s1: all raw materials were placed in a vacuum oven and left to dry overnight;
s2: putting the mixture into a single screw extruder, carrying out melt extrusion and blending twice, wherein the temperature of the screw is set to 265/270/270/270 ℃, and the rotating speed of the screw is set to 80rpm;
s3: and (5) carrying out injection molding on the extruded particles in an injection molding machine to obtain the composite material.
5. The method for preparing a high-toughness conductive nylon material according to claim 4, wherein the injection molding temperature in S3 is set to 255/260/270/270/270 ℃ and the mold temperature is set to 80 ℃.
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