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WO2013183342A1 - Procédé de fabrication d'une matière à base de polypropylène et matière à base de polypropylène - Google Patents

Procédé de fabrication d'une matière à base de polypropylène et matière à base de polypropylène Download PDF

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Publication number
WO2013183342A1
WO2013183342A1 PCT/JP2013/060024 JP2013060024W WO2013183342A1 WO 2013183342 A1 WO2013183342 A1 WO 2013183342A1 JP 2013060024 W JP2013060024 W JP 2013060024W WO 2013183342 A1 WO2013183342 A1 WO 2013183342A1
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WIPO (PCT)
Prior art keywords
polypropylene
polypropylene material
peak temperature
melting
melting peak
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2013/060024
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English (en)
Japanese (ja)
Inventor
中壽賀　章
博則 田畑
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sekisui Chemical Co Ltd
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Sekisui Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
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Priority to JP2013516041A priority Critical patent/JPWO2013183342A1/ja
Publication of WO2013183342A1 publication Critical patent/WO2013183342A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/02—Thermal after-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/02—Thermal after-treatment
    • B29C2071/027—Tempering, i.e. heating an object to a high temperature and quenching it
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2023/00—Use of polyalkenes or derivatives thereof as moulding material
    • B29K2023/10—Polymers of propylene
    • B29K2023/12—PP, i.e. polypropylene

Definitions

  • the present invention relates to a method for producing a polypropylene material and a polypropylene material.
  • Polypropylene materials are used in a wide range of fields because of their high mechanical strength and excellent heat resistance.
  • a method for further increasing the mechanical strength of the polypropylene material a method for increasing the crystallinity of the polypropylene material is known.
  • a method for further increasing the heat resistance of the polypropylene material there is a method of increasing the melting peak temperature of the polypropylene material by orienting the molecular chain in the polypropylene material by stretching the polypropylene material. It has been.
  • Patent Document 1 a polypropylene preform having a melting peak temperature of Tm (° C.) obtained by a differential thermal analysis obtained at a rate of temperature increase of 20 ° C./min is obtained from Tm-15 (° C.) to Tm (° C.). It has been proposed to improve the rigidity and heat resistance of a polypropylene molded body by raising the temperature to a temperature in the range of 1 and heating and heat-treating.
  • the main object of the present invention is to provide a method for producing a polypropylene material that can improve the heat resistance of the polypropylene material.
  • the present inventor after melting the polypropylene-based material within a specific temperature range, and further performing a heat treatment within the specific temperature range, It has been found that the heat resistance of polypropylene materials can be improved.
  • the method for producing a polypropylene-based material according to the present invention includes a melting step of melting a polypropylene-based material at a temperature exceeding the melting peak temperature Tm + 5 ° C. of the polypropylene-based material in the differential scanning calorimetry and not higher than the melting peak temperature Tm + 80 ° C.
  • the heat resistance of a polypropylene material can be improved.
  • the melting peak temperature refers to an endothermic peak on a DSC curve obtained by differential scanning calorimetry (DSC).
  • the polypropylene material is melted at a melting peak temperature Tm + 10 ° C. or higher and a melting peak temperature Tm + 80 ° C. or lower in the melting step.
  • the degree of crystallinity A of the polypropylene material before the melting step is 40% or more.
  • the crystallinity of the polypropylene material is a value calculated by dividing the peak area of the DSC curve by 209 mJ / mg and multiplying by 100.
  • the melting peak temperature Tm of the polypropylene material before the melting step is 160 ° C. or higher.
  • the heat treatment step is performed for 5 minutes to 180 minutes.
  • the polypropylene material according to the present invention is a polypropylene material obtained by the above-described method for producing a polypropylene material.
  • the relationship between the crystallinity A of the polypropylene material before the melting step and the crystallinity B of the polypropylene material after the heat treatment step ((BA) / A) ⁇ 100 is -10% or more.
  • the degree of crystallinity B is 50% or more.
  • the melting peak temperature of the polypropylene material after performing the heat treatment step in differential scanning calorimetry is the melting peak temperature Tm + 5 ° C. or higher of the polypropylene material.
  • the half width from the melting peak temperature of the polypropylene material after the heat treatment step in the differential scanning calorimetry is 12 ° C. or more.
  • FIG. 1 is a graph showing a temperature profile in the first embodiment.
  • FIG. 2 is a graph showing a temperature profile in Comparative Example 1.
  • the method for producing a polypropylene material according to the present invention includes a melting step of melting the polypropylene material at a temperature exceeding the melting peak temperature Tm + 5 ° C. of the polypropylene material in the differential scanning calorimetry and not exceeding the melting peak temperature Tm + 80 ° C. .
  • Examples of the polypropylene material used for the melting step include a propylene homopolymer, a block copolymer of propylene and another ⁇ -olefin, and a random copolymer of propylene and another ⁇ -olefin. It is done.
  • Examples of the ⁇ -olefin include ethylene, 1-butene, 1-hexene, 1-octene and the like.
  • the molecular weight distribution (weight average molecular weight (Mw) / number average molecular weight (Mn)) of the polypropylene material is preferably 1 to 20.
  • the melt flow index (MFR) of the polypropylene-based material is preferably 0.5 g / 10 min to 50 g / 10 min.
  • the MFR is a value measured by a method defined in JIS K7210.
  • the thickness of the polypropylene material is not particularly limited.
  • the thickness of the polypropylene material is preferably about 0.1 mm to 10 mm.
  • the crystallinity A of the polypropylene material is preferably 40% or more, and more preferably 45% or more.
  • the crystallinity A is usually about 50% or less.
  • the melting peak temperature Tm in the differential scanning calorimetry (DSC) of the polypropylene material is usually 160 ° C. or higher.
  • the melting peak temperature Tm is usually less than 170 ° C.
  • the polypropylene material may contain an additive.
  • the additive include antioxidants, weathering stabilizers such as ultraviolet absorbers and radical scavengers, and crystal nucleating agents.
  • the polypropylene material is melted at a temperature exceeding the melting peak temperature Tm + 5 ° C. in the DSC and the melting peak temperature Tm + 80 ° C. or less.
  • the polypropylene-based material is preferably melted at a melting peak temperature Tm + 10 ° C. or more and a melting peak temperature Tm + 80 ° C. or less in DSC, and a melting peak temperature Tm + 15 ° C. or more and a melting peak temperature Tm + 80 ° C. or less. It is more preferable to melt under.
  • the melting peak temperature Tm + 5 ° C. is exceeded and the melting peak temperature Tm + 80 ° C. or lower is maintained for about 5 minutes. In this case, the polypropylene-based material is completely melted.
  • the method for producing a polypropylene material according to the present invention includes a heat treatment step of heat-treating the polypropylene material melted in the melting step at a melting peak temperature Tm ⁇ 20 ° C. or higher and lower than the melting peak temperature Tm ⁇ 10 ° C. .
  • the temperature of the polypropylene material after the melting step is lowered to the temperature condition in the heat treatment step.
  • the polypropylene-based material melted in the melting step is heat-treated at a melting peak temperature Tm-20 ° C. or higher and lower than the melting peak temperature Tm-10 ° C. in DSC.
  • the polypropylene-based material is preferably maintained at a melting peak temperature Tm ⁇ 20 ° C. or more and less than a melting peak temperature Tm ⁇ 10 ° C. for more than 5 minutes and less than 180 minutes, more than 30 minutes It is more preferable to hold for 180 minutes or less.
  • a melting peak temperature Tm ⁇ 20 ° C. or more and less than a melting peak temperature Tm ⁇ 10 ° C. for more than 5 minutes and less than 180 minutes, more than 30 minutes It is more preferable to hold for 180 minutes or less.
  • the polypropylene material according to the present invention is obtained by the above melting process and heat treatment process.
  • the crystallinity A of the polypropylene material before the heat treatment step and the polypropylene material after the heat treatment step (hereinafter referred to as “the polypropylene material after the heat treatment”). )
  • the degree of crystallinity B ((BA) / A) ⁇ 100 can be set to ⁇ 10% or more.
  • the value of ((BA) / A) ⁇ 100 is more preferably 10% or more.
  • the value of ((BA) / A) ⁇ 100 is preferably higher, but the upper limit of this value is about 60%.
  • the degree of crystallinity B is preferably 50% or more, and more preferably 55% or more.
  • the melting peak temperature of the polypropylene material after the heat treatment in DSC can be set to the melting peak temperature Tm or more of the polypropylene material.
  • Tm melting peak temperature
  • the crystallinity and the melting peak temperature of the propylene material hardly change.
  • the polypropylene-based material is melted at a temperature exceeding the melting peak temperature Tm + 5 ° C. and below the melting peak temperature Tm + 80 ° C., and further heat-treated at a melting peak temperature Tm ⁇ 20 ° C.
  • the half width from the melting peak temperature of the polypropylene-based material after heat treatment in DSC is preferably 12 ° C. or more.
  • the heat resistance of the polypropylene material can be improved. Furthermore, according to the method for producing a polypropylene material according to the present invention, the heat resistance of the polypropylene material can be improved while maintaining the crystallinity of the polypropylene material at a high level.
  • Example 1 A polypropylene-based material pellet (manufactured by Nippon Polypro Co., Ltd., polypropylene-based material, grade MA3H, melting peak temperature Tm 166 ° C. to 169 ° C.) was pressed at 190 ° C. and a pressure of 180 kg / cm 2 to obtain a sheet having a thickness of 1 mm. . The obtained sheet was heated to 200 ° C. under a condition of 10 ° C./min using DSC (“DSC 6220” manufactured by SII Nano Technology) and held at 200 ° C. for 5 minutes (melting step). Next, the obtained sheet
  • DSC DSC 6220
  • seat was cooled to 0 degreeC on 20 degree-C / min conditions, and the polypropylene-type material sheet was obtained.
  • the obtained polypropylene material sheet was heated to 200 ° C. under a condition of 10 ° C./min, and held at 200 ° C. for 5 minutes.
  • the temperature profile is shown in FIG. By the above operation, the melting peak temperature and crystallinity of the polypropylene material sheet before the melting step and the melting peak temperature and crystallinity of the polypropylene material sheet after the heat treatment step were measured.
  • the crystallinity was calculated by dividing the peak area of the DSC curve by 209 mJ / mg and multiplying by 100.
  • the endothermic peak of the DSC curve was taken as the melting peak temperature.
  • Example 2 The sheet obtained in Example 1 was heated to 190 ° C. under a condition of 10 ° C./min using DSC (manufactured by SII Nano Technology, “DSC 6220”) and held at 190 ° C. for 5 minutes (melting step) ). Next, the obtained sheet
  • Example 3 The sheet obtained in Example 1 was heated to 220 ° C. under a condition of 10 ° C./min using DSC (manufactured by SII Nano Technology, “DSC 6220”) and held at 220 ° C. for 5 minutes (melting step) ). Next, the obtained sheet
  • Example 4 The sheet obtained in Example 1 was heated to 240 ° C. under a condition of 10 ° C./min using DSC (manufactured by SII Nano Technology, “DSC6220”) and held at 240 ° C. for 5 minutes (melting step) ). Next, the obtained sheet
  • Example 5 The sheet obtained in Example 1 was heated to 200 ° C. under a condition of 10 ° C./min using DSC (“DSC 6220” manufactured by SII Nano Technology Co., Ltd.) and held at 200 ° C. for 5 minutes (melting step). ). Next, the obtained sheet
  • Example 6 The sheet obtained in Example 1 was heated to 200 ° C. under a condition of 10 ° C./min using DSC (“DSC 6220” manufactured by SII Nano Technology Co., Ltd.) and held at 200 ° C. for 5 minutes (melting step). ). Next, the obtained sheet
  • Example 1 A polypropylene material sheet was obtained in the same manner as in Example 1 except that the heat treatment step was not performed. Next, the obtained polypropylene material sheet was heated to 200 ° C. under a condition of 10 ° C./min, and held at 200 ° C. for 5 minutes. The temperature profile is shown in FIG. In the same manner as in Example 1, the melting peak temperature and crystallinity of the polypropylene material sheet before the melting step, the melting peak temperature and crystallinity of the polypropylene material sheet after the melting step, and the heat treatment step were obtained. The half width from the melting peak temperature of the polypropylene material sheet was determined. The results are shown in Table 1.
  • Example 2 The sheet obtained in Example 1 was heated to 200 ° C. under a condition of 50 ° C./min using DSC (“DSC 6220” manufactured by SII Nano Technology) and held at 200 ° C. for 5 minutes (melting step) ). Next, the obtained sheet
  • DSC DSC 6220” manufactured by SII Nano Technology
  • Example 3 The sheet obtained in Example 1 was heated to 200 ° C. under a condition of 10 ° C./min using DSC (“DSC 6220” manufactured by SII Nano Technology Co., Ltd.) and held at 200 ° C. for 5 minutes (melting step). ). Next, the obtained sheet

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  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

L'invention concerne un procédé de fabrication d'une matière à base de polypropylène avec lequel il est possible d'améliorer la résistance à la chaleur d'une matière à base de polypropylène. Le procédé de fabrication d'une matière à base de polypropylène comprend : une étape de fusion dans laquelle une matière à base de polypropylène est fondue à une température qui est supérieure à la [(température de pic de fusion Tm de la matière à base de polypropylène mesurée par calorimétrie différentielle à balayage)+5°C] mais non supérieure à la [(température de pic de fusion Tm)+80°C] ; et une étape de traitement thermique dans laquelle la matière à base de polypropylène fondue dans l'étape de fusion est traitée thermiquement à une température qui est la [(température de pic de fusion Tm)-20°C] ou plus mais inférieure à la [(température de pic de fusion Tm)-10°C].
PCT/JP2013/060024 2012-06-08 2013-04-02 Procédé de fabrication d'une matière à base de polypropylène et matière à base de polypropylène Ceased WO2013183342A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2013516041A JPWO2013183342A1 (ja) 2012-06-08 2013-04-02 ポリプロピレン系材料の製造方法及びポリプロピレン系材料

Applications Claiming Priority (2)

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JP2012130853 2012-06-08
JP2012-130853 2012-06-08

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WO2013183342A1 true WO2013183342A1 (fr) 2013-12-12

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016101736A (ja) * 2014-11-28 2016-06-02 宇部エクシモ株式会社 ファブリック強化樹脂成形体の製造方法及びファブリック強化樹脂成形体

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61130018A (ja) * 1984-11-29 1986-06-17 Idemitsu Petrochem Co Ltd ポリプロピレンシ−トおよびその製造方法
JPS61189920A (ja) * 1985-02-20 1986-08-23 Idemitsu Petrochem Co Ltd 熱成形用ポリプロピレンシートの製造方法
JPS6219206A (ja) * 1985-07-18 1987-01-28 Dainippon Ink & Chem Inc 高分離能高分子膜の製造方法
JPH05104622A (ja) * 1991-10-21 1993-04-27 Mitsubishi Petrochem Co Ltd ポリプロピレン製低熱収縮性延伸テープの製造方法
JPH10298305A (ja) * 1997-04-25 1998-11-10 Sekisui Chem Co Ltd ポリオレフィンシートの製造方法
JP2003170485A (ja) * 2001-12-07 2003-06-17 Idemitsu Unitech Co Ltd 透明ポリプロピレンシートの製造方法および透明ポリプロピレンシート
JP2003278027A (ja) * 2002-03-18 2003-10-02 Mitsubishi Rayon Co Ltd ポリプロピレン繊維及びその製造方法
JP2009012225A (ja) * 2007-07-02 2009-01-22 Sekisui Seikei Ltd ポリオレフィン系樹脂シートの製造方法及びそれに使用する製造装置
JP2009013357A (ja) * 2007-07-06 2009-01-22 Idemitsu Unitech Co Ltd ポリプロピレン成形品、シート状ポリプロピレン成形品およびポリプロピレン熱成形品の製造方法

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61130018A (ja) * 1984-11-29 1986-06-17 Idemitsu Petrochem Co Ltd ポリプロピレンシ−トおよびその製造方法
JPS61189920A (ja) * 1985-02-20 1986-08-23 Idemitsu Petrochem Co Ltd 熱成形用ポリプロピレンシートの製造方法
JPS6219206A (ja) * 1985-07-18 1987-01-28 Dainippon Ink & Chem Inc 高分離能高分子膜の製造方法
JPH05104622A (ja) * 1991-10-21 1993-04-27 Mitsubishi Petrochem Co Ltd ポリプロピレン製低熱収縮性延伸テープの製造方法
JPH10298305A (ja) * 1997-04-25 1998-11-10 Sekisui Chem Co Ltd ポリオレフィンシートの製造方法
JP2003170485A (ja) * 2001-12-07 2003-06-17 Idemitsu Unitech Co Ltd 透明ポリプロピレンシートの製造方法および透明ポリプロピレンシート
JP2003278027A (ja) * 2002-03-18 2003-10-02 Mitsubishi Rayon Co Ltd ポリプロピレン繊維及びその製造方法
JP2009012225A (ja) * 2007-07-02 2009-01-22 Sekisui Seikei Ltd ポリオレフィン系樹脂シートの製造方法及びそれに使用する製造装置
JP2009013357A (ja) * 2007-07-06 2009-01-22 Idemitsu Unitech Co Ltd ポリプロピレン成形品、シート状ポリプロピレン成形品およびポリプロピレン熱成形品の製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016101736A (ja) * 2014-11-28 2016-06-02 宇部エクシモ株式会社 ファブリック強化樹脂成形体の製造方法及びファブリック強化樹脂成形体

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