WO2015053476A1 - Procédé de fabrication de composition ayant des fonctions de des et d'iem - Google Patents

Procédé de fabrication de composition ayant des fonctions de des et d'iem Download PDF

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Publication number
WO2015053476A1
WO2015053476A1 PCT/KR2014/007918 KR2014007918W WO2015053476A1 WO 2015053476 A1 WO2015053476 A1 WO 2015053476A1 KR 2014007918 W KR2014007918 W KR 2014007918W WO 2015053476 A1 WO2015053476 A1 WO 2015053476A1
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Prior art keywords
composition
carbon nanotubes
molecular weight
weight polyethylene
high molecular
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PCT/KR2014/007918
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English (en)
Korean (ko)
Inventor
김기천
서정국
장인목
김태영
Original Assignee
(주)씨엔티솔루션
김기천
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Publication of WO2015053476A1 publication Critical patent/WO2015053476A1/fr

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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
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/005—Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered materials
    • 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
    • C08K3/04—Carbon
    • C08K3/041—Carbon nanotubes
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds
    • C08L101/12—Compositions of unspecified macromolecular compounds characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • 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
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00—Properties characterising the ingredient of the composition
    • C08L2207/06—Properties of polyethylene
    • C08L2207/068—Ultra high molecular weight polyethylene

Definitions

  • the present invention relates to a method for preparing a composition having ESD and EMI functions by dispersion stabilization of multi-walled carbon nanotubes using a metal catalyst and mixing with ultra high molecular weight polyethylene.
  • Carbon nanotube is a carbon form of a tube is combined with other carbon atoms and hexagonal honeycomb pattern to form a tube, the diameter of the tube is extremely small to the nanometer level, showing a unique electrochemical characteristics.
  • Carbon nanotubes have excellent mechanical properties, electrical selectivity, and excellent field emission characteristics.
  • shape of the semiconductor has the characteristics of the semiconductor and the energy gap varies depending on the diameter, it is attracting attention in the electronics, biotechnology, and medicine.
  • carbon nanotubes are being actively researched in the formation of conductive films and field emission displays (FEDs).
  • the present invention has been made to solve the above problems, an object of the present invention is to mix the carbon nanotubes and ultra high molecular weight polyethylene (ultra high molecular weight polyethylene), to quickly extinguish the external electromagnetic shock, the composition itself
  • the present invention provides a method for preparing a composition having ESD and EMI functions by suppressing electromagnetic energy to impart ESD and EMI functions to minimize damage.
  • the present invention as a means for solving the above problems, the step of preparing a multi-walled carbon nanotubes grown using a metal catalyst (S100);
  • the multi-walled carbon nanotubes undergo a pretreatment process (S200);
  • the present invention allows the multi-walled carbon nanotubes (MWCNT) grown by using a metal catalyst to undergo a pre-treatment process (DISPERSION), the size of the final purpose of the carbon nanotubes, Van Der The agglomeration of carbon nanotubes (CNT) by the Waals Force's 950 meV / nm energy is eliminated, and the aspect ratio can be determined and the short circuit contamination of the composition, which is the cause of conductivity and contamination, can be significantly controlled. .
  • MWCNT multi-walled carbon nanotubes
  • DISPERSION pre-treatment process
  • the present invention by mixing the carbon nanotubes with ultra high molecular weight polyethylene (ultra high molecular weight polyethylene) to give a conductive conductive properties, there is an effect that can freely generate the required ESD and EMI region.
  • ultra high molecular weight polyethylene ultra high molecular weight polyethylene
  • the present invention has the effect of enabling stable use in various fields by minimizing the deterioration of physical properties of the ultra high molecular weight polyethylene constituting the base of the composition.
  • FIG. 1 is a flow chart of one embodiment showing a method for manufacturing a composition having ESD and EMI functions in accordance with the present invention.
  • the present invention has the following features to achieve the above object.
  • the step of preparing a multi-walled carbon nanotubes grown using a metal catalyst (S100);
  • the multi-walled carbon nanotubes undergo a pretreatment process (S200);
  • the multi-walled carbon nanotubes have an aspect ratio of 5 nm to 15 nm in diameter and 100 nm to 300 nm in length.
  • the ultra-high molecular weight polyethylene is characterized in that the molecular weight of 4.0Mmg / mol ⁇ 10Mmg / mol.
  • the stirring mixture is rotated clockwise at a rotational speed of 200rpm / min, the internal temperature 30 °C 3 minutes, then rotates counterclockwise for 7 minutes at a rotational speed 500rpm / min, the internal temperature 50 °C Characterized in that the stirring mixture by the high speed mixer.
  • the composition is characterized in that it is added in a mixing ratio of 0.1 to 1% of the processed material 100%.
  • the workpiece in step S400 has an electrical surface resistance of 1.0E + 00 ⁇ 1.0E + 10 ⁇ / sq by the composition, the heat is applied to 180 °C ⁇ 230 °C characterized in that it is processed in the form of a plate or rod It is done.
  • the method of manufacturing a composition having ESD and EMI functions is a multi-walled carbon nanotubes (MWCNT) grown using a metal catalyst through the process (DISPERSION) process to the function of multi-walled carbon nanotubes
  • MWCNT multi-walled carbon nanotubes
  • DISPERSION process to improve the agglomeration of carbon nanotubes (CNT) by the size of the target, 950 meV / nm energy of Van Der Waals Force, and to determine the aspect ratio of 5nm to 15nm in diameter and 100nm to 300nm in length
  • the present invention relates to a manufacturing method for imparting electrical properties by mixing pinholes, roughness, and carbon nanotubes with reduced gas generation on the surface and inside of the composition with ultra high molecular weight polyethylene.
  • the manufacturing method for this is as follows.
  • the multi-walled carbon nanotubes have a predetermined size (aspect ratio of 5 nm to 15 nm in diameter and 100 nm to 300 nm in length), and Van Der Waals Force
  • the agglomeration of carbon nanotubes (CNT) by the energy of 950 meV / nm is improved, and the pinholes, roughness and gas generation on the surface and inside of the composition are suppressed, which will be described later.
  • CNT carbon nanotubes
  • Ultra High Molecular Weight Polyethylene UHMWPE
  • UHMWPE ultra high molecular weight polyethylene
  • UHMWPE ultra high molecular weight polyethylene
  • MWCNT multiwall carbon nanotubes
  • metal catalyst cobalt Co Ultra High Molecular Weight Polyethylene
  • UHMWPE ultra high molecular weight Polyethylene
  • MWCNT carbon nanotubes
  • DISPERSED products that have undergone the pretreatment process of carbon nanotubes, and DISPERSION-free products, respectively, are prepared and the performance is improved. The verification was confirmed as shown in Table 1 below.
  • composition with the multi-walled carbon nanotubes pretreated preliminarily for stabilization of dispersion did not cause roughness of the outer surface and the cross-section after cutting, or the generation of pinholes.
  • ultra high molecular weight polyethylene ultra high molecular weight polyethylene
  • the ultra high molecular weight polyethylene used at this time (4.0Mmg / mol ⁇ 10Mmg / mol) has a molecular weight of 4 million to 10 million.
  • the conductive material and the pre-processing multi-walled carbon nanotubes are stirred and mixed, and the multi-walled carbon nanotubes are uniformly dispersed in the ultra-high molecular weight polyethylene by the aforementioned pretreatment process. And mixing is possible.
  • the high speed mixer is a super high molecular weight polyethylene and a multi-walled carbon nanotube which are introduced into the first high speed mixer at a rotational speed of 200 rpm / min and an internal temperature of 30 ° C. for 3 minutes.
  • the electrical resistance can be freely set by the user and a predetermined value.
  • composition of the high molecular weight polyethylene and multi-walled carbon nanotubes has an ESD function, but may be subjected to a process of applying heat at an extrusion temperature of 180 ° C. to 230 ° C. after mixing.
  • Combination ratio of ultra high molecular weight polyethylene and ultra high molecular weight polyethylene (hereinafter referred to as 'MWCNT' for convenience of description) after the first pretreatment process is set to 99.8%: 0.2%, and the rotation direction is 200 rpm to the right through a high speed mixer. / min, the internal temperature of the mixer was set to 30 °C and rotated for 3 minutes, and then the direction of rotation was changed to the left, and the stirring speed was maintained for 7 minutes while maintaining the speed of the high speed mixer at 500 rpm and the mixer internal temperature of 50 °C.
  • the stirred composition was heated at 200 ° C. for 10 minutes at a pressure of 10 MPa in the mold to make a test piece to check the electrical resistance.
  • Combination ratio of ultra high molecular weight polyethylene and ultra high molecular weight polyethylene (hereinafter referred to as 'MWCNT' for convenience of description) after the first pretreatment process is set to 99.75%: 0.25%, and the rotation direction is 200 rpm to the right through a high speed mixer. / min, the internal temperature of the mixer was set to 30 degrees and rotated for 3 minutes, the direction of rotation was changed to the left, and the stirring speed was maintained for 7 minutes while maintaining the speed of the high speed mixer at 500rpm and the mixer internal temperature of 50 °C.
  • the stirred composition was heated at 200 ° C. for 10 minutes at a pressure of 10 MPa in the mold to make a test piece to check the electrical resistance.
  • Combination ratio of ultra high molecular weight polyethylene and ultra high molecular weight polyethylene (hereinafter referred to as 'MWCNT' for convenience of description) after the first pretreatment process is set to 99.7%: 0.3%, and the rotation direction is 200 rpm to the right through a high speed mixer. / min, the internal temperature of the mixer was set to 30 degrees and rotated for 3 minutes, the direction of rotation was changed to the left, and the stirring speed was maintained for 7 minutes while maintaining the speed of the high speed mixer at 500rpm and the mixer internal temperature of 50 °C.
  • the stirred composition was heated at 200 ° C. for 10 minutes at a pressure of 10 MPa in the mold to make a test piece to check the electrical resistance.
  • Combination ratio of ultra high molecular weight polyethylene and ultra high molecular weight polyethylene (hereinafter referred to as 'MWCNT' for convenience of description) after the first pretreatment process is set to 99.65%: 0.35%, and through the high speed mixer, the direction of rotation is 200rpm to the right. / min, the internal temperature of the mixer was set to 30 degrees and rotated for 3 minutes, the direction of rotation was changed to the left, and the stirring speed was maintained for 7 minutes while maintaining the speed of the high speed mixer at 500rpm and the mixer internal temperature of 50 °C.
  • the stirred composition was heated at 200 ° C. for 10 minutes at a pressure of 10 MPa in the mold to make a test piece to check the electrical resistance.
  • the combination ratio of ultra high molecular weight polyethylene and ultra high molecular weight polyethylene (hereinafter referred to as 'MWCNT' for convenience of description) after the first pretreatment process is set to 99.6%: 0.4%, and the rotation direction is 200 rpm to the right through a high speed mixer. / min, the internal temperature of the mixer was set to 30 degrees and rotated for 3 minutes, the direction of rotation was changed to the left, and the stirring speed was maintained for 7 minutes while maintaining the speed of the high speed mixer at 500rpm and the mixer internal temperature of 50 °C.
  • the stirred composition was heated at 200 ° C. for 10 minutes at a pressure of 10 MPa in the mold to make a test piece to check the electrical resistance.
  • Combination ratio of ultra high molecular weight polyethylene and ultra high molecular weight polyethylene (hereinafter referred to as 'MWCNT' for convenience of description) after the first pretreatment process is set to 99.55%: 0.45%, and the rotation direction is 200 rpm to the right through a high speed mixer. / min, the internal temperature of the mixer was set to 30 degrees and rotated for 3 minutes, the direction of rotation was changed to the left, and the stirring speed was maintained for 7 minutes while maintaining the speed of the high speed mixer at 500rpm and the mixer internal temperature of 50 °C.
  • the stirred composition was heated at 200 ° C. for 10 minutes at a pressure of 10 MPa in the mold to make a test piece to check the electrical resistance.
  • Combination ratio of ultra high molecular weight polyethylene and ultra high molecular weight polyethylene (hereinafter referred to as 'MWCNT' for convenience of description) after the first pretreatment process is set to 99.5%: 0.5%, and the rotation direction is 200 rpm to the right through a high speed mixer. / min, the internal temperature of the mixer was set to 30 degrees and rotated for 3 minutes, the direction of rotation was changed to the left, and the stirring speed was maintained for 7 minutes while maintaining the speed of the high speed mixer at 500rpm and the mixer internal temperature of 50 °C.
  • the stirred composition was heated at 200 ° C. for 10 minutes at a pressure of 10 MPa in the mold to make a test piece to check the electrical resistance.
  • Combination ratio of ultra high molecular weight polyethylene and ultra high molecular weight polyethylene (hereinafter referred to as 'MWCNT' for convenience of description) after the first pretreatment process is set to 99.45%: 0.55%, and through the high speed mixer, the direction of rotation is 200rpm to the right. / min, the internal temperature of the mixer was set to 30 degrees and rotated for 3 minutes, the direction of rotation was changed to the left, and the stirring speed was maintained for 7 minutes while maintaining the speed of the high speed mixer at 500rpm and the mixer internal temperature of 50 °C.
  • the stirred composition was heated at 200 ° C. for 10 minutes at a pressure of 10 MPa in the mold to make a test piece to check the electrical resistance.
  • Combination ratio of ultra high molecular weight polyethylene and ultra high molecular weight polyethylene (hereinafter referred to as 'MWCNT' for convenience of description) after the first pretreatment process is set to 99.4%: 0.6%, and the direction of rotation is 200 rpm to the right through a high speed mixer. / min, the internal temperature of the mixer was set to 30 degrees and rotated for 3 minutes, the direction of rotation was changed to the left, and the stirring speed was maintained for 7 minutes while maintaining the speed of the high speed mixer at 500rpm and the mixer internal temperature of 50 °C.
  • the stirred composition was heated at 200 ° C. for 10 minutes at a pressure of 10 MPa in the mold to make a test piece to check the electrical resistance.
  • the combination ratio of ultra high molecular weight polyethylene and ultra high molecular weight polyethylene (hereinafter referred to as 'MWCNT' for convenience of description) after the first pretreatment process is set to 99.35%: 0.65%, and through the high speed mixer, the direction of rotation is 200 rpm to the right. / min, the internal temperature of the mixer was set to 30 degrees and rotated for 3 minutes, the direction of rotation was changed to the left, and the stirring speed was maintained for 7 minutes while maintaining the speed of the high speed mixer at 500rpm and the mixer internal temperature of 50 °C.
  • the stirred composition was heated at 200 ° C. for 10 minutes at a pressure of 10 MPa in the mold to make a test piece to check the electrical resistance.
  • (1.0E + 00 ⁇ 01) 1.0 represents an integer and + is not-, and 00 to 01 represents a power of 0 to 10 of 1 in the sign of surface resistance.
  • the step of adding the composition to which the conductivity is imparted in the manufacture of the workpiece to prepare the workpiece in a predetermined shape (S400):
  • the composition to which the conductivity is imparted to the workpiece is added through the step S300 described above, and the workpiece itself is It has conductive properties, that is, the composition and the workpiece to which the composition is added have an electrical surface resistance of 1.0E + 00 to 1.0E + 10 ⁇ s / sq.
  • the workpiece to which the composition is added may be manufactured in various shapes in the form of a plate or rod by applying a heat of 180 °C ⁇ 230 °C, the mixing ratio of the composition added to the workpiece is 100% of the workpiece It is to be added in a mixing ratio of 0.1 ⁇ 1% of, and the processed material at this time may be a resin of various materials according to the purpose of use, the user's embodiment, the production of a composition for the purpose of having ESD and EMI functions Ramen can be a variety of materials.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

La présente invention porte sur un procédé de fabrication d'une composition ayant des fonctions de décharge électrostatique DES et d'interférence électromagnétique IEM et, plus particulièrement, sur un procédé de fabrication d'une composition ayant des fonctions de DES et d'IEM dans lequel un processus de dispersion est effectué sur des nanotubes de carbone multifeuillets (MWCNT) amenés à croître à l'aide d'un catalyseur métallique et ensuite les forces de Van Der Waals (qui représentent le plus gros problème en utilisant des nanotubes de carbone) sont réduites et, en même temps, du polyéthylène de masse moléculaire très élevée (UHMWPE) est mélangé avec les MWCNT pour permettre à une résistance électrique d'être librement réalisée. En raison de ces caractéristiques, le dispositif peut être protégé d'un choc électromagnétique externe divisant la capacité et être immunisé contre un endommagement provoqué par l'électricité statique et les ondes électromagnétiques.
PCT/KR2014/007918 2013-10-11 2014-08-26 Procédé de fabrication de composition ayant des fonctions de des et d'iem WO2015053476A1 (fr)

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KR20130121587A KR101378374B1 (ko) 2013-10-11 2013-10-11 Esd 및 emi 기능을 가지는 조성물 제조방법
KR10-2013-0121587 2013-10-11

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WO2015053476A1 true WO2015053476A1 (fr) 2015-04-16

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107630144A (zh) * 2017-10-12 2018-01-26 云南大学 一种聚三乙基苄基氯化铵丙胺多壁碳纳米管及制备和吸附[Pd(CN)4]2‑的方法

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KR20110101238A (ko) * 2009-01-09 2011-09-15 데이진 아라미드 비.브이. 내화 입자를 포함하는 초고분자량 폴리에틸렌

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JP4669876B2 (ja) * 2004-07-27 2011-04-13 ディーエスエム アイピー アセッツ ビー．ブイ． カーボンナノチューブ／超高分子量ポリエチレン複合繊維を製造するための方法
JP2008274060A (ja) * 2007-04-27 2008-11-13 Nano Carbon Technologies Kk 樹脂材料と導電性フィラーとの混合方法及び該方法により作製された複合材料及びマスターペレット
KR100873870B1 (ko) * 2007-12-24 2008-12-15 호남석유화학 주식회사 전기전도성을 갖는 탄소 나노 튜브/폴리올레핀 혼합 조성물및 그의 제조 방법
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107630144A (zh) * 2017-10-12 2018-01-26 云南大学 一种聚三乙基苄基氯化铵丙胺多壁碳纳米管及制备和吸附[Pd(CN)4]2‑的方法
CN107630144B (zh) * 2017-10-12 2019-04-19 云南大学 一种聚三乙基苄基氯化铵丙胺多壁碳纳米管及制备和吸附[Pd(CN)4]2-的方法

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