KR20130047031A - The method and facility that is able to make recycled polytetrafluoroethylene powder with nano meter size through gamma rays and basket mill - Google Patents
The method and facility that is able to make recycled polytetrafluoroethylene powder with nano meter size through gamma rays and basket mill Download PDFInfo
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- KR20130047031A KR20130047031A KR20110111792A KR20110111792A KR20130047031A KR 20130047031 A KR20130047031 A KR 20130047031A KR 20110111792 A KR20110111792 A KR 20110111792A KR 20110111792 A KR20110111792 A KR 20110111792A KR 20130047031 A KR20130047031 A KR 20130047031A
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- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
- B29B17/04—Disintegrating plastics, e.g. by milling
- B29B17/0404—Disintegrating plastics, e.g. by milling to powder
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- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/28—Treatment by wave energy or particle radiation
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/18—Homopolymers or copolymers or tetrafluoroethene
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- 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
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/52—Mechanical processing of waste for the recovery of materials, e.g. crushing, shredding, separation or disassembly
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
Description
본 발명은 고분자 개질을 통한 폐 폴리테트라플루오로에틸렌을 나노미터 크기로 분말화하는 방법에 관한 것으로서, 더욱 상세하게는 현재 주로 농수축산물 원료 또는 가공식품들의 살균 또는 살충과 의료용구 및 의료용품들의 멸균 등에 주로 사용되는 코발트-60 방사성동위원소에서 나오는 단파장 빛인 감마선을 이용하여 온도상승 없이 고분자 물질의 화합적 결합구조를 변화시켜 폐폴리테트라플루오로에틸렌의 주쇄부분을 끊기 용이한 저분자량 상태로 개질하고 바스켓밀 분쇄기를 이용하여 습식상태에서 마이크로미터 이하 수백나노미터 크기의 폴리테트라플루오로에틸렌 슬러지를 생산하고 건조하여, 최종적으로 건식분쇄 장치를 이용하여 나노미터 크기의 폴리테트라플루오로에틸렌 분말화 장치 및 그 방법에 관한 것이다. The present invention relates to a method for powdering waste polytetrafluoroethylene to nanometer size through polymer modification, and more particularly, currently sterilization or insecticide of agricultural livestock products or processed foods and sterilization of medical equipment and medical supplies. By using gamma rays, short-wavelength light emitted from cobalt-60 radioisotope, which is mainly used in the back, the compound structure of polymer polyether is changed to low molecular weight state without breaking the temperature, and the main chain of waste polytetrafluoroethylene is easily broken. Polytetrafluoroethylene sludge having a size of several hundred nanometers or less in micrometers in a wet state using a basket mill grinder and dried, and finally, a nanometer-sized polytetrafluoroethylene powdering apparatus using a dry mill It's about how.
본 발명은 PTFE 표면의 개질방법에 관한 것으로서, 더욱 상세하게는 단파장 빛인 감마선을 이용하여 강력한 투과력을 지닌 방사선으로 온도상승 없이 고분자 물질의 화합적 결합구조를 변화시켜 보다 안정한 구조로 전화시키거나 원하는 물성으로 개질할 수 있는 방법을 이용하여 폐폴리테트라플루오로에틸렌의 주쇄부분을 끊기 용이한 저분자량 상태로 개질하고 바스켓밀 분쇄기를 이용하여 습식상태에서 마이크로미터 이하 수백나노미터 크기의 폴리테트라플루오로에틸렌 분말화 장치 및 그 방법에 관한 것이다. The present invention relates to a method for modifying the surface of PTFE, and more particularly, using a short-wavelength light gamma rays to change the coupling structure of the polymer material to a more stable structure without changing the temperature to the radiation having a strong permeability, without increasing the temperature or desired physical properties Polytetrafluoroethylene of up to several hundred nanometers in size under micrometers in a wet state by modifying the main chain portion of the waste polytetrafluoroethylene using a method capable of A powdering apparatus and a method thereof.
불소계수지란 탄소골격과 불소원자로 이루어진 합성수지로 대표적으로 알려진 불소수지는 PTFE,FEP,PFA,PVDF 가 대표적이며, 그 중에서 가장 많이 사용되고 있는 불소수지가 폴리테트라플루오로에틸렌(PTFE)이다. 폴리테트라플루오로에틸렌은 미국 듀퐁(DUPONT)사에서 처음 개발한 것으로 테프론이라는 제품명으로 더 잘 알려져 있다.Fluorine resin is a fluorocarbon resin known as a synthetic resin composed of carbon skeleton and fluorine atoms, and PTFE, FEP, PFA, PVDF are representative of the fluorine resin, the most commonly used fluorine resin is polytetrafluoroethylene (PTFE). Polytetrafluoroethylene was first developed by DUPONT in the United States and is better known under the product name Teflon.
불소는 전기음성도가 가장 큰 원소로 반응성이 크고 전자밀도가 높으며, 수소에 비하여 원자반경이 크다 이로 인해 불소계 수지는 화학적, 물리적 안정성을 띄게 되는데 이는 내열성, 내약품성이 뛰어나 고성능을 나타내게 되며, 자기윤활성, 비점착성, 전기절연성, 고주파특성이 우수하여 고기능성을 겸비한 엔지니어링플라스틱에 적합하다. 이러한 기능으로 인하여 불소계 수지는 전기전자재료, 기계재료, 생산설비에서의 내식성 방지를 위한 라이닝, 항공기재료, 기능성 섬유원료, 프라이팬등의 조리도구 등에 범용적으로 사용되고 있다. 폴리플루오로에틸렌은 연속사용온도는 260℃이고 저온(-268℃)에서 고온까지 안정된 상태에서 사용할 수 있다. Fluorine is the most electron-negative element, which has high reactivity, high electron density, and large atomic radius compared to hydrogen. As a result, fluorine resin has chemical and physical stability, which shows high performance due to its excellent heat resistance and chemical resistance. It has excellent lubricity, non-adhesiveness, electrical insulation and high frequency characteristics, making it suitable for engineering plastics with high functionality. Due to these functions, fluorine-based resins are widely used in electrical and electronic materials, mechanical materials, lining for preventing corrosion resistance in production facilities, aircraft materials, functional fiber raw materials, and cooking tools such as frying pans. Polyfluoroethylene can be used in a stable condition from 260 ° C continuous temperature to low temperature (-268 ° C).
그러나 제품 생산시 압축성형, 절삭 등 기계가공법이 많이 사용되어 가공할 때 원료의 폐기물이 발생한다. 이렇게 발생된 폐폴리테트라플루오로에틸렌 폐기물은 아주 소량만이 재활용되고 있다.However, in the production of the product, a lot of machining methods such as compression molding and cutting are used, and the waste of raw materials is generated when processing. Only a small amount of the waste polytetrafluoroethylene waste thus produced is recycled.
일반적으로 폴리테트라플루오로에틸렌을 분말화하는 방법으로는 대한민국 공개특허 제2001-0024038호 또는 대한민국 공개특허 제1999-0067072호와 같이 유화중합법에 의해 폴리머라텍스를 얻고, 그 후 응석할 때에, 라텍스중에 계면활성제를 첨가하여 응석하는 방법으로 폴리테트라플루오로에틸렌 분말을 제조할 수 있다. 그러나 상기 기술을 응용하더라도 본 발명처럼 폐폴리테트라플루오로에틸렌을 재활용할 수 없다. In general, as a method of powdering polytetrafluoroethylene, the latex is obtained when the polymer latex is obtained by emulsion polymerization method as disclosed in Korean Patent Laid-Open Publication No. 2001-0024038 or Korean Patent Publication No. 1999-0067072, and then coagulated thereafter. The polytetrafluoroethylene powder can be manufactured by the method of adding a surfactant in and coagulating. However, even if the above technique is applied, waste polytetrafluoroethylene cannot be recycled as in the present invention.
일반적으로 폴리테트라플루오로에틸렌을 분말화하는 방법으로는 대한민국 공개특허 제2008-0105946호와 같이 전자빔을 이용하여 분자결합구조를 끊고 ACM 기기를 이용한 건식분쇄 방법으로 마이크로미터 크기의 폴리테트라플루오로에틸렌 분말을 제조할 수 있다. 그러나 상기 기술을 응용하더라도 본 발명처럼 폐폴리테트라플루오로에틸렌을 나노미터크기로 재활용할 수 없다.In general, a method of powdering polytetrafluoroethylene is a micrometer-sized polytetrafluoroethylene by a method of breaking the molecular bond structure using an electron beam and dry grinding using an ACM device as shown in Korean Patent Publication No. 2008-0105946. Powders can be prepared. However, even if the above technology is applied, waste polytetrafluoroethylene cannot be recycled to nanometer size like the present invention.
다른 방법으로는 대한민국 공개특허 제2002-0006344호에 따른 폴리테트라플루오로에틸렌을 5torr미만의 압력 및 500℃이상의 온도에서 열분해하여 고분자 사슬을 절단하는 방법이 있다. 하지만 열분해를 이용한 방법은 폴리테트라플루오로에틸렌이 순간적으로 열분해가 되는 것이 아니기 때문에 장시간 고온과 진공상태를 유지해 주어야 하는 등 공정이 복잡하고 에너지 소모가 많은 문제점이 있다.As another method, a polytetrafluoroethylene according to Korean Patent Laid-Open Publication No. 2002-0006344 is thermally decomposed at a pressure of less than 5 torr and a temperature of 500 ° C. or more to cut polymer chains. However, the method using pyrolysis does not instantaneously pyrolyze polytetrafluoroethylene, so the process is complicated and energy consuming such as maintaining high temperature and vacuum for a long time.
대한민국 공개특허공보 제 2002-0011822호에는 고분자의 발수막 코팅을 위한 표면 개질 방법을 개시하고 있으나, 실시예에서는 폴리카보네이트에 대한 표면개질만을 개시하고 있으며, 접촉각 향상의 효과만을 기술하고 있는데, 이 접촉각의 향상이 극성 작용기에 의한 것인지 아니면 고분자재 표면에 물리적 손상에 의해서 향상된 것인지 전혀 기재되어 있지 않다. 또한, 상기 공보에 개시되어 있는 바와 같이, 이온빔으로서 아르곤이온빔을 사용하고, 반응성 가스로서 산소를 사용하는 경우에는 금속막과의 접촉력은 향상시킬 수 있지만, 금속막의 표면상태가 열악해진다는 문제점이 있다.Korean Patent Laid-Open Publication No. 2002-0011822 discloses a surface modification method for coating a water repellent membrane of a polymer, but the embodiment discloses only surface modification for polycarbonate, and describes only the effect of improving the contact angle. It is not described at all whether the improvement is due to the polar functional group or the physical damage to the surface of the polymer material. Further, as disclosed in the above publication, when argon ion beam is used as the ion beam and oxygen is used as the reactive gas, the contact force with the metal film can be improved, but there is a problem that the surface state of the metal film becomes poor. .
US 특허 No. 6,203,733은 물과 퍼플루오로알킬 알킬 에테르를 함유하는 액상 매질로 PTFE 분말을 응고시킴에 의한 입상 PTFE 분말의 제조 방법을 개시하고 있다. PTFE 1차 분말을 액상 매질과 혼합한 다음 일정 강도로 교반하여 목적하는 응고도 및 제립도를 성취한다.US Patent No. 6,203,733 discloses a process for preparing granular PTFE powder by coagulating the PTFE powder in a liquid medium containing water and perfluoroalkyl alkyl ethers. The PTFE primary powder is mixed with the liquid medium and then stirred to a certain strength to achieve the desired degree of solidification and granulation.
US 특허 No. 4,370,436 및 5,321,059는 미분 PTFE 입자와 표면-처리된 충진제를, 수-혼화성 유기 액체를 포함하는 수성 매질에서 교반함에 의한 충진된 응집 PTFE 성형 분말의 제조 방법을 개시하고 있다.US Patent No. 4,370,436 and 5,321,059 disclose methods for making filled aggregated PTFE molded powders by stirring finely divided PTFE particles and surface-treated fillers in an aqueous medium comprising a water-miscible organic liquid.
US 특허 No. 6,197,862는 PTFE 분말, 충진제, 및 물을 유기 액체와 비-이온계 용매의 존재하에 교반함에 의한 충진된 PTFE 입상 분말의 제조 방법을 개시하고 있다.US Patent No. 6,197,862 discloses a process for preparing filled PTFE granular powders by stirring PTFE powder, fillers, and water in the presence of organic liquids and non-ionic solvents.
US 특허 No. 6,281,281은 PTFE 분말과 충진제의 혼합물 100 중량부를 규정 농도의 음이온계 계면활성제를 함유하는 수용액 30 내지 60 중량부로 습윤시킴에 의한, 충진된 PTFE의 입상 분말의 제조 방법을 개시하고 있다.US Patent No. 6,281,281 discloses a process for the preparation of granular powder of filled PTFE by moistening 100 parts by weight of a mixture of PTFE powder and filler to 30 to 60 parts by weight of an aqueous solution containing a defined concentration of anionic surfactant.
US 특허 No. 6,350,801은 물과 액체-액체 계면을 형성하는 유기 액체와 비이온계 계면활성제를 사용하여 PTFE 분말과 충진제의 수성 슬러리를 형성시킨 다음 교반 및 해응집과 병행하여 입상화함에 의한, 충진된 입상 PTFE 분말의 제조 방법을 개시하고 있다.US Patent No. 6,350,801 is filled granular PTFE powder by forming an aqueous slurry of PTFE powder and filler using an organic liquid and a nonionic surfactant forming a water-liquid-liquid interface and then granulating in parallel with stirring and deagglomeration. The manufacturing method of this is disclosed.
US 특허 No. 3,597,405는 중합체 분말을 표면 장력이 낮은 소량의 액체로 습윤시킨 다음 습윤 분말을 예를 들면, 텀블링 작업에 의해 응집체로 형성시키는 응집 방법을 기재하고 있다. 응집체 형성 후, 액체는 가열에 의해 제거된다.US Patent No. 3,597,405 describes agglomeration methods in which the polymer powder is wetted with a small amount of liquid with low surface tension and then the wet powder is formed into agglomerates, for example by a tumbling operation. After formation of the aggregate, the liquid is removed by heating.
US 특허 No. 3,682,859는 테트라플루오로에틸렌 중합체를 유기 액체로 습윤시키는 유사 방법을 개시하고 있다.US Patent No. 3,682,859 discloses a similar process for wetting tetrafluoroethylene polymers with organic liquids.
US 특허 No. 3,882,217은 테트라플루오로에틸렌 중합체 산물을 응집에 앞서서 소량의 휘발성 비-이온계 계면활성제의 수용액으로 습윤시키는 응집 방법을 기재하고 있다. US Patent No. 3,882,217 describes a flocculation method in which the tetrafluoroethylene polymer product is wetted with an aqueous solution of a small amount of volatile non-ionic surfactant prior to flocculation.
US 특허 No. 3,983,200은 테트라플루오로에틸렌 중 합체를 보호성 콜로이드를 함유하는 수용액으로 먼저 습윤시키는 방법을 개시하고 있다.US Patent No. 3,983,200 discloses a method of first wetting a tetrafluoroethylene polymer with an aqueous solution containing a protective colloid.
따라서, 본 발명의 목적은 스크랩이나 시트형태의 폐폴리테트라플루오르에틸렌을 감마선조사가 가능한 미세분말형태로 가공하고 고분자의 분자량을 줄여 1차 습식분쇄 및 2차 건식분쇄를 통해 나노미터 크기의 폐폴리테트라플루오르에틸렌 분말화 방법을 제공함에 목적이 있다.Accordingly, an object of the present invention is to process waste polytetrafluoroethylene in the form of scrap or sheet into a fine powder that can be gamma-irradiated, and reduce the molecular weight of the polymer to reduce waste molecular weight of the nanometer through primary wet grinding and secondary dry grinding. It is an object to provide a tetrafluoroethylene powdering method.
상기한 목적을 달성하기 위하여, 폐폴리테트라플루오로에틸렌을 감마선조사가 용이하기 위한 조분쇄단계; 상기 조분쇄된 페폴리테트라플루오로에틸렌의 고분자 개질을 위한 감마선 조사; 감마선조사 되어 분자량이 저감된 개질된 페폴리테트라플루오로에틸렌을 나노미터사이즈로 습식 분쇄하기 위한 단계; 나노미터 크기로 습식분쇄된 페폴리테트라플루오로에틸렌의 건조단계; 건조된 폐폴리테트라플루오로에틸렌 덩어리를 나노미터 파우더로 건식 분산 분쇄시키는 단계를 제공하는데 있다. In order to achieve the above object, coarse grinding step to facilitate gamma irradiation of waste polytetrafluoroethylene; Gamma irradiation for polymer modification of the co-pulverized pepolytetrafluoroethylene; Gamma irradiation to wet mill the modified pepolytetrafluoroethylene having a reduced molecular weight to nanometer size; Drying the wet milled pepolytetrafluoroethylene to nanometer size; It is to provide a step of dry dispersion grinding the dried waste polytetrafluoroethylene chunks into nanometer powder.
상술한 바와 같이, 본 발명의 감마선을 이용한 고분자 개질을 통하여 폴리테트라플루오로에틸렌의 분자결합구조를 끊음으로써 스크랩 형태의 폐폴리테트라플루오로에틸렌을 나노미터 크기로 분말화할 수 있는 효과기 있으며, 감사선량 및 분쇄시간을 조절함으로써 나노미터 분말 크기를 조절할 수 있는 효과가 있다.As described above, by breaking the molecular bond structure of the polytetrafluoroethylene through the polymer modification using the gamma ray of the present invention, there is an effector capable of powdering the waste polytetrafluoroethylene in the form of scrap to nanometer size, And by controlling the grinding time has the effect of adjusting the nanometer powder size.
도 1은 본 발명의 일실시예에 따른 주요 장치 구성도
도 2 및 도3은 본 발명의 일실시예에 따른 폴리테트라플루오로에틸렌 입도분포도1 is a block diagram of a main device according to an embodiment of the present invention;
2 and 3 is a particle size distribution diagram of polytetrafluoroethylene according to an embodiment of the present invention
본 명세서 및 청구범위에 사용된 용어나 단어는 통상적이거나 사전적인 의미로 한정해서 해석되어서는 아니되며, 발명자는 그 자신의 발명을 가장 최선의 방법으로 설명하기 위해 용어의 개념을 적절하게 정의할 수 있다는 원칙에 입각하여 본 발명의 기술적 사상에 부합하는 의미와 개념으로 해석되어야만 한다.The terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms and the inventor may appropriately define the concept of the term in order to best describe its invention It should be construed as meaning and concept consistent with the technical idea of the present invention.
따라서, 본 명세서에 기재된 실시예와 도면에 도시된 구성은 본 발명의 가장 바람직한 일실시예에 불과할 뿐이고 본 발명의 기술적 사상을 모두 대변하는 것은 아니므로, 본 출원시점에 있어서 이들을 대체할 수 있는 다양한 균등물과 변형예들이 있을 수 있음을 이해하여야 한다. Therefore, the embodiments described in the specification and the drawings shown in the drawings are only one of the most preferred embodiments of the present invention and do not represent all of the technical idea of the present invention, various modifications that can be replaced at the time of the present application It should be understood that there may be equivalents and variations.
이하 첨부된 도면을 참조하여 본 발명의 바람직한 실시예를 상세히 설명하기로 한다Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.
도1은 본 발명의 일실시예에 따른 제조방법을 보인 공정도이다. 도 1을 참조하면 폐폴리테트라플루오로에틸렌 스크랩을 40kg을 감마선조사에 적합한 형태로 조분쇄하여 약1~5mm 크기의 flake 상태로 된다. flake 상태의 폐폴리테트라플루오로에틸렌을 Aluminium Carriers에 40kg을 적재하여 600KGy의 선량으로 방출되는 감마선 최대선량이 선원 판넬에 고루 분포되어 강력하게 침투되어 폐폴리테트라플루오로에틸렌의 분자사슬을 끊어 분자량을 줄이고 분쇄되기 쉬운 형태로 고분자개질 작업을 진행한다.1 is a process chart showing a manufacturing method according to an embodiment of the present invention. Referring to FIG. 1, 40 kg of waste polytetrafluoroethylene scraps are coarsely pulverized into a form suitable for gamma irradiation to form a flake of about 1 to 5 mm in size. The maximum dose of gamma-rays emitted from the 600kgy dose of 40kg of pulmonary waste polytetrafluoroethylene in aluminum carriers is evenly distributed in the source panel, which penetrates strongly and breaks the molecular chain of waste polytetrafluoroethylene. The polymer modification works in a form that is easy to reduce and crush.
고분자 개질된 폐폴리테트라플루오로에틸렌 40kg과 물 60kg을 바스켓밀에 넣고 지름 10mm 지르코늄볼 2kg, 지름 5mm 지르코늄볼 2kg, 지름 1mm 지르코늄볼 2kg, 지름 0.1~0.5mm가 혼용된 지르코늄볼 4kg을 넣고 90분간 분쇄를 거치면 <표1>과 <도2> 입도 분석된 결과와 같이 물에 분산된 평균입도(D50) 642nm 크기의 폴리테트라플루오로에틸렌 슬러지가 만들어 진다.Put 40 kg of polymer modified waste polytetrafluoroethylene and 60 kg of water into a basket mill, and then add 10 kg of
상기 평균입도 600~700nm 크기의 폴리테트라플루오로에틸렌 슬러지를 150도 건조기에 4시간 넣고 수분을 날려주어 덩어리 형태의 폴리테트라플루오로에틸렌을 얻을 수 있다. Polytetrafluoroethylene sludge having an average particle size of 600 to 700 nm is put in a 150 degree dryer for 4 hours to blow moisture to obtain polytetrafluoroethylene in the form of agglomerates.
상기 건조된 폴리테트라플루오로에틸렌을 건식분쇄가 가능한 Air zet mill 또는 ACM(Air Classification mill) 장치에 넣어 최종 분쇄하여 폴리테트라플루오로에틸렌 분말을 얻을수 있다. 이렇게 생산된 분말의 입자사이즈 분석을 위해 입도분석기로 입자크기를 측정하여 1마이크로 미만이면 포장하여 코팅용 제품으로 사용하고 1마이크로미터 이상이면 포장하여 잉크나 도료용 첨가제로 사용하거나, 습식분쇄를 다시 진행하여 1마이크로미터 미만크기의 분말 제품으로 재가공처리한다.The dried polytetrafluoroethylene is put into an air zet mill or an ACM (Air Classification mill) device capable of dry grinding, and finally pulverized to obtain a polytetrafluoroethylene powder. In order to analyze the particle size of the powder thus produced, the particle size is measured using a particle size analyzer, and if it is less than 1 micrometer, it is packaged and used as a coating product. Proceed and reprocess into powder products less than 1 micrometer in size.
<표2>와 <도3>는 상기에서 건조된 폴리테트라플루오로에틸렌을 ACM 장치를 통해 최종분쇄하여 평균입도 사이즈를 346nm로 만든 입도분석자료이다. <Table 2> and <Figure 3> is a particle size analysis data of the final particle size of the dried polytetrafluoroethylene through an ACM device to make an average particle size of 346nm.
상술한 바와 같이 본 발명의 바람직한 제조예 및 실시예를 참조하여 설명하였지만 해당 기술분야의 숙련된 당업자라면 하기의 특허청구의 범위에 기재된 본 발명의 사상 및 영역으로부터 벗어나지 않는 범위 내에서 본 발명을 다양하게 수정 및 변경 시킬 수 있음을 이해할 수 있을 것이다. As described above, the present invention has been described with reference to the preferred preparations and examples, but those skilled in the art can vary the present invention without departing from the spirit and scope of the present invention as set forth in the claims below. It will be understood that modifications and changes can be made.
도1은 본 발명의 일시시예에 따른 제조방법을 보인 공정도
도2, 도3은 본 발명의 일시시예에 따른 폴리테트라플루오로에틸렌 입도분포도1 is a process chart showing a manufacturing method according to a temporary embodiment of the present invention
2 and 3 is a particle size distribution diagram of polytetrafluoroethylene according to one embodiment of the present invention
Claims (8)
상기 조분쇄된 폴리테트라플루오로에틸렌 flake의 고분자 개질을 위한 감마선조사기:
상기 감마선 조사기에 의해 고분자개질된 폴리테트라플루오로에틸렌을 습식분쇄하기 위한 습식분쇄기:
습식 분쇄되어 슬러지 형태의 폴리테트라플루오로에틸렌을 건조하기 위한 건조기: 및 건조된 덩어리를 건식분쇄하기 위한 건식분쇄기 및 분급화 장치
를 포함하는 감마선 조사를 이용한 고분자개질을 통한 폴리테트라플루오로에틸렌의 나노미터 크기의 분말화 장치 Mill for Flake co-pulverization of waste polytetrafluoroethylene:
Gamma irradiator for polymer modification of the co-pulverized polytetrafluoroethylene flake:
Wet mill for wet milling polymer-modified polytetrafluoroethylene by the gamma irradiator:
Dryer for wet grinding to dry polytetrafluoroethylene in sludge form: and a dry mill and classification apparatus for dry milling the dried mass
Nanometer-sized powdering apparatus of polytetrafluoroethylene through polymer modification using gamma irradiation
폐폴리테트라플루오로에틸렌 스크랩을 분쇄기를 통하여서 0.5~10mm 크기의 flake 상태로 조절하는 폐폴리테트라플루오로에틸렌의 슬러지를 제조하는 감마선을 이용한 폐폴리테트라플루오로에틸렌의 분말화 장치The method of claim 1,
Pulverizing apparatus for waste polytetrafluoroethylene using gamma rays for producing sludge of waste polytetrafluoroethylene which controls waste polytetrafluoroethylene scrap into a flake state of 0.5 to 10 mm in size through a mill
감마선 조사기를 통하여서 감마선 조사량을 100kGy 내지 1100kGy로 조절하는 폐폴리테트라플루오로에틸렌의 슬러지를 제조하는 감마선을 이용한 폐폴리테트라플루오로에틸렌의 분말화 장치The method of claim 1,
Pulverizing apparatus for waste polytetrafluoroethylene using gamma rays for producing sludge of waste polytetrafluoroethylene which controls the gamma radiation dose from 100 kGy to 1100 kGy through a gamma ray irradiator
습식분쇄시 지름 0.1~10mm 크기의 지르코니아볼 또는 세라믹볼 등의 습식용 볼을 이용하여 폐폴리테트라플루오로에틸렌의 슬러지를 제조하는 감마선을 이용한 폐폴리테트라플루오로에틸렌의 분말화 장치The method of claim 1,
Powder milling apparatus for waste polytetrafluoroethylene using gamma rays for producing sludge of waste polytetrafluoroethylene using wet balls such as zirconia balls or ceramic balls having a diameter of 0.1 to 10 mm during wet grinding
건식분쇄시 Air zet mill 또는 Air Classification mill 장치를 이용하여 폐폴리테트라플루오로에틸렌의 슬러지를 제조하는 감마선을 이용한 폐폴리테트라플루오로에틸렌의 분말화 장치The method of claim 1,
Powder milling device for waste polytetrafluoroethylene using gamma rays for producing sludge of waste polytetrafluoroethylene using air zet mill or air classification mill
상기 조분쇄된 폴리테트라플루오로에틸렌 flake를 고분자 개질을 위해 감마선을 조사하는 단계 ;
상기 감마선 조사기에 의해 고분자개질된 폴리테트라플루오로에틸렌을 습식분쇄하는 단계 ;
습식 분쇄된 슬러지 형태의 폴리테트라플루오로에틸렌을 건조하는 단계 ;
건조된 덩어리를 건식분쇄 및 분급화하는 단계 ;
를 포함하는 감마선 조사를 이용한 고분자개질을 통한 폴리테트라플루오로에틸렌의 나노미터 크기의 분말화 방법. Flake waste polytetrafluoroethylene with a coarsely mill;
Irradiating gamma rays for polymer modification of the coarsely pulverized polytetrafluoroethylene flake;
Wet grinding a polymer-modified polytetrafluoroethylene by the gamma-irradiator;
Drying the polytetrafluoroethylene in the form of wet milled sludge;
Dry grinding and classifying the dried mass;
Nanometer-sized powdering method of polytetrafluoroethylene through polymer modification using gamma irradiation.
상기 감마선 조사량을 100kGy 내지 1100kGy로 조절하는 폴리테트라플루오로에틸렌분말을 제조하는 감마선을 이용한 폐폴리테트라플루오로에틸렌의 분말화 방법The method according to claim 6,
A method for powdering waste polytetrafluoroethylene using gamma rays to prepare a polytetrafluoroethylene powder for adjusting the gamma radiation dose to 100 kGy to 1100 kGy
상기 폴리테트라플루오로에틸렌분말의 입자사이즈가 10nm 내지 1,000nm로 형성하는 폴리테트라플루오로에틸렌분말을 제조하는 감마선을 이용한 폐폴리테트라플루오로에틸렌의 분말화 방법
The method according to claim 6,
A method for powdering waste polytetrafluoroethylene using gamma rays for preparing a polytetrafluoroethylene powder having a particle size of the polytetrafluoroethylene powder of 10 nm to 1,000 nm.
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| JP2021014543A (en) * | 2019-07-12 | 2021-02-12 | ダイキン工業株式会社 | Method for producing low-molecular-weight polytetrafluoroethylene, and powder |
| KR102334324B1 (en) * | 2021-06-04 | 2021-12-07 | 주식회사 에스화인켐 | Method of preparing polytetrafluoroethylene powder and polytetrafluoroethylene powder prepared by the same |
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| JP2021014543A (en) * | 2019-07-12 | 2021-02-12 | ダイキン工業株式会社 | Method for producing low-molecular-weight polytetrafluoroethylene, and powder |
| JP7261422B2 (en) | 2019-07-12 | 2023-04-20 | ダイキン工業株式会社 | Method for producing low-molecular-weight polytetrafluoroethylene and powder |
| KR102334324B1 (en) * | 2021-06-04 | 2021-12-07 | 주식회사 에스화인켐 | Method of preparing polytetrafluoroethylene powder and polytetrafluoroethylene powder prepared by the same |
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