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Method for measuring crosslinking density of molded article of crosslinked thermoplastic polymer foam and molded article of crosslinked foam

A thermoplastic polymer, cross-linking density technology, applied in shoemaking machinery, using stable tension/pressure to test material strength, measuring devices, etc., can solve problems such as effective network chain structure identification

Active Publication Date: 2013-04-24
SUMITOMO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, although the approximate amount of the portion having an effective network chain structure can be determined, there is a problem that a smaller effective network chain structure cannot be recognized as an effective network chain structure because it is selected only according to its size. , so seek a more accurate method for the determination of crosslink density

Method used

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  • Method for measuring crosslinking density of molded article of crosslinked thermoplastic polymer foam and molded article of crosslinked foam
  • Method for measuring crosslinking density of molded article of crosslinked thermoplastic polymer foam and molded article of crosslinked foam
  • Method for measuring crosslinking density of molded article of crosslinked thermoplastic polymer foam and molded article of crosslinked foam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0170] (1) Preparation of co-catalyst carrier

[0171] In a reactor with a stirrer after nitrogen replacement, put silicon dioxide (Sylopol948 manufactured by Davison Company; 50% volume average particle diameter=59 μm; pore volume=1.68ml / g; specific surface area = 313m 2 / g) 0.36 kg and 3.5 liters of toluene were stirred. Then, after cooling to 5°C, 0.15 liters of 1,1,1,3,3,3-hexamethyldisilazane and 0.2 liters of toluene were added dropwise over 30 minutes while keeping the temperature in the reactor at 5°C. mixed solution. After completion of the dropwise addition, the mixture was stirred at 5° C. for 1 hour, then heated up to 95° C., stirred at 95° C. for 3 hours, and filtered. The obtained solid content was washed 6 times with 2 liters of toluene. Then, 2 liters of toluene was added to make a slurry, which was allowed to stand overnight.

[0172] Into the slurry obtained above, 0.27 liter of a hexane solution of diethylzinc (diethylzinc concentration: 2 mol / liter) w...

Embodiment 2

[0181] (1) Pressurized cross-linked foam molding

[0182] Except for changing the chemical foaming amount to 2.2 parts by weight, kneading was carried out under exactly the same conditions as in Example 1, and pressure crosslinking and foaming were performed to obtain a crosslinked foamed molded article (2). Table 3 shows the evaluation results of the physical properties of the obtained cross-linked foamed molded article, as well as the evaluation results of the cross-linking density and the gel fraction.

Embodiment 3

[0184] (1) Manufacture of ethylene-α-olefin copolymer

[0185] Using the prepolymerized catalyst component (1) obtained in Example 1, ethylene and 1-hexene were copolymerized in a continuous fluidized bed gas phase polymerization apparatus to obtain a polymer powder. In terms of polymerization conditions, the polymerization temperature is 84° C., the polymerization pressure is 2 MPa, the molar ratio of hydrogen to ethylene is 0.38%, and the molar ratio of 1-hexene to the sum of ethylene and 1-hexene is 2.0%. In order to keep the gas composition constant during the polymerization, ethylene, 1-hexene and hydrogen were continuously supplied. In addition, the above-mentioned prepolymerized catalyst component and triisobutylaluminum were continuously supplied to keep the total powder weight of 80 kg in the fluidized bed constant. The average polymerization time was 4 hr. The obtained polymer powder was extruded using an extruder (LCM50 manufactured by Kobe Steel Co., Ltd.) under ...

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Abstract

The present invention relates to a molded article of a crosslinked ethylenic polymer foam. The molded article of a crosslinked ethylenic polymer foam has a crosslinking density of 0.30 mol / kg or higher as determined using a relaxation modulus based on a stress relaxation measurement obtained by measuring the stress relaxation of the molded article of the crosslinked foam when the molded article of the crosslinked foam is subjected to compressive deformation under conditions of a measurement temperature of 60 C, compressive strain of 50%, and a measurement time of 1,800 seconds. The present invention also relates to a method for measuring the crosslinking density of a molded article of a crosslinked thermoplastic polymer foam, the method comprising: a step for heating the molded article of the crosslinked thermoplastic polymer foam to a predetermined temperature; a step for applying pressure to the molded article of the crosslinked thermoplastic polymer foam, which is maintained at the predetermined temperature, in order to induce compressive deformation of the molded article of the crosslinked foam, and for measuring the stress relaxation of the molded article of the crosslinked foam while the compressive strain of the molded article of the crosslinked foam is maintained at a constant level; a step for determining a relaxation modulus (Gc) from the stress relaxation; and a step for calculating the crosslinking density of the crosslinked thermoplastic polymer foam from Gc using the following formula in which Gc is the elastic modulus when the stress of the molded article of the crosslinked foam is at a constant level: n = Gc / RT (n: crosslinking density, R: gas constant, T: measurement temperature).

Description

technical field [0001] The present invention relates to a method for measuring the crosslink density of a thermoplastic polymer-made crosslinked foamed molded article, and a crosslinked foamed molded article whose crosslinked density calculated by the measurement method is a certain value or more. Background technique [0002] Cross-linked foam moldings made of thermoplastic polymers are widely used in daily sundries, flooring materials, sound insulation materials, heat insulation materials, etc. Among them, cross-linked foamed molded articles made of ethylene-based polymers are used for shoe parts (outersole (lower sole), midsole (upper sole), inner sole (sole, etc.). As a cross-linked foamed molded article made of an ethylene-based polymer, a cross-linked foamed molded article made by crosslinking and foaming an ethylene-vinyl acetate copolymer as described in Japanese Patent Publication No. 3-2657 is known, such as A cross-linked foamed molded article obtained by cross-l...

Claims

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Application Information

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IPC IPC(8): C08J9/06A43B13/02A43D25/06A43D86/00G01N3/08
CPCC08J2201/03G01N2203/0092C08J3/248A43B13/04G01N2203/0222C08J9/06G01N3/08C08J2201/026B29D35/122C08J2323/04
Inventor 山田胜大丰田博
Owner SUMITOMO CHEM CO LTD
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