WO2014069911A1 - Technologie pour produire des mélanges maîtres de peroxyde, et procédé de reformage de polypropylène l'utilisant - Google Patents

Technologie pour produire des mélanges maîtres de peroxyde, et procédé de reformage de polypropylène l'utilisant Download PDF

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WO2014069911A1
WO2014069911A1 PCT/KR2013/009779 KR2013009779W WO2014069911A1 WO 2014069911 A1 WO2014069911 A1 WO 2014069911A1 KR 2013009779 W KR2013009779 W KR 2013009779W WO 2014069911 A1 WO2014069911 A1 WO 2014069911A1
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polypropylene
masterbatch
present
melt index
weight
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PCT/KR2013/009779
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English (en)
Korean (ko)
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정만협
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주식회사 만텍
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00—Chemical modification by after-treatment
    • C08F8/06—Oxidation
    • 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
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/01—Hydrocarbons
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/14—Peroxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2810/00—Chemical modification of a polymer
    • C08F2810/20—Chemical modification of a polymer leading to a crosslinking, either explicitly or inherently
    • 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
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/10—Homopolymers or copolymers of propene
    • 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
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/10—Homopolymers or copolymers of propene
    • 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
    • C08L23/10—Homopolymers or copolymers of propene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2310/00—Masterbatches

Definitions

  • the present invention relates to a peroxide masterbatch production technology and a polypropylene reforming method using the same.
  • Polypropylene is a relatively recently developed high quality resin that has been industrially produced since the late 1950s and occupies an important position among various resins developed to date.
  • the demand for polypropylene is still increasing day by day.
  • a Ziegler-Natta catalyst typically a complex salt consisting of titanium trichloride and diethylaluminum chloride
  • polypropylene can be synthesized by treating propylene at about 70 ° C. and 5 atm.
  • Polypropylene has an isotactic structure. Therefore, the methyl groups are arranged in the same direction.
  • Polypropylene is one of the four general-purpose resins, together with polyethylene, PVC, and polystyrene, accounting for 24% of the thermoplastic resin usage. It also has advantages in terms of cost and environment. Applications are packaging films, stretched tapes, fibers, clothing, carpets, pipes, daily necessities, toys, industrial parts, containers and the like. Peroxides are often used in the production of polypropylene.
  • Modification of the polymer chain with peroxide improves the melting properties of the polypropylene.
  • the use of peroxides can lower the viscosity of the polymer and control the melting properties during the process. This means that selective chain cleavage can result in narrower molecular weight distributions, lower molecular weights, and lower melting points.
  • This property is expressed as a melt flow index (MFI).
  • MFI melt flow index
  • This index represents the amount of polypropylene released per unit time (10 minutes) through a nozzle with a specific aperture under certain temperature conditions. However, if the melt index (MFI) required for spinning extrusion of polypropylene is not met, screen clogging may occur due to the pressure rise of the spinning extruder.
  • polypropylene Due to the weak melt strength due to the linear chain structure, polypropylene has a characteristic that the melt tension is sharply lowered at a temperature above the melting point. Therefore, in the case of foaming, breakage occurs in the cell walls, making it difficult to form fine cells. In addition, the foaming ratio and the compressive strength is lowered due to this, the mechanical properties are lowered, which did not show satisfactory formability compared to other plastic compositions. Therefore, there is a need for a method of modifying polypropylene that is easy to modify, safer and more reliable so that end users can exhibit desired melting characteristics.
  • Prior art in this field includes Korea Patent Publication 2009-0135247.
  • an object of the present invention is to provide a masterbatch composition for the modification of polypropylene is easy, safer and more reliable so that the end user can exhibit the desired melting characteristics.
  • Another object of the present invention is to provide a polypropylene modification method using the masterbatch composition.
  • the polypropylene component may be one or more selected from the group consisting of propylene homopolymers, random copolymers and terpolymers.
  • the additive may be a phosphate-based antioxidant.
  • the steps of A), B) and C) components to the extruder (Extruder); Heating and extruding at 100 to 200 ° C. to prepare a masterbatch as granules or pellets; And crosslinking the polypropylene with the extruded masterbatch by mixing and heating.
  • the modification is to change the physical properties of the polypropylene in the melt index (MFI) of the polypropylene in the range of 12 to 1800, within the error range of 1 to 5% by weight of the target melt index (MFI) It may be to.
  • MFI melt index
  • a masterbatch composition for modifying polypropylene that is easy, safer and more reliable can be provided so that the end user can exhibit the desired melting characteristics.
  • the master batch according to the invention has a solid form of physical form. Therefore, the storage stability and the dispersibility in processing are improved compared to the existing method, thereby improving the performance of the manufactured product through this, it can be free from fire, explosion due to the rise of the external temperature.
  • a method for modifying polypropylene using the master batch composition may be provided.
  • FIG. 2 is a graph showing a change in the melting index (Melting Index) of the polypropylene prepared according to an embodiment of the present invention.
  • 3 is a graph showing the molecular weight distribution of polypropylene prepared according to one embodiment of the present invention.
  • 5 is a graph showing the molecular weight distribution of polypropylene prepared according to one embodiment of the present invention.
  • master batch refers to a kneading of a compounding agent at a higher concentration than previously prescribed in the process of mixing the compounding agent with the raw rubber, which can be mixed into the rubber to accurately weigh each compounding agent and disperse It can improve the quality and prevent the scattering during work. It is used to improve the dispersion of pigments in the molding process of plastics.
  • Extruder refers to a screw-rotating machine which extrudes a rubber or synthetic resin tube, a rod of various cross-sectional shapes, a plate, a shape, or performs a strainer operation or a heating operation.
  • the raw material introduced into the dosing is supplied to the feeding zone through the rotation of the screw, and some of the raw material begins to be broken by friction and impact. At this time, the raw material starts to melt by frictional heat and heating heat, and completely melts in a melting zone, and a resin having a uniform viscosity is extruded in a mixing zone.
  • melt index MI may be represented as MFI or MFR.
  • Polypropylene has good oil resistance and heat resistance up to 100 ° C.
  • polypropylene is used in a wide range of fields such as automobiles, electrical and electronic parts because of its excellent mechanical properties and secondary molding and recycling.
  • polypropylene due to the weak melt strength resulting from the linear chain structure, polypropylene has the property that the melt tension is sharply lowered at temperatures above the melting point. Therefore, in the case of foaming, breakage occurs in the cell walls, making it difficult to form fine cells.
  • the foaming ratio and the compressive strength is lowered due to this, the mechanical properties are lowered, which did not show satisfactory formability compared to other plastic compositions.
  • the first is to introduce a long chain branch by irradiating electron beams to the polyolefin. This method reduces the attraction between the polymer chains and gives easy flow characteristics. In applications requiring dimensional stability, such as a large blow, etc., long side branches form physical crosslinks with adjacent chains to increase melt strength, and thus may exhibit high melt tension.
  • the first is a chain polypropylene by irradiating an electron beam to the polypropylene from the polymerization reactor or by reacting the radical formed through the reaction extrusion method
  • a method was used to allow long branches to form.
  • the second method is to physically blend polypropylene having a very high molecular weight.
  • the workability is lowered because the melt index is very low.
  • Both of the above methods have a disadvantage in that commercialization is difficult because the polypropylene is polymerized through a polymerization reaction and then functionalities are imparted through post-processing such as electron beam crosslinking and blending.
  • FIG. 1 of the present invention a conventional polypropylene reforming method (above) and a polypropylene reforming method (below) using the masterbatch composition according to the present invention are shown schematically.
  • the conventional method has shown that polypropylene having a desired melt index is prepared in advance and introduced into an extruder.
  • the modification method of the polypropylene according to the present invention is to mix and feed the polypropylene and the master batch composition, through which the desired melt index can be obtained in the extrusion process.
  • UV stabilizers may be used within an appropriate range that does not impair the effects of the present invention.
  • the masterbatch composition according to the invention it is possible to: 1) excellent processability and dispersibility; 2) lower manufacturing costs of meltblown nonwovens and SM (M) S composites; 3) easy to control the final melt index can be applied to various applications (the melt index can vary from 12 to 1800 target value depending on the user's requirements); And 4) advantages such as maintaining high safety.
  • the melt index can vary from 12 to 1800 target value depending on the user's requirements.
  • advantages such as maintaining high safety.
  • the technical feature of the present invention is that 2,5-dimethyl 2,5-di (tert-butylperoxy) hexane (DTBPH) does not react with propylene in the masterbatch manufacturing process, so that the end-user does not prepare the final polypropylene product.
  • DTBPH 2,5-dimethyl 2,5-di (tert-butylperoxy) hexane
  • DTBPH 2,5-dimethyl 2,5-di (tert-butylperoxy) hexane
  • the masterbatch composition according to the present invention can be used to easily control the melt index of the polyethylene or polypropylene in the range of 12 ⁇ 1800.
  • the present invention allows end users to more easily inject polypropylene.
  • the present invention makes it possible to manufacture polypropylene having a high melt index with high reliability.
  • the masterbatch composition according to the invention makes it very easy to process polypropylene.
  • the masterbatch according to the present invention When using the masterbatch according to the present invention, it is possible to ensure high safety in the production of polypropylene. If the remaining catalyst reacts with the hydrocarbon, there is a risk of explosion at temperatures above 80 degrees Celsius. However, the masterbatch according to the present invention does not leave unreacted peroxide that does not participate in the crosslinking reaction, so there is no risk of side reactions and explosion with hydrocarbons.
  • MFI melt index
  • the polypropylene component may be at least one selected from the group consisting of propylene homopolymer, random copolymer and terpolymer.
  • the additive may be a phosphate-based antioxidant.
  • the phosphate antioxidant may be used such as ALKANOX, ULTRANOX, WESTON, POLYGARD and SONGNOX, but is not limited thereto.
  • a method for producing a peroxide masterbatch and a method for modifying polypropylene comprising the following steps.
  • the modification may be to change the polypropylene melt index (MFI) of the polypropylene within an error range of 1 to 5% in the range of 12 ⁇ 1800.
  • MFI polypropylene melt index
  • a feature of the present invention lies in the remarkable advantages of the process that end users can very easily extrude polypropylene resins having a wide range of melt indexes to the extent desired.
  • a resin of very uniform quality can be obtained.
  • the error range of the melt index is only 1 to 5% has the advantage of ensuring a very reliable resin. This advantage is well illustrated in the following examples.
  • a mast batch prepared in the same manner as in Preparation Example 2 (referred to as "peroxide MB 5.5 wt%" in the following table) was used for polypropylene modification.
  • the properties of the polypropylene according to the content of the masterbatch according to the present invention were measured as follows.
  • MFI data was measured with a 1 mm orifice MFI and converted to a 2.095 mm MFI. (1 mm MFI * 19.6 + k)
  • Table 4 Melt Index (g / 10min) Number average molecular weight Weight average molecular weight Polydispersity (PI) Base Polypropylene (1st Generation) 193 10200 73800 7.24 Concentration of 5.5% by weight of peroxide MB 0 216 10200 71200 6.98 1.0 610 9050 51100 5.65 1.5 884 8120 39600 4.88 2.0 1080 7530 41600 5.52 2.5 1237 8210 40200 4.90 3.0 1531 7080 38000 5.37 3.5 1962 7840 35900 4.58
  • Example 4 In the same manner as in Example 4, 1.2 wt% of "IRGATEC CR76" manufactured by Shiva Corporation was charged and melt spun at 10 wt% of the nonwoven fabric's weight to obtain a long fiber spanbonded nonwoven fabric.
  • Example 5 In the same manner as in Example 5, 1.5 wt% of Shiva Corporation's "IRGATEC CR76" was charged and melt spun at 10 wt% of the nonwoven fabric's weight to obtain a long fiber spanbonded nonwoven fabric.
  • a 6 wt% masterbatch with a high concentration of polypropylene with a melt index (MFI) of about 900-1100 g / 10 min and a phthalocyanine blue pigment was added to an extruder with five heating parts.
  • region was set to 180 degreeC, and the temperature of the remaining melting part and kneading part was set to 285 degreeC.
  • the fiber was melted and spun at 10 wt% of the nonwoven fabric and laminated on a porous conveyor belt to obtain a five-layer long fiber spanbond nonwoven fabric of SSMMS in a combination of a spunbond and meltblown having a basis weight of 50 gsm / s.
  • the present invention can be implemented in the polypropylene resin uniformly, without the risk of explosion, such an increase in the melt index as described above.

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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)
  • General Chemical & Material Sciences (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

La présente invention concerne une technologie pour produire des mélanges maîtres de peroxyde et un procédé de reformage de polypropylène l'utilisant. Selon la présente invention, une composition de mélange maître est fournie qui permet un reformage facile de façon à présenter des caractéristiques de fusion souhaitées par un utilisateur final, et qui permet un reformage plus sûr et plus fiable de polypropylène. L'invention concerne également un procédé de reformage de polypropylène à l'aide de la composition.
PCT/KR2013/009779 2012-11-05 2013-10-31 Technologie pour produire des mélanges maîtres de peroxyde, et procédé de reformage de polypropylène l'utilisant WO2014069911A1 (fr)

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KR10-2012-0124354 2012-11-05

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3034552A1 (fr) * 2014-12-15 2016-06-22 Borealis AG Composition de viscoréduction synergique de peroxyde et d'ester d'hydroxylamine pour augmenter l'efficacité de viscoréduction
CN106751352A (zh) * 2016-12-26 2017-05-31 重庆普利特新材料有限公司 一种超高流动性聚丙烯美学树脂复合材料及其制备方法
CN111518336A (zh) * 2020-05-28 2020-08-11 广州市聚赛龙工程塑料股份有限公司 一种可控流变聚丙烯材料及其制备方法和应用
CN112778636A (zh) * 2020-12-28 2021-05-11 金发科技股份有限公司 一种熔喷聚丙烯料及制备方法和应用
CN113388203A (zh) * 2021-06-30 2021-09-14 中国石油化工股份有限公司 耐辐照杀菌聚丙烯纺粘无纺布专用料及其制备方法
CN114163730A (zh) * 2021-12-27 2022-03-11 锦州英诺威科技服务有限公司 一种聚丙烯可控流变改性剂及其制备方法

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JPH0830133B2 (ja) * 1988-11-21 1996-03-27 富士写真フイルム株式会社 感光材料用包装材料
KR20020029066A (ko) * 1999-07-07 2002-04-17 샬크비즈크 피이터 코르넬리스; 페트귄터 고농도 교차결합 마스터배치
JP2003138075A (ja) * 2001-10-30 2003-05-14 Japan Polychem Corp 有機過酸化物含有ポリプロピレン系樹脂組成物及びこれを用いた成形体
KR100811922B1 (ko) * 2007-02-13 2008-03-10 현대자동차주식회사 폴리프로필렌 수지 조성물

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0830133B2 (ja) * 1988-11-21 1996-03-27 富士写真フイルム株式会社 感光材料用包装材料
KR20020029066A (ko) * 1999-07-07 2002-04-17 샬크비즈크 피이터 코르넬리스; 페트귄터 고농도 교차결합 마스터배치
JP2003138075A (ja) * 2001-10-30 2003-05-14 Japan Polychem Corp 有機過酸化物含有ポリプロピレン系樹脂組成物及びこれを用いた成形体
KR100811922B1 (ko) * 2007-02-13 2008-03-10 현대자동차주식회사 폴리프로필렌 수지 조성물

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3034552A1 (fr) * 2014-12-15 2016-06-22 Borealis AG Composition de viscoréduction synergique de peroxyde et d'ester d'hydroxylamine pour augmenter l'efficacité de viscoréduction
WO2016096687A1 (fr) * 2014-12-15 2016-06-23 Borealis Ag Composition de viscoréduction synergique de peroxyde et d'ester d'hydroxylamine pour accroître l'efficacité de viscoréduction
CN107001503A (zh) * 2014-12-15 2017-08-01 博里利斯股份公司 用于提高减粘裂化效率的过氧化物和羟胺酯的协同减粘裂化组合物
RU2661868C1 (ru) * 2014-12-15 2018-07-20 Бореалис Аг Композиция для синергетического висбрекинга из перекиси и сложного эфира гидроксиламина для увеличения эффективности висбрекинга
US10982022B2 (en) 2014-12-15 2021-04-20 Borealis Ag Method of forming melt-blown non-wovens
CN106751352A (zh) * 2016-12-26 2017-05-31 重庆普利特新材料有限公司 一种超高流动性聚丙烯美学树脂复合材料及其制备方法
CN111518336A (zh) * 2020-05-28 2020-08-11 广州市聚赛龙工程塑料股份有限公司 一种可控流变聚丙烯材料及其制备方法和应用
CN112778636A (zh) * 2020-12-28 2021-05-11 金发科技股份有限公司 一种熔喷聚丙烯料及制备方法和应用
CN112778636B (zh) * 2020-12-28 2022-10-04 金发科技股份有限公司 一种熔喷聚丙烯料及制备方法和应用
CN113388203A (zh) * 2021-06-30 2021-09-14 中国石油化工股份有限公司 耐辐照杀菌聚丙烯纺粘无纺布专用料及其制备方法
CN113388203B (zh) * 2021-06-30 2022-07-05 中国石油化工股份有限公司 耐辐照杀菌聚丙烯纺粘无纺布专用料及其制备方法
CN114163730A (zh) * 2021-12-27 2022-03-11 锦州英诺威科技服务有限公司 一种聚丙烯可控流变改性剂及其制备方法

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