WO2021181999A1 - Composition de résine et procédé de recyclage de résine de poly(vinyl acétal) - Google Patents

Composition de résine et procédé de recyclage de résine de poly(vinyl acétal) Download PDF

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WO2021181999A1
WO2021181999A1 PCT/JP2021/005046 JP2021005046W WO2021181999A1 WO 2021181999 A1 WO2021181999 A1 WO 2021181999A1 JP 2021005046 W JP2021005046 W JP 2021005046W WO 2021181999 A1 WO2021181999 A1 WO 2021181999A1
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resin
plasticizer
polyvinyl acetal
infrared spectroscopic
spectroscopic spectrum
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PCT/JP2021/005046
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English (en)
Japanese (ja)
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一人 國領
幸次 増田
浩一 平尾
神澤 岳史
博之 脇坂
隆志 上田中
Original Assignee
株式会社ガラステクノシナジー
マスダ商事株式会社
滋賀県
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Priority to JP2022505855A priority Critical patent/JPWO2021181999A1/ja
Publication of WO2021181999A1 publication Critical patent/WO2021181999A1/fr

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/10Esters; Ether-esters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L21/00Compositions of unspecified rubbers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions 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
    • C08L23/04Homopolymers or copolymers of ethene
    • C08L23/06Polyethene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions 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
    • C08L23/10Homopolymers or copolymers of propene
    • C08L23/12Polypropene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L29/00Compositions 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 an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
    • C08L29/14Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols

Definitions

  • the present invention particularly relates to a bleed-controlled resin composition and a method for recycling a polyvinyl acetal resin.
  • laminated glass has been widely used for windowpanes of automobiles and aircraft for the purpose of preventing glass fragments from scattering when broken.
  • the laminated glass there is one in which an interlayer film sheet containing a polyvinyl acetal resin such as polyvinyl butyral resin is interposed between glass plates and integrated.
  • the polyvinyl acetal resin for a laminated glass interlayer sheet contains about several tens of percent of a liquid plasticizer as an essential component for the purpose of adjusting the viscosity and imparting sound absorbing performance (see, for example, Patent Document 1). Therefore, in order to recycle the laminated glass sheet on the market, it is necessary to handle it in a state where the plasticizer is contained.
  • the plasticizer may bleed (bleed out), making it difficult to use as a product.
  • the present invention solves the above problems, and controls bleeding from a composition such as a plasticizer even when a material containing a large amount of a plasticizer such as an interlayer film sheet is contained, and is a raw material particularly in recycling.
  • the purpose is to obtain a resin composition that enables the utilization of resin.
  • the plasticizer preferably contains an ester compound having an ether bond in the molecule.
  • the flexible resin is ethylene propylene rubber, ethylene propylene diene rubber, butadiene rubber, styrene butadiene rubber, nitrile rubber, nitrile butadiene rubber, isoprene rubber, styrene butadiene / butylene / styrene elastomer, ethylene acetate. It is preferably at least one selected from the group consisting of vinyl copolymers and mixtures thereof.
  • the polyvinyl acetal resin is preferably at least one selected from the group consisting of polyvinyl acetal acetal and polyvinyl butyral.
  • the polyolefin-based resin is preferably at least one selected from the group consisting of polypropylene resin and polyethylene resin.
  • the method for recycling a polyvinyl acetal resin of the present invention is a method for recycling a polyvinyl acetal resin (excluding polyvinyl formal resin) containing a plasticizer, in which the polyvinyl acetal resin containing the plasticizer and a polyolefin resin are kneaded.
  • the bleed control agent is characterized by adding at least one flexible resin selected from the group consisting of synthetic rubbers, elastomers and copolymerized olefin resins.
  • a material containing a large amount of a plasticizer such as an interlayer film sheet is contained, bleeding from a composition such as a plasticizer can be controlled, and the raw material resin can be utilized especially in recycling.
  • a resin composition can be obtained.
  • FIG. 1 is an infrared spectroscopic spectrum for bleed evaluation measured using the resin composition of Example 1.
  • FIG. 2 is an infrared spectroscopic spectrum for bleed evaluation measured using the resin composition of Example 2.
  • FIG. 3 is an infrared spectroscopic spectrum for bleed evaluation measured using the resin composition of Example 3.
  • FIG. 4 is an infrared spectroscopic spectrum for bleed evaluation measured using the resin composition of Example 4.
  • FIG. 5 is an infrared spectroscopic spectrum for bleed evaluation measured using the resin composition of Example 5.
  • FIG. 6 is an infrared spectroscopic spectrum of the resin composition of the reference example, which is an infrared spectroscopic spectrum of the surface of the test piece made of the PVB interlayer film of the process scrap and an infrared spectroscopic spectrum which is a reference for bleed evaluation.
  • FIG. 7 (A) is an infrared spectroscopic spectrum for bleed evaluation measured using the resin composition of Comparative Example 1
  • FIG. 7 (B) is a resin composition of Comparative Example 2.
  • 8 (A) to 8 (E) are infrared spectroscopic spectra for bleed evaluation measured using the resin compositions of Examples 6 to 10.
  • 9 (A) is an infrared spectroscopic spectrum for bleed evaluation measured using the resin composition of Example 11 and FIG.
  • FIG. 10A shows the results of gas chromatograph mass spectrometry using the resin composition of Comparative Example 3
  • FIG. 10B shows the results of Comparative Example 4
  • FIG. 10C shows the results of mass spectrometric analysis using the resin composition of Example 13. ..
  • the resin composition of the present invention contains a polyolefin-based resin, a polyvinyl acetal resin containing a plasticizer (excluding polyvinyl formal resin), and further contains a flexible resin.
  • the present invention was obtained by adding the flexible resin to a material containing a large amount of plasticizer such as an interlayer film sheet made of polyvinyl acetal resin such as PVB when kneading with a polyolefin resin in recycling. It has been found that the bleeding of the resin composition can be controlled and the bleeding suppressing effect of the contained plasticizer can be obtained.
  • the interlayer film sheet often contains an ester compound having an ether bond in the molecule because it has a good affinity with a polyvinyl acetal resin such as PVB. Therefore, in the present invention, the plasticizer preferably contains an ester compound having an ether bond in the molecule.
  • This ester compound is often contained in a material such as an interlayer film because it has a low environmental load as an ester, is highly productive, and can be provided at low cost. The compound is also excellent in conductivity performance and bleed resistance.
  • diethylene glycol di-2-ethylhexanoate triethylene glycol di-n-hexanoate, diethylene glycol di-n-hexanoate, triethylene glycol di-2-ethylhexanoate, bis adipate (2-( 2-Butoxyethoxy) ethyl) and the like can be mentioned.
  • Particularly preferred esters include triethylene glycol di-2-ethylhexanoate, bis adipate (2- (2-butoxyethoxy) ethyl) and the like.
  • the compound one kind may be blended alone, or two or more kinds of the said compound may be used in combination.
  • the flexible resin is at least one resin selected from the group consisting of synthetic rubber, elastomer and copolymerized olefin resin.
  • the synthetic rubber includes ethylene propylene rubber (EPM), ethylene propylene diene rubber (EPDM), butadiene rubber (BR), styrene butadiene rubber (SBR), nitrile rubber (NR), nitrile butadiene rubber (NBR), isoprene rubber, and It is preferably at least one selected from the group consisting of these mixtures.
  • EPM ethylene propylene rubber
  • EPDM ethylene propylene diene rubber
  • BR butadiene rubber
  • SBR styrene butadiene rubber
  • NR nitrile butadiene rubber
  • NBR nitrile butadiene rubber
  • isoprene rubber It is preferably at least one selected from the group consisting of these mixtures.
  • the elastomer styrene butadiene /
  • the flexible resin may be added in a small amount of about 2.5 parts by weight with respect to 60 parts by weight of the polyolefin resin and 20 parts by weight of the polyvinyl acetal resin containing the plasticizer corresponding to the interlayer film.
  • the bleeding suppressing effect of the plasticizer can be obtained.
  • the blending amount of the flexible resin is 5.0 parts by weight to 30 parts by weight, the bleeding suppressing effect is large, which is preferable. More preferably, it is in the range of 10 parts by weight to 20 parts by weight.
  • the polyvinyl acetal resin is preferably at least one selected from the group consisting of polyvinyl acetal acetal and polyvinyl butyral.
  • the molecular weight of the polyvinyl acetal resin is preferably 1,000 or more, more preferably 10,000 or more. According to the present invention, the molecular weight of the polyvinyl acetal resin may be in the range of 1.0 ⁇ 10 5 or more.
  • the polyolefin resin is preferably at least one selected from the group consisting of polypropylene resin, polyethylene resin, and various copolymers containing the resin as a main component. It is particularly preferable that the polyolefin resin is at least one selected from the group consisting of polypropylene resin and polyethylene resin. Further, as the polyolefin resin, one type may be blended alone, or two or more types of polyolefin resins may be used in combination.
  • the resin composition of the present invention has optional components such as an inorganic filler, an organic filler, a pigment, a dye, a radical initiator, a flame retardant, an antioxidant, an antioxidant, an antibacterial agent, an antibacterial agent, and a bactericidal agent.
  • the general additives and the like may be contained as long as the effects in the present invention are not impaired.
  • the radical initiator a peroxide agent or the like can be preferably used.
  • the antioxidant polyphenols such as catechin can be preferably used.
  • the resin composition of the present invention can be produced, for example, by putting each material into a kneader, kneading them, and then producing them with an extrusion molding machine.
  • the bleeding characteristics of the obtained resin composition can be controlled only by adding the flexible resin as a third component at the time of kneading, and the raw material resin material in which bleeding is likely to occur after recycling can also be utilized.
  • the obtained resin composition may be pelletized, or may be processed into a sheet or a film. In particular, since sheets and films have a large surface area, even a small amount of bleeding can affect the entire product such as texture and performance. Therefore, it can be preferably used as an applicable product of the technique.
  • FIG. 6 is an infrared spectroscopic spectrum obtained by measuring the surface of the test piece sheet by ATR measurement using a diamond crystal using Spectrum One manufactured by Perkin Elmer Japan Co., Ltd. in order to observe bleeding of the test piece.
  • the broken line shows the infrared spectroscopic spectrum of the surface of the test piece when pressurized with a force of 40% by the pressurizing unit of the universal ATR attached to the apparatus. Further, what is shown by a solid line is an infrared spectroscopic spectrum measured as it is without wiping the diamond crystal after removing the test piece from the diamond crystal by releasing the pressure after the above measurement. It can be seen that there is a peak due to bleeding between 1700 cm -1 and 1800 cm -1.
  • the test piece is once pressurized and opened by the ATR pressurizing unit with a force of 40%, then the test piece is removed from the diamond crystal, and the infrared spectroscopic spectrum is used as it is without wiping the diamond crystal.
  • the bleeding performance was evaluated by measuring the “infrared spectroscopic spectrum for bleeding evaluation”) and comparing it with the bleeding amount in this reference example.
  • FIG. 7A is obtained by using low density polyethylene (LDPE, “Novatec HD” LC525, manufactured by Nippon Polyethylene Co., Ltd.) as the polyolefin resin, kneading the components corresponding to the interlayer film, and forming a sheet by the T-die method. Similar to the reference example, the test piece was once pressurized and opened with a force of 40% by the ATR pressurizing unit, then the test piece was removed from the diamond crystal, and the infrared measured as it was without wiping the diamond crystal. It is a spectroscopic spectrum (infrared spectroscopic spectrum for bleed evaluation). In the figure, the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece. Moreover, what is shown by a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • LDPE low density polyethylene
  • LC525 manufactured by Nippon Polyethylene Co., Ltd.
  • the intermediate layer corresponds components, the molecular weight of 1.15 ⁇ 10 5 PVB ( "S-LEC B ⁇ K" BH-A, manufactured by Sekisui Chemical Co., Ltd.) to, triethylene glycol di-2-Echiruhekisano as a plasticizer
  • To 60 parts by weight of the polyolefin resin 20 parts by weight of the intermediate film equivalent component was added and kneaded, and a sheet was formed by the T-die method to obtain a test piece.
  • Example 1 low-density polyethylene (LDPE, "Novatec HD” LC525, manufactured by Nippon Polyethylene Co., Ltd.) is used as a polyolefin resin, and an interlayer equivalent component and a flexible resin component are kneaded and sheet-formed by the T-die method.
  • the obtained test piece is an infrared spectroscopic spectrum (infrared spectroscopic spectrum for bleed evaluation) measured in the same manner as in the reference example.
  • the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • the intermediate layer corresponds components, as in Comparative Example 1, the molecular weight of 1.15 ⁇ 10 5 PVB ( "S-LEC B ⁇ K" BH-A, manufactured by Sekisui Chemical Co., Ltd.) to, triethylene glycol as a plasticizer
  • a mixture of di-2-ethylhexanoate (G-260, manufactured by Sekisui Chemical Co., Ltd.) in a weight ratio of PVB: plasticizer 3: 1 was used.
  • the polyolefin resin With respect to 60 parts by weight of the polyolefin resin, 20 parts by weight of the interlayer film equivalent component and 5 parts by weight of a block-type styrene-butadiene rubber B-SBR (“Nipol” NS380S, manufactured by Nippon Zeon Corporation) as a flexible resin component.
  • B-SBR block-type styrene-butadiene rubber
  • the mixture was kneaded and sheet-molded by the T-die method to obtain a test piece.
  • Example 2 A test piece was prepared in the same manner as in Example 1 except that 10 parts by weight of a block-type styrene-butadiene rubber B-SBR (“Nipol” NS380S, manufactured by Nippon Zeon Corporation) was added as a flexible resin component.
  • B-SBR block-type styrene-butadiene rubber
  • the result of measuring the infrared spectroscopic spectrum for bleed evaluation is shown in FIG.
  • the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • Example 3 A test piece was prepared in the same manner as in Example 1 except that 15 parts by weight of a block-type styrene-butadiene rubber B-SBR (“Nipol” NS380S, manufactured by Nippon Zeon Corporation) was added as a flexible resin component.
  • B-SBR block-type styrene-butadiene rubber
  • the result of measuring the infrared spectroscopic spectrum for bleed evaluation is shown in FIG.
  • the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • Example 4 A test piece was prepared in the same manner as in Example 1 except that 20 parts by weight of a random type styrene-butadiene rubber R-SBR (“Nipol” 1502, manufactured by Nippon Zeon Corporation) was added as a flexible resin component.
  • R-SBR random type styrene-butadiene rubber
  • the result of measuring the infrared spectroscopic spectrum for bleed evaluation is shown in FIG.
  • the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • Example 5 Test piece as in Example 1 except that 20 parts by weight of ethylene vinyl acetate copolymer EVA (“Ultrasen” injection grade 633, manufactured by Tosoh Corporation), which is a copolymerized olefin resin, was added as a flexible resin component. was produced.
  • EVA ethylene vinyl acetate copolymer
  • the result of measuring the infrared spectroscopic spectrum for bleed evaluation is shown in FIG. In the figure, the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • FIG. 7B shows a test piece obtained by kneading a component corresponding to an interlayer film using low-density polyethylene (LDPE, “Novatec HD” LC525, manufactured by Nippon Polyethylene Co., Ltd.) as a polyolefin resin and injection molding. It is an infrared spectroscopic spectrum (infrared spectroscopic spectrum for bleed evaluation) measured in the same manner as the reference example. In the figure, the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece. Moreover, what is shown by a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • LDPE low-density polyethylene
  • low-density polyethylene (LDPE, “Novatec HD” LC525, manufactured by Nippon Polyethylene Co., Ltd.) is used as the polyolefin resin, and the interlayer film equivalent component and the flexible resin component are kneaded and sheeted by the T-die method.
  • LDPE low-density polyethylene
  • the interlayer film equivalent component and the flexible resin component are kneaded and sheeted by the T-die method.
  • the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • what is shown by a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • PVB polymethyl methacrylate
  • PVB plasticizer
  • 3: 1 ester-based plasticizer
  • Example 7 A test piece was prepared in the same manner as in Example 6 except that 5 parts by weight of a block-type styrene-butadiene rubber B-SBR (“Nipol” NS380S, manufactured by Nippon Zeon Corporation) was added as a flexible resin component.
  • B-SBR block-type styrene-butadiene rubber
  • FIG. 8 (B) The result of measuring the infrared spectroscopic spectrum for bleed evaluation is shown in FIG. 8 (B).
  • the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • Example 8 A test piece was prepared in the same manner as in Example 6 except that 10 parts by weight of a block-type styrene-butadiene rubber B-SBR (“Nipol” NS380S, manufactured by Nippon Zeon Corporation) was added as a flexible resin component.
  • B-SBR block-type styrene-butadiene rubber
  • FIG. 8 (C) The results of measuring the infrared spectroscopic spectrum for bleed evaluation are shown in FIG. 8 (C).
  • the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • Example 9 A test piece was prepared in the same manner as in Example 6 except that 15 parts by weight of a block-type styrene-butadiene rubber B-SBR (“Nipol” NS380S, manufactured by Nippon Zeon Corporation) was added as a flexible resin component.
  • B-SBR block-type styrene-butadiene rubber
  • FIG. 8 (D) The results of measuring the infrared spectroscopic spectrum for bleed evaluation are shown in FIG. 8 (D).
  • the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • Example 10 A test piece was prepared in the same manner as in Example 6 except that 20 parts by weight of a block-type styrene-butadiene rubber B-SBR (“Nipol” NS380S, manufactured by Nippon Zeon Corporation) was added as a flexible resin component.
  • B-SBR block-type styrene-butadiene rubber
  • FIG. 8 (E) The result of measuring the infrared spectroscopic spectrum for bleed evaluation is shown in FIG. 8 (E).
  • the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • Example 11 A test piece was prepared in the same manner as in Example 6 except that 20 parts by weight of a high diene type ethylene propylene diene rubber (EPDM, "ESPRENE505", manufactured by Sumitomo Chemical Co., Ltd.) was added as a flexible resin component.
  • EPDM high diene type ethylene propylene diene rubber
  • FIG. 9 (A) The result of measuring the infrared spectroscopic spectrum for bleed evaluation is shown in FIG. 9 (A).
  • the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • Example 12 Test piece as in Example 6 except that 20 parts by weight of ethylene vinyl acetate copolymer EVA (“Ultrasen” injection grade 633, manufactured by Tosoh Corporation), which is a copolymerized olefin resin, was added as a flexible resin component. was produced.
  • EVA ethylene vinyl acetate copolymer
  • FIG. 9 (B) The result of measuring the infrared spectroscopic spectrum for bleed evaluation is shown in FIG. 9 (B).
  • the broken line shows the infrared spectroscopic spectrum for bleed evaluation of this test piece.
  • a solid line is an infrared spectroscopic spectrum for bleed evaluation for a reference example.
  • the method for preparing the test piece for measurement used in the above is as follows. When there was a material that was not blended in each test piece, the step was appropriately omitted and the following production method was applied.
  • each material was processed into a shape that can be put into the hopper of a twin-screw extruder (for example, a powder or granular material of several millimeters square).
  • each material was mixed in advance before being put into the hopper of the twin-screw extruder.
  • each material processed as described above was kneaded using a twin-screw extruder equipped with a T-type die (T die) as a die.
  • T die T-type die
  • the operating conditions of the device were a screw rotation speed of 250 rpm and a feeder discharge rate of 15 g / min.
  • the twin-screw extruder has six cylinders of the first to sixth cylinders, and the set temperature of each cylinder is set to 160 ° C. for the first cylinder to the sixth cylinder and the T die.
  • Each material was heated and mixed with a twin-screw extruder, and the resin mixture was extruded from the T-die of the twin-screw extruder.
  • the extruded mixture was a sheet, which was immediately cooled and solidified with a rotary cooling roll set at 25 ° C., and then wound around a paper tube to obtain a test piece.
  • FIG. 10A is obtained by using low density polyethylene (LDPE, “Novatec HD” LC525, manufactured by Nippon Polyethylene Co., Ltd.) as the polyolefin resin, kneading the components corresponding to the interlayer film, and forming a sheet by a heat pressing method. This is the result of extracting the surface component of the test piece and measuring the extracted component by the gas chromatograph mass spectrometry method.
  • LDPE low density polyethylene
  • LC525 low density polyethylene
  • the intermediate layer corresponds components, the molecular weight of 1.15 ⁇ 10 5 PVB ( "S-LEC B ⁇ K" BH-A, manufactured by Sekisui Chemical Co., Ltd.) to, triethylene glycol di-2-Echiruhekisano as a plasticizer
  • To 60 parts by weight of the polyolefin resin 20 parts by weight of the interlayer film equivalent component was added and kneaded in a batch manner, and a sheet was formed by a heat pressing method to obtain a test piece.
  • FIG. 10B is obtained by using low density polyethylene (LDPE, “Novatec HD” LC525, manufactured by Nippon Polyethylene Co., Ltd.) as the polyolefin resin, kneading the components corresponding to the interlayer film, and forming a sheet by a heat pressing method. This is the result of extracting the surface component of the test piece and measuring the extracted component by the gas chromatograph mass spectrometry method.
  • LDPE low density polyethylene
  • FIG. 10C shows a sheet using low-density polyethylene (LDPE, “Novatec HD” LC525, manufactured by Japan Polyethylene Corporation) as a polyolefin resin, kneading an interlayer film-equivalent component and a flexible resin component, and using a heat pressing method.
  • LDPE low-density polyethylene
  • LC525 low-density polyethylene
  • the polyolefin resin With respect to 60 parts by weight of the polyolefin resin, 20 parts by weight of the interlayer film equivalent component and ethylene vinyl acetate copolymer EVA (“Ultrasen” grade 633 for injection, which is a copolymerized olefin resin as a flexible resin component, Toso Co., Ltd.) (Manufactured by the company) 10 parts by weight was added, batch kneading was performed, and a sheet was formed by a heating press method to obtain a test piece.
  • EVA ethylene vinyl acetate copolymer
  • the method for producing the test piece for measurement used in Comparative Examples 3 and 4 and Example 13 is as follows. (Batch type kneading) Each material was put into a batch type kneader (10S100, manufactured by Toyo Seiki Seisakusho Co., Ltd.) set at 140 ° C. and kneaded at a rotation speed of 12.5 rpm for 10 minutes to obtain a kneaded sample.
  • the above-described embodiment is merely an example for carrying out the present invention. Therefore, the present invention is not limited to the above-described embodiment, and the above-described embodiment can be appropriately modified and implemented within a range that does not deviate from the gist thereof.
  • the present invention it is possible to utilize the polyvinyl acetal for a laminated glass interlayer film sheet containing a liquid plasticizer, which is on the market. According to the present invention, it is possible to utilize materials such as used glass interlayer films, which have had to be discarded until now, as valuable resources because it is difficult to recycle due to difficulty in handling and problems in terms of properties. Not only will it have the effect of reducing the burden on the environment, but it will also contribute significantly to industrial use.

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Abstract

Dans la présente invention, une composition de résine est obtenue dans laquelle le dégorgement d'un agent plastifiant ou similaire depuis la composition est régulé même dans les cas où une matière première contenant une grande quantité d'agent plastifiant est contenue à l'intérieur, telle qu'une feuille intermédiaire, et qui permet l'utilisation d'une résine matière première dans le recyclage. Cette composition de résine est caractérisée par : le fait qu'elle contient une résine à base de polyoléfine et une résine de poly(vinyl acétal) (excluant une résine de poly(vinyl formal)) qui contient un agent plastifiant ; et contenant en outre au moins un type de résine souple sélectionné dans le groupe constitué d'un caoutchouc synthétique, d'un élastomère et d'une résine d'oléfine copolymère. Lorsque la résine de poly(vinyl acétal) contenant un agent plastifiant et la résine à base de polyoléfine sont malaxées, au moins un type de résine souple sélectionné dans le groupe constitué d'un caoutchouc synthétique, d'un élastomère et d'une résine d'oléfine copolymère est ajouté comme agent de régulation du dégorgement.
PCT/JP2021/005046 2020-03-10 2021-02-10 Composition de résine et procédé de recyclage de résine de poly(vinyl acétal) WO2021181999A1 (fr)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012026501A1 (fr) * 2010-08-27 2012-03-01 株式会社クラレ Composition polymère thermoplastique et article moulé
JP2013141794A (ja) * 2012-01-11 2013-07-22 Kuraray Co Ltd 接着体の製造方法
WO2017200052A1 (fr) * 2016-05-18 2017-11-23 株式会社クラレ Composition de résine, film et couche intermédiaire pour verre feuilleté
WO2017200053A1 (fr) * 2016-05-18 2017-11-23 株式会社クラレ Couche intermédiaire de verre feuilleté, et verre feuilleté
WO2019065920A1 (fr) * 2017-09-29 2019-04-04 積水化学工業株式会社 Système de cellule solaire
WO2019098187A1 (fr) * 2017-11-14 2019-05-23 株式会社ガラステクノシナジー Composition de résine
CN109880196A (zh) * 2019-04-01 2019-06-14 华东理工大学 一种丁腈橡胶组合物及其发泡材料

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012026501A1 (fr) * 2010-08-27 2012-03-01 株式会社クラレ Composition polymère thermoplastique et article moulé
JP2013141794A (ja) * 2012-01-11 2013-07-22 Kuraray Co Ltd 接着体の製造方法
WO2017200052A1 (fr) * 2016-05-18 2017-11-23 株式会社クラレ Composition de résine, film et couche intermédiaire pour verre feuilleté
WO2017200053A1 (fr) * 2016-05-18 2017-11-23 株式会社クラレ Couche intermédiaire de verre feuilleté, et verre feuilleté
WO2019065920A1 (fr) * 2017-09-29 2019-04-04 積水化学工業株式会社 Système de cellule solaire
WO2019098187A1 (fr) * 2017-11-14 2019-05-23 株式会社ガラステクノシナジー Composition de résine
CN109880196A (zh) * 2019-04-01 2019-06-14 华东理工大学 一种丁腈橡胶组合物及其发泡材料

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