WO2012026127A1 - Composition de résine et verre feuilleté granulaire - Google Patents

Composition de résine et verre feuilleté granulaire Download PDF

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Publication number
WO2012026127A1
WO2012026127A1 PCT/JP2011/004737 JP2011004737W WO2012026127A1 WO 2012026127 A1 WO2012026127 A1 WO 2012026127A1 JP 2011004737 W JP2011004737 W JP 2011004737W WO 2012026127 A1 WO2012026127 A1 WO 2012026127A1
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WIPO (PCT)
Prior art keywords
flaky glass
glass
granular
binder
mass
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PCT/JP2011/004737
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English (en)
Japanese (ja)
Inventor
健 前田
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日本板硝子株式会社
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Priority to JP2012530541A priority Critical patent/JP5858916B2/ja
Publication of WO2012026127A1 publication Critical patent/WO2012026127A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/005—Manufacture of flakes
    • 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
    • C08K3/40—Glass

Definitions

  • the present invention relates to a resin composition and granular flaky glass.
  • Flaked glass is widely used for applications such as resin reinforcements and anticorrosion lining fillers.
  • Japanese Patent Application Laid-Open No. 62-109855 discloses a technique for improving the strength and dimensional stability of flaky glass blended with a thermoplastic resin.
  • JP-A-63-225554, JP-A-3-86753, JP-A-5-287175, JP-A-2002-212421 and JP-A-2003-82260 disclose a binder or surface treatment.
  • a technique of blending granule-type flaky glass granulated with an agent into a thermoplastic resin is described.
  • Flaked glass is a scaly flake, so it has a high scattering property, and there is a problem that workability until blended with a thermoplastic resin is poor.
  • an extrusion molding machine is generally used.
  • flaky glass is bulky and has poor fluidity, it clogs the feed part of the molding machine, There is a problem that the bite is bad.
  • a technique has been developed in which flaky glass is granulated using a binder or a surface treatment agent to form granules and then blended into a thermoplastic resin.
  • a flaky glass filler containing 90% by mass of a flaky glass having a thickness of 0.01 to 2.0 ⁇ m it is known to use a flaky glass filler containing 90% by mass of a flaky glass having a thickness of 0.01 to 2.0 ⁇ m. It is described in.
  • a molecular weight for example, a weight average molecular weight
  • a decrease in the molecular weight of the resin is not preferable because the viscosity of the resin decreases. If the molecular weight is extremely lowered, the strength characteristics of the resin molded product may be lowered.
  • the object of the present invention is to prevent as much as possible a decrease in the molecular weight of a resin (particularly polycarbonate) when granulated flaky glass is added to the resin.
  • the present invention Including polycarbonate and granular flaky glass
  • the granular flaky glass is (A) flaky glass having an average thickness of 0.1 to 2.0 ⁇ m and an average particle diameter of 10 to 2000 ⁇ m; (B) a binder that is contained in a range of more than 2.0% by mass and 5.0% by mass or less in terms of solid content with respect to the granular flaky glass, and granulates the flaky glass; A resin composition is provided.
  • the present invention is a granular flaky glass comprising: Flaky glass having an average thickness of 0.1 to 2.0 ⁇ m and an average particle size of 10 to 2000 ⁇ m; A binder that is contained in a range of more than 2.0% by mass and 5.0% by mass or less in terms of solid content with respect to the granular flaky glass, and granulating the flaky glass; A granular flaky glass is provided.
  • the resin composition of the present invention contains polycarbonate and granular flaky glass.
  • the content of the binder in the granular flaky glass is adjusted to a specific range.
  • By attaching a specific amount of binder to the flaky glass it is considered that the hydroxyl groups and the like on the surface of the glass, which is the starting point for the decrease in the molecular weight of the polycarbonate, can be reduced. Therefore, if the resin composition of the present invention is used, a resin molded product having high strength and low shrinkage can be provided.
  • the granular flaky glass of the present invention contains flaky glass and a specific amount of binder attached to the flaky glass.
  • a specific amount of the binder By attaching a specific amount of the binder to the flaky glass, it is considered that the hydroxyl groups and the like on the surface of the glass, from which the molecular weight of the thermoplastic resin starts to decrease, can be reduced.
  • the granular flaky glass of the present embodiment comprises (I) a step of adding a binder to the flaky glass, stirring the mixture of the flaky glass and the binder, and (II) a flaky glass having the binder attached thereto. And a step of drying.
  • a plurality of flaky glasses are bonded to each other using a binder to obtain a granular flaky glass.
  • the flaky glass as the raw material of the granular flaky glass can be produced by a so-called blow method or a rotary method.
  • the glass manufacturing apparatus shown in FIG. 1 can be used.
  • the glass manufacturing apparatus includes a refractory kiln 12, a blow nozzle 15, and a press roll 17.
  • the glass substrate 11 melted in the refractory kiln 12 (melting tank) is inflated into a balloon shape by the gas fed into the blow nozzle 15 to become a hollow glass film 16.
  • the hollow glass film 16 is pulverized by the pressing roll 17 to obtain the flaky glass 1.
  • the thickness of the flaky glass 1 can be controlled by adjusting the tensile speed of the hollow glass film 16 and the flow rate of the gas fed from the blow nozzle 15.
  • the glass manufacturing apparatus shown in FIG. 2 can be used.
  • the glass manufacturing apparatus includes a rotating cup 22, a pair of annular plates 23, and an annular cyclone type collector 24.
  • the molten glass substrate 11 is poured into the rotating cup 22, flows out radially from the upper edge of the rotating cup 22 by centrifugal force, is sucked by the air flow between the annular plates 23, and the annular cyclone collector 24.
  • the glass While passing through the annular plate 23, the glass is cooled and solidified in the form of a thin film, and further crushed into small pieces, whereby the flaky glass 1 is obtained.
  • the thickness of the flaky glass 1 can be controlled by adjusting the interval between the annular plates 23, the speed of the air flow, and the like.
  • composition of the flaky glass a generally known glass composition can be used. Specifically, a glass with little alkali metal oxide such as E glass can be suitably used. A typical composition of E glass is shown below. The unit of the following composition is mass%.
  • a glass with less alkali metal oxide expressed as mass%, 59 ⁇ SiO 2 ⁇ 65, 8 ⁇ Al 2 O 3 ⁇ 15, 47 ⁇ (SiO 2 —Al 2 O 3 ) ⁇ 57, 1 ⁇ MgO. ⁇ 5, 20 ⁇ CaO ⁇ 30, 0 ⁇ (Li 2 O + Na 2 O + K 2 O) ⁇ 2, 0 ⁇ TiO 2 ⁇ 5, B 2 O 3 , F, ZnO, BaO, SrO, ZrO 2 Can be used.
  • the glass composition is disclosed by the present applicant in WO 2006/068255.
  • each content of B 2 O 3 , F, ZnO, BaO, SrO and ZrO 2 is less than 0.1% by mass (preferably less than 0.05% by mass, more preferably 0.03% by mass). Less).
  • the average thickness and average particle diameter of the flaky glass are not particularly limited. However, since the thin flake glass has a small bulk density, the volume per unit weight is large, and the effect of volume reduction obtained by using the granular flake glass is large. For this reason, using thin flaky glass as a raw material for granular flaky glass is effective in terms of workability and inventory.
  • the average thickness is preferably 0.1 ⁇ m or more.
  • the average particle size is preferably 10 to 2000 ⁇ m in order to more effectively realize the reinforcing effect and the reduction effect of the molding shrinkage rate.
  • the average aspect ratio is preferably 2000 or less because of dispersibility in the resin.
  • the “average thickness” means that a predetermined number (for example, 100 or more) of flake glass is extracted from a large number of flake glass, and the flake glass is thickened using a scanning electron microscope (SEM). This is a value obtained by measuring the thickness and dividing the total thickness by the number of sheets to be measured.
  • the “average particle size” is a particle size (D50) corresponding to a cumulative mass percentage of 50% in the particle size distribution measured based on the laser diffraction scattering method.
  • the “average aspect ratio” is a value obtained by dividing the average particle diameter by the average thickness.
  • the surface of the flaky glass may be covered with a metal and / or metal oxide thin film.
  • the flaky glass contains an alkali component
  • the elution of the alkali component from the flaky glass can be prevented by coating the surface of the flaky glass with a thin film.
  • it is possible to prevent disadvantages based on the elution of the alkali component for example, a decrease in the adhesive strength between the resin and the flaky glass, and the discoloration of the resin.
  • flaky glass whose surface is coated with a thin film often has high glitter. When such flaky glass is used as a raw material for granular flaky glass, the design of a resin molded product containing the granular flaky glass can be enhanced.
  • Granule flaky glass is produced by adding a binder to flaky glass, stirring and drying.
  • the specific method of adding, stirring and drying the binder is not particularly limited, but examples thereof will be described below.
  • a predetermined amount of a binder is added by spraying or the like while the flaky glass is flowed in a mixer, and mixed and stirred.
  • the flaky glass is dried while stirring in the mixer, or the flaky glass is taken out from the mixer and dried.
  • the mixer include a rotary disk mixer, a Henschel mixer equipped with a rotary blade in a mixing container, and the like.
  • granular flaky glass can be produced using a rolling granulation method as described in JP-A-2-124732. That is, flaky glass is put in a horizontal vibration granulator equipped with stirring blades, and a binder is sprayed on the flaky glass for granulation. Thereby, granular flaky glass is obtained.
  • granular flaky glass can be produced by applying known methods such as agitation granulation method, fluidized bed granulation method, spray granulation method and rotary granulation method.
  • the drying step is performed, for example, by heating the granular flaky glass to a temperature equal to or higher than the boiling point of the solvent for making the binder liquid. That is, the granular flaky glass is dried so that the solvent is sufficiently volatilized.
  • the solvent water and / or a volatile organic solvent can be used. Alcohol is mentioned as a volatile organic solvent.
  • the binder is not particularly limited, but preferably includes an adhesive component and a coupling agent component, and a lubricant component such as an oil agent and a surfactant can also be used.
  • the adhesive component is a component for granulating the flaky glass and increasing the affinity between the flaky glass and the molding resin.
  • the coupling agent component reacts with the surface of the flaky glass and is a component for increasing the affinity between the glass surface and the molding resin.
  • the adhesive component is not particularly limited, and organic and inorganic materials can be used.
  • organic adhesive component include methyl cellulose, carboxymethyl cellulose, starch, carboxymethyl starch, hydroxyethyl cellulose, hydroxypropyl cellulose, polyvinyl alcohol, acrylic resin, epoxy resin, phenol resin, vinyl acetate, and polyurethane resin.
  • inorganic adhesive component include water glass, colloidal silica, and colloidal alumina.
  • the coupling agent component is not particularly limited, and examples thereof include a silane coupling agent, a titanium coupling agent, an aluminum coupling agent, and a zirconia coupling agent, and a mixture thereof can also be used.
  • silane coupling agents include ⁇ -aminopropyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane, N- ⁇ -aminoethyl- ⁇ -aminopropyltrimethoxysilane, ⁇ -glycidoxypropyltrimethoxysilane, vinyltri Examples include ethoxysilane and ⁇ -methacryloxypropyltrimethoxysilane.
  • a liquid binder can be prepared by appropriately adding an adhesive component and a coupling agent component to a solvent at room temperature and atmospheric pressure and stirring until uniform.
  • the adhesion rate (attachment amount) of the binder in the granular flaky glass can be controlled by the concentration and amount of the binder added to or sprayed on the flaky glass. That is, a predetermined amount of binder solution is added or sprayed on a predetermined amount of flaky glass so that the solid content of the binder becomes a predetermined amount. Thereby, the granule flake shaped glass of a predetermined adhesion rate can be manufactured.
  • the granular flaky glass of the present embodiment includes flaky glass having an average thickness of 0.1 to 2.0 ⁇ m and an average particle diameter of 10 to 2000 ⁇ m, and a binder granulating the flaky glass. .
  • the binder is contained in the granular flake glass in a range of more than 2.0% by mass and 5.0% by mass or less in terms of solid content.
  • the adhesion rate of the binder is 2.0% by mass or less, the flake glass cannot be sufficiently covered with the binder due to the surface area of the flake glass, and the decrease in the molecular weight of the resin cannot be sufficiently suppressed. It may cause a decrease in strength of the product.
  • the adhesion rate of the binder is larger than 5.0% by mass, problems such as generation of gas during extrusion molding and contamination of the mold or discoloration of the resin molded product are likely to occur.
  • the resin composition of the present embodiment can be obtained by blending the granular flaky glass as described above with a resin.
  • a thermoplastic resin can be used as the resin.
  • the thermoplastic resin is not particularly limited, and polyvinyl chloride, polypropylene, polyethylene, polystyrene, polyester, polyamide, polycarbonate, polybutylene, polybutylene terephthalate or a copolymer thereof, polyphenylene sulfide, polyphenylene ether, polyether ether ketone, Examples thereof include liquid crystal polymers (type I, type II and type III).
  • the effect which suppresses the fall of molecular weight is acquired notably.
  • the content of granular flaky glass in the resin composition is preferably 5 to 70% by mass. By setting it as 5 mass% or more, the function as a reinforcing material of granule flake shaped glass can fully be exhibited. On the other hand, the granular flaky glass can be uniformly dispersed in the resin composition by adjusting the content to 70% by weight or less. In order to keep the molding shrinkage rate lower, the content of the granular flaky glass is more preferably 30% by mass or more and 60% by mass or less.
  • the resin composition may contain a reinforcing material other than flaky glass such as glass fiber depending on its application.
  • a reinforcing material other than flaky glass such as glass fiber depending on its application.
  • glass fibers having the same amount as that of granular flaky glass may be mixed.
  • the resin molded product produced using the resin composition of the present embodiment has high tensile strength and bending strength due to the reinforcing effect of granular flaky glass. Moreover, since the resin composition of this embodiment has a low mold shrinkage rate, a resin molded product produced using the resin composition is excellent in dimensional stability. Moreover, the flaky glass contained in the resin composition of this embodiment has an average thickness smaller than the average thickness of the flaky glass contained in the conventional resin composition. Therefore, according to the resin composition of this embodiment, a molded product having a small surface roughness and a smooth surface can be obtained.
  • Example 1 First, using glass E having the composition shown in Table 1, flaky glass was produced by the blow method described with reference to FIG. Specifically, E glass was put into a melting tank heated to 1200 ° C. or higher and dissolved. A thin glass was produced while blowing air from a nozzle, and this thin glass was continuously drawn out by a roller. The amount of air blown and the number of roller rotations were adjusted to obtain a glass having an average thickness of 0.7 ⁇ m. Thereafter, pulverization and classification were performed to obtain a flaky glass having an average particle size of 160 ⁇ m. After pulverizing the flake glass, the flake glass having a uniform size can be obtained by classifying the flake glass using a sieve having an appropriate opening.
  • the adhesion rate of the binder in the obtained granular flaky glass was examined by an ignition loss method. Specifically, an appropriate amount of granular flaky glass was dried at 110 ° C. and then heated in an atmosphere of 625 ° C. to remove the binder from the surface of the flaky glass. From the difference between the mass of the granular flaky glass before heating and the mass of the flaky glass after heating, the adhesion rate of the binder in the granular flaky glass was calculated. The results are shown in Table 2.
  • the characteristics of resin molded products were examined.
  • the maximum tensile strength, tensile modulus, and tensile strain were measured according to JIS K 7113.
  • the maximum bending strength, bending elastic modulus and bending strain were measured according to JIS K7171.
  • the Izod impact strength was measured according to JIS K-7111-1.
  • MFR mass flow rate
  • MFR is known as a parameter that represents a measure of the molecular weight of a resin.
  • the MFR is expressed by the amount of resin that flows out from the orifice in 10 minutes while holding a molten resin in a cylinder and applying an appropriate load to the resin.
  • MFR is an indicator of the viscosity of the molten resin, but is also related to molecular weight. That is, as the molecular weight of the resin increases, the MFR decreases, and as the molecular weight decreases, the MFR increases. As the molecular weight of the resin increases, the strength of the molded product tends to increase.
  • Examples 2 to 4, Comparative Examples 1 to 4 By adjusting the content of solids (binder component and coupling agent component) in the binder, granule flake glasses of Examples 2 to 4 and Comparative Examples 1 to 4 were obtained. However, the ratio of the adhesive component to the coupling agent component in the binders used in Examples 2 to 4 and Comparative Examples 1 to 4 was the same as that of the binder used in Example 1. The adhesion rate of the binder was measured by the same method as in Example 1. Moreover, the resin molded product was produced by the same method as Example 1, and those various characteristics were measured. The results are shown in Tables 2 and 3.
  • the MFRs of Examples 1 to 4 were relatively low, and the MFRs of Comparative Examples 1 to 4 were relatively high.
  • the content of granular flaky glass in the resin molded product is constant (30% by mass) in all Examples and Comparative Examples. Therefore, it can be said that MFR correlates with the adhesion rate of the binder in the granular flaky glass.
  • the MFR was substantially constant despite the difference in the adhesion rate of the binder.
  • Comparative Examples 1 to 3 the MFR also decreased as the adhesion rate of the binder increased. Further, the MFR showed a substantially constant value in Examples 1 to 4, and then began to increase again in Comparative Example 4.
  • the granular flaky glass of the present invention can be applied to various applications because it can effectively reinforce a resin molded product while suppressing a decrease in the molecular weight of the resin.
  • the resin composition containing granular flaky glass and polycarbonate of the present invention is suitably used in the field of automobiles, the field of electronic parts, and the like.

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
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  • Manufacturing & Machinery (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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Abstract

La composition de résine selon la présente invention comprend un polycarbonate et un verre feuilleté granulaire. Le verre feuilleté granulaire comprend un verre feuilleté et un liant qui rend le verre feuilleté granulaire. Le verre feuilleté a une épaisseur moyenne de 0,1 à 2,0 µm et un diamètre moyen de particules de 10 à 2000 µm. Le liant est contenu dans le verre feuilleté granulaire en une quantité supérieure à 2,0 % en poids et inférieure ou égale à 5,0 % en poids en termes de teneur solide en poids.
PCT/JP2011/004737 2010-08-26 2011-08-25 Composition de résine et verre feuilleté granulaire WO2012026127A1 (fr)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015119302A1 (fr) * 2014-02-10 2015-08-13 日本碍子株式会社 Ensemble de charges poreuses en forme de plaque, son procédé de production, et film isolant contenant l'ensemble de charges poreuses en forme de plaque
JP6054587B1 (ja) * 2015-07-31 2016-12-27 日本板硝子株式会社 フレーク状ガラス及び樹脂組成物
WO2017141792A1 (fr) * 2016-02-18 2017-08-24 日本板硝子株式会社 Verre en paillettes et composition de résine
WO2018151153A1 (fr) * 2017-02-20 2018-08-23 日本板硝子株式会社 Matériau de renfort et article moulé en résine

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63201041A (ja) * 1987-02-16 1988-08-19 Nippon Glass Fiber Co Ltd 熱可塑性樹脂又は熱硬化性樹脂成形用の補強材
JPS63225554A (ja) * 1987-03-12 1988-09-20 Nippon Glass Fiber Co Ltd 顆粒状のフレ−ク状ガラス
JPH069791A (ja) * 1993-03-04 1994-01-18 Nippon Glass Fiber Co Ltd 樹脂組成物の成形体

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101687692B (zh) * 2007-06-18 2012-11-14 日本板硝子株式会社 玻璃组合物

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63201041A (ja) * 1987-02-16 1988-08-19 Nippon Glass Fiber Co Ltd 熱可塑性樹脂又は熱硬化性樹脂成形用の補強材
JPS63225554A (ja) * 1987-03-12 1988-09-20 Nippon Glass Fiber Co Ltd 顆粒状のフレ−ク状ガラス
JPH069791A (ja) * 1993-03-04 1994-01-18 Nippon Glass Fiber Co Ltd 樹脂組成物の成形体

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015119302A1 (fr) * 2014-02-10 2015-08-13 日本碍子株式会社 Ensemble de charges poreuses en forme de plaque, son procédé de production, et film isolant contenant l'ensemble de charges poreuses en forme de plaque
JPWO2015119302A1 (ja) * 2014-02-10 2017-03-30 日本碍子株式会社 多孔質板状フィラー集合体及びその製造方法、並びに多孔質板状フィラー集合体を含む断熱膜
US10392310B2 (en) 2014-02-10 2019-08-27 Ngk Insulators, Ltd. Porous plate-shaped filler aggregate, producing method therefor, and heat-insulation film containing porous plate-shaped filler aggregate
JP6054587B1 (ja) * 2015-07-31 2016-12-27 日本板硝子株式会社 フレーク状ガラス及び樹脂組成物
WO2017141792A1 (fr) * 2016-02-18 2017-08-24 日本板硝子株式会社 Verre en paillettes et composition de résine
US11008459B2 (en) 2016-02-18 2021-05-18 Nippon Sheet Glass Company, Limited Glass flakes and resin composition
WO2018151153A1 (fr) * 2017-02-20 2018-08-23 日本板硝子株式会社 Matériau de renfort et article moulé en résine

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