WO2023243176A1 - Mélange-maître en forme de pastille, composition de résine et procédé de fabrication d'une composition de résine - Google Patents

Mélange-maître en forme de pastille, composition de résine et procédé de fabrication d'une composition de résine Download PDF

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Publication number
WO2023243176A1
WO2023243176A1 PCT/JP2023/011878 JP2023011878W WO2023243176A1 WO 2023243176 A1 WO2023243176 A1 WO 2023243176A1 JP 2023011878 W JP2023011878 W JP 2023011878W WO 2023243176 A1 WO2023243176 A1 WO 2023243176A1
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component
masterbatch
resin
resin composition
minutes
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PCT/JP2023/011878
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English (en)
Japanese (ja)
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美帆子 西尾
真理 矢部
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出光興産株式会社
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Publication of WO2023243176A1 publication Critical patent/WO2023243176A1/fr

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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
    • C08J3/20—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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • 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
    • 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
    • C08L23/12—Polypropene

Definitions

  • the present invention relates to a pellet masterbatch, a resin composition, and a method for producing a resin composition.
  • thermoplastic resins such as molded products and nonwoven fabrics
  • additives for the purpose of imparting functionality or coloring.
  • a method is known in which masterbatch pellets containing additives at a relatively high concentration are produced in advance and the pellets are added to a thermoplastic resin.
  • Patent Document 1 discloses a masterbatch composition having a specific composition.
  • An object of the present invention is to provide a pellet-like masterbatch that can provide a greater effect of additives to a thermoplastic resin.
  • the masterbatch was developed by using a polypropylene resin having specific physical properties as the resin component (dispersion medium for additives) and by making almost the entire amount of the polypropylene resin. It is possible to improve the dispersibility when blending additives into thermoplastic resin using a batch process, and as a result, it becomes possible to impart a greater effect of additives to thermoplastic resin (resin composition). They discovered this and completed the present invention. According to the present invention, the following pelleted masterbatch and the like are provided. 1.
  • thermoplastic resin is a polypropylene resin.
  • B A method for producing a resin composition containing an additive that is solid at room temperature and normal pressure and a thermoplastic resin, (A) Using a differential scanning calorimeter (DSC), the sample was heated from -40°C under a nitrogen atmosphere to 220°C at a rate of 10°C/min, held for 5 minutes, and then raised to -40°C at a rate of 10°C/min. The melting endotherm ( ⁇ H-D) obtained from the melting endothermic curve obtained by lowering the temperature and holding it for 15 minutes, then raising the temperature again at 10°C/min to 220°C is 0 J/g or more and 80 J/g or less. Dispersing the component (B) in the thermoplastic resin by blending a pelletized masterbatch containing a certain polypropylene resin and the component (B) into the thermoplastic resin, A method for producing a resin composition.
  • DSC differential scanning calorimeter
  • thermoplastic resins According to the present invention, it is possible to provide a pellet-shaped masterbatch that can impart greater effects of additives to thermoplastic resins.
  • x to y represents a numerical range of "x to y”.
  • the upper limit and lower limit may be arbitrarily selected and combined. shall be able to do so.
  • the pellet masterbatch according to one aspect of the present invention contains the following components (A) and (B), with more than 99% by mass being the component (A) and the component (B).
  • A Using a differential scanning calorimeter (DSC), the sample was heated from -40°C under a nitrogen atmosphere to 220°C at a rate of 10°C/min, held for 5 minutes, and then raised to -40°C at a rate of 10°C/min. If the melting endotherm ( ⁇ H-D) obtained from the melting endothermic curve obtained by lowering the temperature and holding it for 15 minutes, then raising the temperature again at 10 ° C / min to 220 ° C.
  • DSC differential scanning calorimeter
  • a masterbatch is a pellet used when mixing additives with a thermoplastic resin. It is a resin composition in which the additive is dispersed in another resin at a predetermined concentration.
  • the polypropylene resin of component (A) is a material with an extremely small melting endotherm ( ⁇ HD) and a very low degree of crystallinity.
  • ⁇ HD extremely small melting endotherm
  • Component (A) is a resin having a considerably large proportion of amorphous portions, and is a material in which countless sparse amorphous regions with low density exist throughout the resin.
  • the additive By retaining a very small amount of the additive (component (B)) in each of these countless amorphous regions, the additive can easily diffuse throughout the component (A) and is less likely to aggregate. Conceivable.
  • the additive can be easily dispersed also in the thermoplastic resin. That is, at the masterbatch stage, the additives are captured by the amorphous regions of component (A) and are finely dispersed, so when the masterbatch and thermoplastic resin are kneaded, the component (A) becomes It is thought that by diffusing into the thermoplastic resin, the additive is also uniformly and finely dispersed in the thermoplastic resin in a form led by the component (A).
  • the effect of the additive can be maximized, that is, it becomes possible to impart a greater effect of the additive to the thermoplastic resin. This allows the same effect to be obtained with a smaller amount, making it possible to reduce the amount of additive.
  • a resin other than component (A) is used as a dispersion medium in a masterbatch, that is, a resin with a high degree of crystallinity and a small amount of amorphous region
  • the additive has no choice but to remain in a small amount of amorphous region, resulting in poor dispersibility. becomes lower and aggregation becomes more likely to occur.
  • the results are the same even if component (A) is used as the thermoplastic resin in which the masterbatch is blended, and it is difficult to disperse the additive once it is captured in other resins. Even if component (A) is added afterwards, the dispersibility of the additive in the thermoplastic resin is hardly improved.
  • Component (A) is a polypropylene resin with an extremely small melting endotherm ( ⁇ HD) (condition (i)).
  • ⁇ HD melting endotherm
  • the melting endotherm ( ⁇ HD) of component (A) is 70 J/g or less, 60 J/g or less, or 50 J/g or less. It is expected that the lower the melting endotherm ( ⁇ HD), the more amorphous regions there will be in component (A), and the more the dispersibility of the additive can be improved.
  • the melting endotherm ( ⁇ HD) of component (A) is 5 J/g or more, or 15 J/g or more. When the melting endotherm ( ⁇ HD) is within this range, stickiness can be suppressed and handling properties can be improved.
  • the melting endotherm ( ⁇ HD) is measured by the following method. Using a differential scanning calorimeter (Perkin Elmer's "DSC-8500"), 10 mg of the sample was heated from -40°C to 220°C at a rate of 10°C/min in a nitrogen atmosphere, held for 5 minutes, and then heated to 10°C. The temperature was lowered to -40°C at a rate of 10°C/min, held for 15 minutes, and then raised again to 220°C at a rate of 10°C/min. The melting endothermic amount ( ⁇ HD) is determined from the melting endothermic curve obtained during the second temperature increase.
  • DSC-8500 differential scanning calorimeter
  • the endotherm of fusion ( ⁇ H-D) is measured using a differential scanning calorimeter (Perkin-Elmer "DSC") using a line connecting a point on the low temperature side with no change in calorific value and a point on the high temperature side with no change in calorific value as the baseline. It is calculated by determining the area surrounded by the base line and the line portion including the peak of the melting endothermic curve obtained by DSC measurement using "-8500").
  • the melting endotherm ( ⁇ HD) can be appropriately controlled by adjusting the monomer concentration and reaction pressure.
  • Component (A) is preferably a propylene homopolymer.
  • Component (A) preferably satisfies the following condition (ii).
  • (ii) Half crystallization time at 25°C is 30 seconds or more.
  • a long half-crystallization time means a slow crystallization rate, and the slower the crystallization rate, the longer the contact time with the component (B) in the molten state, which is preferable.
  • the half-crystallization time of component (A) is 1 minute or more, or 5 minutes or more.
  • the half crystallization time of component (A) is 30 minutes or less, 40 minutes or less, or 50 minutes or less.
  • the crystallization rate is measured by the following method. Using a differential scanning calorimeter (Perkin Elmer “DSC-8500”), 10 mg of the sample was held at 25°C for 5 minutes, then heated to 220°C at 320°C/sec, held for 5 minutes, and then heated to 320°C. The sample is cooled to 25° C./second and held for 60 minutes to measure the change in calorific value over time during the isothermal crystallization process. When the integral value of the calorific value from the start of isothermal crystallization to the completion of crystallization is taken as 100%, the time from the start of isothermal crystallization until the integral value of the calorific value reaches 50% is determined as the half crystallization time. .
  • DSC-8500 differential scanning calorimeter
  • Component (A) preferably satisfies the following condition (iii).
  • (iii) Using a differential scanning calorimeter (DSC), the sample was held at -40°C for 5 minutes in a nitrogen atmosphere, and then heated at a rate of 10°C/min.
  • the melting point (Tm-D) defined as the observed peak top is 40°C or more and 100°C or less.
  • the melting point (Tm-D) of component (A) is 50°C or higher, or 60°C or higher.
  • the melting point (Tm-D) of component (A) is 90°C or less.
  • the melting point (Tm-D) is measured using a differential scanning calorimeter (Perkin-Elmer "DSC-8500") after holding 10 mg of the sample at -40°C for 5 minutes in a nitrogen atmosphere. This value is defined as the peak top observed on the highest temperature side of the melting endothermic curve obtained by raising the temperature at a rate of °C/min.
  • Component (A) preferably satisfies the following condition (iv).
  • the mesopentad fraction [mmmm] is 20 to 60 mol%.
  • the mesopentad fraction [mmmm] is an index representing the stereoregularity of a propylene homopolymer, and the larger the mesopentad fraction [mmmm], the higher the stereoregularity.
  • the mesopentad fraction [mmmm] of component (A) is 30 mol% or more, or 40 mol% or more.
  • the mesopentad fraction [mmmm] of component (A) is 55 mol% or less, or 50 mol% or less.
  • the mesopentad fraction [mmmm] is measured by the signal of the methyl group in the 13 C-NMR spectrum according to the method proposed by A. Zambelli et al. in "Macromolecules, 6, 925 (1973)". This value is determined as the meso fraction of pentad units in the polypropylene molecular chain.
  • Component (A) preferably satisfies the following condition (v) from the viewpoint of pelletizing the masterbatch.
  • (v) Weight average molecular weight (Mw) is 25,000 or more. In one embodiment, the Mw of component (A) is 30,000 or more, 35,000 or more, or 40,000 or more. There is no particular upper limit, but it is, for example, 500,000 or less.
  • the weight average molecular weight (Mw) is a value determined by gel permeation chromatography (GPC), measured using the GPC device shown below under the conditions shown below.
  • GPC device > Equipment: “HLC8321GPC/HT” manufactured by Tosoh Corporation Detector: RI detector column: Tosoh Corporation "TOSOH GMHHR-H(S)HT” x 2 ⁇ Measurement conditions> Solvent: 1,2,4-trichlorobenzene Measurement temperature: 145°C Flow rate: 1.0mL/min Sample concentration: 0.5mg/mL Injection volume: 300 ⁇ L Calibration curve: Prepared using PS standard material Molecular weight conversion: Converted using Universal Calibration method ⁇ PS: 0.707, ⁇ PS: 0.00121, ⁇ PP: 0.750, ⁇ PP: 0.0137 Analysis program: 8321GPC-WS
  • Component (A) preferably satisfies the following condition (vi).
  • Melt flow rate (MFR) is 1 g/10 minutes or more.
  • the MFR of component (A) is 7 g/10 minutes or more, or 10 g/10 minutes or more.
  • the MFR of component (A) is 5000 g/10 minutes or less, 4500 g/10 minutes or less, or 4000 g/10 minutes or less.
  • MFR is measured in accordance with ISO 1133:1997 at a temperature of 230° C. and a load of 2.16 kg.
  • Component (A) can be produced in the same manner as the method for producing the "olefin polymer” in Patent Document 1.
  • component (A) commercially available products can be used, such as "L-MODU” (registered trademark) manufactured by Idemitsu Kosan Co., Ltd. (for example, “S400”, “S401”, “S600”, “S901”) etc. can be used.
  • any additive that is solid at normal temperature and normal pressure in an environment of 1 bar and 0° C.
  • the additive is preferably in powder form, and the particle shape may be spherical, fibrous (acicular), plate-like, or the like.
  • the particle size for example, particles with a diameter of 100 nm to 100 ⁇ m can be used. Note that the particle diameter is determined by the major axis.
  • Additives are generally used for the purpose of improving (modifying) the physical properties of thermoplastic resins, imparting functionality, improving moldability, stabilizing them, and the like.
  • Physical property improvers include strength improvers, crosslinking agents, decomposition agents, softeners, flame retardants, flame retardant aids, coupling agents, photosensitizers, photopolymerization initiators, curing agents, etc. It will be done.
  • Functionality-imparting agents include sliding agents (slip agents), antifogging agents, conductive agents, antistatic agents, thermal conductive agents, foaming agents, coloring agents (dyes, pigments), fluorescent agents, fragrances, deodorants, Examples include surfactants, insect repellents, insecticides, antibacterial and antifungal agents, and the like.
  • Formability improvers include viscosity modifiers (thickeners, thinners), plasticizers, crystal nucleating agents, crystallization rate modifiers, lubricants, and release agents. Examples include molding agents.
  • the stabilizer include antioxidants, anti-aging agents, weathering agents, light stabilizers, agents that prevent decomposition such as main chain cleavage due to heat or hydrolysis, antibacterial agents, and the like.
  • the additive it is also possible to use materials (fillers) that are added simply for the purpose of increasing the bulk of the resin composition or for the purpose of substituting the resin component.
  • the additive does not impart a specific effect to the thermoplastic resin, according to the present invention, by increasing the dispersibility of the material, it is possible to suppress deterioration of the physical properties of the resin component due to the additive. It can be said that the effect of the additive can be sufficiently enhanced. Furthermore, it can fully respond to demands such as reducing the amount of plastic used due to environmental concerns, and can play an important role.
  • component (B) is calcium carbonate (modifier, functionality-imparting agent or filler), talc (modifier, functionality-imparting agent or filler), montmorillonite (modifier or functionality-imparting agent), ), carbon (modifier or functionality-imparting agent), colorant/pigment (modifier or functionality-imparting agent), titanium oxide (modifier, functionality-imparting agent, or filler), cellulose (modifier, One or more components selected from the group consisting of (functionality imparting agent or filler), glass, and a nucleating agent (formability improving agent).
  • pellet masterbatch The content of component (B) in the pelletized masterbatch according to one aspect of the present invention is not particularly limited, but is, for example, 80% by mass or less, and, for example, 30% by mass or more.
  • More than 99% by mass of the pelleted masterbatch is the (A) component and the (B) component, and 99.5% by mass or more, 99.9% by mass or more, or 100% by mass is the (A) component and the (B) component. There may be.
  • Examples of the method for producing a pellet masterbatch include a method in which components (A) and (B) are put into an extruder, heated, kneaded, extruded into strands, and cut into pellets. However, it is not limited to this.
  • a resin composition in which the component (B) (additive) is uniformly dispersed can be produced by blending the pelletized masterbatch according to one aspect of the present invention described above with a thermoplastic resin. Can be done.
  • thermoplastic resin is not particularly limited, and polyolefin resins and thermoplastic resins other than polyolefin resins can be used.
  • polyolefin resin examples thereof include ⁇ -olefin homopolymers, ⁇ -olefin copolymers, copolymers of ⁇ -olefins and vinyl monomers, ethylene-unsaturated carboxylic acid ester copolymers, and ethylene-unsaturated carboxylic acid ester copolymers. Examples include carboxylic acid unsaturated ester copolymers.
  • Polyolefin resins may be used alone or in combination of two or more. Furthermore, the above-mentioned component (A) may be used as at least a part of the thermoplastic resin.
  • Thermoplastic resins other than polyolefin resins include, for example, polystyrene resins such as polystyrene, rubber reinforced polystyrene (HIPS), isotactic polystyrene, and syndiotactic polystyrene; acrylonitrile-styrene resin (AS), acrylonitrile-butadiene- Polyacrylonitrile resins such as styrene resin (ABS); polymethacrylate resins, polyamide resins, polyester resins, polycarbonate resins, polyphenylene resins, polyphenylene ether resins, polyphenylene sulfide resins, polyphenylene sulfone resins, rosin Examples include terpene-based resins, chroman-indene-based resins, petroleum resins, and the like. These thermoplastic resins may be used alone or in combination of two or more.
  • the amount of the pellet masterbatch to be added to the thermoplastic resin is, for example, 0.1 to 90 parts by mass, or 1 to 80 parts by mass, based on 100 parts by mass of the thermoplastic resin.
  • the amount of the pelletized masterbatch is more than 10 parts by mass based on 100 parts by mass of the thermoplastic resin, for example, more than 10 parts by mass and 90 parts by mass or less, or more than 10 parts by mass. and 80 parts by mass or less.
  • the amount of the pelletized masterbatch is more than 10 parts by mass based on 100 parts by mass of the polyolefin resin in the thermoplastic resin, for example, more than 10 parts by mass and 90 parts by mass or less, or , more than 10 parts by mass and not more than 80 parts by mass.
  • the method for producing the resin composition can also be expressed as follows.
  • DSC differential scanning calorimeter
  • the melting endotherm ( ⁇ H-D) obtained from the melting endothermic curve obtained by lowering the temperature and holding it for 15 minutes, then raising the temperature again at 10°C/min to 220°C is 0 J/g or more and 80 J/g or less.
  • the resin composition obtained above can be used as a raw material for various resin products.
  • molded products made by injection molding or extrusion molding can be mentioned, and specific examples include sheets, films, various containers (food, daily necessities, etc.), various parts (for automobiles, packaging materials, etc.), but are not limited to these. Not done.
  • ⁇ Polypropylene> A1 Homopolypropylene (“L-MODU S401” manufactured by Idemitsu Kosan Co., Ltd., melting endotherm ( ⁇ H-D): 36 J/g, half-crystalization time at 25°C: 21 minutes, melting point (Tm-D): 80°C , weight average molecular weight: 45,000, MFR: 2,600g/10min)
  • A2 Homopolypropylene (“L-MODU S901” manufactured by Idemitsu Kosan Co., Ltd., melting endotherm ( ⁇ H-D): 40 J/g, half-crystalization time at 25°C: 4 minutes, melting point (Tm-D): 80°C , weight average molecular weight: 130,000, MFR: 50g/10min)
  • A'1 Homopolypropylene (commercial product, melting endotherm ( ⁇ H-D): 120 J/g, half crystallization time
  • Example 1 Manufacture of pelleted masterbatch
  • Polypropylene A1 (pellet form) and additive B1 were put into a twin screw extruder and kneaded while heating.
  • the amount of B1 was 60% by mass based on the total amount of A1 and B1.
  • the kneaded masterbatch composition was extruded into a strand shape and cooled to about room temperature.
  • the cooled masterbatch composition was cut into pellets to obtain pelletized masterbatch 1.
  • Raw material mixture 1 was prepared by dry blending pellet masterbatch 1 and polypropylene Z1 (pellet) so that the proportion of pellet masterbatch 1 was 25% by mass.
  • the suction pressure of the ejector was gradually increased, and the ejector pressure (also referred to as "maximum ejector pressure") immediately before fiber breakage occurred was measured.
  • a high maximum ejector pressure means that the fiber has high drawability and spinnability.
  • Example 2 A pellet masterbatch and a raw material mixture were prepared and evaluated in the same manner as in Example 1, except that Additive B1 was changed to Additive B2. The results are shown in Table 1.
  • Example 3 A pellet masterbatch and a raw material mixture were prepared and evaluated in the same manner as in Example 1 except that polypropylene A1 was changed to polypropylene A2. The results are shown in Table 1.
  • Comparative example 1 Pellet masterbatch Ref. containing polypropylene A'1 (28.5% by mass) and additive B2 (71.5% by mass). 1 was used. Pellet masterbatch Ref. 1 and polypropylene Z1 (pellet-like) were mixed into a pellet-like masterbatch Ref. A raw material mixture was produced by dry blending so that the proportion of 1 was 21% by mass. Evaluation was performed in the same manner as in Example 1 using the raw material mixture. The results are shown in Table 1.
  • Comparative example 2 Polypropylene A1 (10% by mass), polypropylene Z1 (69% by mass), and pelletized masterbatch Ref. 1 (21% by mass) to produce a raw material mixture. Evaluation was performed in the same manner as in Example 1 using the raw material mixture. The results are shown in Table 1.
  • Comparative example 3 [Manufacture of pelleted masterbatch] A dry blend of polypropylene A2 (pellet form) and polypropylene Z1 (pellet form) at a mass ratio of 2:1 and additive B1 were charged into a twin screw extruder and kneaded while heating. The amount of B1 was 60% by mass based on the total amount of A2, Z1 and B1. The kneaded masterbatch composition was extruded into a strand shape and cooled to about room temperature. The cooled masterbatch composition is cut into pellets, and the pelletized masterbatch Ref. I got 2.
  • Example 2 the additive and component (A) were first kneaded to form a masterbatch, and then mixed with other resins to form a resin composition, thereby improving the dispersibility of the additive in the resin composition. This is thought to have resulted in the realization of superior strength.
  • Comparative Examples 1 and 2 since a resin other than component (A) was used as the dispersion medium resin in the masterbatch, the degree of dispersion of the additive in the resin composition could not be increased, and the strength could not be increased. There wasn't.
  • component (A) was not used as the resin component of the masterbatch, but component (A) was added during the production of the resin composition.
  • component (A) was not used as the resin component of the masterbatch, but component (A) was added during the production of the resin composition.
  • the results are similar to those of Comparative Example 1 in which component (A) is not used at all, so in order to improve the dispersibility of the additive in the resin composition, it is necessary to It can be seen that it is important to use component (A) as a dispersion medium for the resin, that is, the masterbatch.

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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)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne un mélange-maître en forme de pastille contenant : (A) une résine de polypropylène qui présente une énergie endothermique à l'état fondu (ΔH-D) de 0 à 80 J/g, inclusivement, lorsqu'elle est obtenue à partir d'une courbe endothermique à l'état fondu obtenue en utilisant un calorimètre différentiel à balayage (DSC), en chauffant un échantillon dans une atmosphère d'azote de -40°C à 220°C à une vitesse de 10°C/minute, en maintenant cette température pendant 5 minutes, puis en refroidissant l'échantillon à -40°C à une vitesse de 10°C/minute, en maintenant cette température pendant 15 minutes, puis en chauffant à nouveau l'échantillon à 220°C à une vitesse de 10°C/minute ; (B) et un additif qui est solide à une température et une pression normales. Ainsi, le composant (A) et le composant (B) constituent plus de 99 % en masse du mélange-maître.
PCT/JP2023/011878 2022-06-15 2023-03-24 Mélange-maître en forme de pastille, composition de résine et procédé de fabrication d'une composition de résine WO2023243176A1 (fr)

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