WO2017221637A1 - Procédé de fabrication de fibres de verre - Google Patents

Procédé de fabrication de fibres de verre Download PDF

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Publication number
WO2017221637A1
WO2017221637A1 PCT/JP2017/019826 JP2017019826W WO2017221637A1 WO 2017221637 A1 WO2017221637 A1 WO 2017221637A1 JP 2017019826 W JP2017019826 W JP 2017019826W WO 2017221637 A1 WO2017221637 A1 WO 2017221637A1
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WO
WIPO (PCT)
Prior art keywords
glass
raw material
cullet
temperature
content
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2017/019826
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English (en)
Japanese (ja)
Inventor
拡志 澤里
長壽　研
稔 松本
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Nippon Electric Glass Co Ltd
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Nippon Electric Glass Co Ltd
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Filing date
Publication date
Application filed by Nippon Electric Glass Co Ltd filed Critical Nippon Electric Glass Co Ltd
Publication of WO2017221637A1 publication Critical patent/WO2017221637A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C03B37/01—Manufacture of glass fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/02—Pretreated ingredients
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C13/00—Fibre or filament compositions

Definitions

  • the present invention relates to a method for producing a glass fiber used as a reinforcing material for a composite material.
  • Glass fibers also called glass fibers used for composite materials with resins are generally manufactured as follows.
  • a raw material mixture (called a raw material batch) prepared and mixed to have the desired composition is put into a melting furnace, and glass is heated by burner combustion of heavy oil or gas, or by direct energization, and the surface of the batch Then, the melting is advanced to gradually make a glass melt.
  • the molten glass is supplied to a molding apparatus called a bushing (also called a spinning furnace).
  • the bushing is a device having a substantially rectangular appearance with a large number of nozzle parts (or orifice parts), and the temperature is controlled so that the viscosity of the molten glass at the tip part of the bushing nozzle is approximately 10 3 dPa ⁇ s.
  • the temperature at which the viscosity of the molten glass becomes 10 3 dPa ⁇ s is called the molding temperature T X, and the smaller the temperature difference ⁇ T XL between T X and the liquidus temperature TL , the more the loss in the glass melt at the bushing nozzle tip. Permeability is likely to occur, and thread breakage is likely to occur. For this reason, it is preferable that ⁇ T XL is larger.
  • glass fiber is produced by spinning molten glass. More specifically, molten glass supplied to the bushing is continuously drawn out from the tip of the bushing nozzle and rapidly cooled to form a filament shape, and a predetermined number of the glass melts to obtain glass fibers.
  • the glass fibers produced in this way are called long fibers and are used for fiber reinforced plastics (Fiber® Reinforced Plastics, FRP), which are structural members such as printed wiring boards, cars and airplanes.
  • FRP fiber reinforced Plastics
  • E glass a low alkali glass fiber
  • FRP printed wiring boards
  • E glass although containing B (boron) as a glass component, which is capable of lowering the melting temperature and forming temperature T X of the glass at the same time enhances the network strength of the glass by introducing the B
  • the liquidus temperature TL can also be lowered.
  • the raw material containing B is very expensive.
  • B is heated together with other powdery raw materials in a melting furnace, a part thereof becomes B 2 O 3 and evaporates. B lost by evaporation not only leads to a further increase in production costs, but also tends to cause environmental problems when released into the atmosphere. For this reason, the glass fiber composition which hardly contains B is proposed (patent document 2).
  • An object of the present invention is to provide a glass fiber production method that can be produced at low cost with a small amount of B released into the atmosphere, and a glass fiber produced by this production method.
  • the present inventors have found that the above object can be achieved by using glass cullet containing B as a glass composition as a main B supply source, and propose the present invention.
  • the glass fiber manufacturing method of the present invention is a method for manufacturing a glass fiber in which a raw material batch composed of a mixture of a glass raw material and a glass cullet is melted in a glass melting furnace, and the molten glass is continuously drawn from the bushing and formed into a fiber shape.
  • the method is characterized in that a raw material batch containing more than 25 mass% of B (boron) -containing glass cullet is used as the glass cullet.
  • the “glass cullet” refers to glass that does not become a product generated in the glass manufacturing process, and waste glass such as recycled glass collected from home appliances.
  • B (boron) -containing glass cullet refers to a glass cullet made of glass containing a B (boron) component in its composition.
  • the method of the present invention adopting the above configuration can reduce the raw material cost since the glass cullet available at low cost is used as the B (boron) supply source. Further, since there is no need to change the glass fiber composition, it is possible to avoid early deterioration of the bushing due to an increase in spinning temperature and deterioration of spinnability. Moreover, since the amount of the B raw material used is reduced and the amount of evaporation of B 2 O 3 can be effectively reduced, the burden on the environment can be reduced.
  • B raw material refers to a natural raw material or chemical raw material containing B (boron).
  • the raw material batch it is preferable to prepare the raw material batch so that 20% by mass or more of the B 2 O 3 content of the target glass fiber composition is supplied from the B-containing glass cullet.
  • the amount of the raw material B can be greatly reduced.
  • the B-containing glass cullet is preferably made of a glass having a glass composition of 5% by mass or more of B 2 O 3 .
  • glass fibers can be produced with a small amount of glass cullet, so the degree of freedom in preparing the raw material batch is increased.
  • the B-containing glass cullet is preferably made of glass having a glass composition of Li 2 O + Na 2 O + K 2 O 0-2%.
  • Li 2 O + Na 2 O + K 2 O means the total content of Li 2 O, Na 2 O and K 2 O.
  • the raw material batch it is preferable to prepare the raw material batch so that the glass contains 3 to 6.3% by mass of B 2 O 3 .
  • the glass fiber of the present invention is manufactured by the above method.
  • the production method of the present invention includes a step of preparing a raw material batch, a step of melting the raw material batch to form molten glass, and a step of forming the molten glass into a fiber shape.
  • B-containing glass cullet is used as one of the materials constituting the raw material batch.
  • the glass cullet content in the raw material batch is preferably more than 25%, 26% or more, 27% or more, particularly 30 to 50%. If the ratio of glass cullet is too small, the amount of B supply decreases, making it difficult to enjoy the effects of the present invention. Although it is desirable to supplement all necessary B from the glass cullet, if this is difficult, the shortage of the B supply amount may be supplemented with natural raw materials or chemical raw materials. Or a gas containing B 2 O 3 was evaporated in a glass melting process and solidified by cooling, it may be used powdery material containing the recovered B (B harvest).
  • the present invention 20% or more, 35% or more, 40% or more, 45% or more, particularly 50% or more of the B 2 O 3 content of the target glass fiber composition is supplied from the B-containing glass cullet. It is preferable to prepare the raw material batch. When this ratio is too low, a large amount of B raw material must be used, and it becomes difficult to enjoy the effects of the present invention.
  • the B-containing glass cullet it is preferable to use a glass cullet containing B 2 O 3 in a glass composition of 3% or more, 4% or more, 5% or more, 6% or more, 8% or more, particularly 10% or more.
  • a glass cullet containing B 2 O 3 in a glass composition of 3% or more, 4% or more, 5% or more, 6% or more, 8% or more, particularly 10% or more.
  • the B-containing glass cullet it is preferable to use a glass cullet having a Li 2 O + Na 2 O + K 2 O content of 0 to 2%, 0 to 1%, particularly 0 to 0.5%.
  • Li 2 O + Na 2 O + K 2 O content is too much, an alkali elution amount of the obtained glass fiber is increased.
  • the adhesive strength at the resin-glass interface decreases, and the mechanical strength tends to decrease.
  • the B-containing glass cullet is specifically composed of SiO 2 50 to 70%, Al 2 O 3 10 to 25%, B 2 O 3 3 to 20%, MgO 0 to 10%, CaO 1 to 20%, SrO 0. Glass containing ⁇ 15%, BaO 0 ⁇ 15%, Li 2 O + Na 2 O + K 2 O 0 ⁇ 2%, especially SiO 2 55 ⁇ 65%, Al 2 O 3 15 ⁇ 20%, B 2 O 3 5 ⁇ 12% MgO 0.1-5%, CaO 3-10%, SrO 0.1-10%, BaO 0.1-10%, Li 2 O + Na 2 O + K 2 O 0.01-1% Is preferred.
  • the glass cullet is preferably made of glass having a composition different from that of the glass fiber to be produced, and is particularly preferably made of glass having a higher B 2 O 3 content than the glass fiber to be produced. If it does in this way, it will become possible to introduce B into glass efficiently.
  • the glass raw material batch prepared as described above is put into a glass melting furnace, vitrified, melted and homogenized.
  • the glass is preferably melted at about 1300 to 1600 ° C.
  • a suitable composition of the target glass fiber will be described later.
  • molten glass that has been uniformly melted is supplied to the bushing.
  • the molten glass supplied to the bushing is continuously drawn out in filament form from a number of bushing nozzles provided on the bottom surface.
  • Various processing agents are applied to the monofilaments drawn in this way, and glass fibers are obtained by focusing each monofilament.
  • the temperature at which the glass fiber is spun is preferably 1100 to 1300 ° C.
  • the glass fiber molded in this way is processed into chopped strands, yarns, rovings, etc. and used for various purposes.
  • the glass fiber produced by the method of the present invention is a glass containing 3 to 6.3% B 2 O 3 as a composition, particularly SiO 2 50 to 60%, Al 2 O 3 10 to 18%, B 2 O 3 3 A glass containing ⁇ 6.3%, MgO 0 to 5%, CaO 18 to 28%, Li 2 O + Na 2 O + K 2 O 0 to 2% is preferable.
  • B 2 O 3 as a composition, particularly SiO 2 50 to 60%, Al 2 O 3 10 to 18%, B 2 O 3 3
  • a glass containing ⁇ 6.3%, MgO 0 to 5%, CaO 18 to 28%, Li 2 O + Na 2 O + K 2 O 0 to 2% is preferable. The reason why the content of each component is limited as described above will be described below.
  • SiO 2 is one of the elements constituting the glass network.
  • the content is preferably 50 to 60%, 50 to 58%, particularly preferably 52 to 56%. If the SiO 2 content is too small, the structural strength of the glass is remarkably deteriorated and the mechanical strength required for the composite member using glass fibers cannot be satisfied. On the other hand, when the SiO 2 content is too large, the high temperature viscosity increases. As a result, if an attempt is made to produce such a glass composition to be homogeneous with high efficiency by a melting method, the energy required for melting the glass increases and the production cost increases. In addition, when melting at a low temperature, a process such as pulverizing the raw material to make it fine is necessary, which also increases the manufacturing cost.
  • Al 2 O 3 is a component that suppresses crystal crystallization and phase separation in molten glass.
  • the content of Al 2 O 3 is preferably 10 to 18%, 11 to 16%, particularly preferably 12 to 15%. If the content of Al 2 O 3 is too small, the liquidus temperature rises and ⁇ T XL becomes small, which is not preferable. On the other hand, the Al 2 O 3 content is too large, the high temperature viscosity of the glass is increased, the melting property tends to deteriorate.
  • B 2 O 3 is a glass network structure similarly to SiO 2, is a component that forms the skeleton, rather than increasing the high temperature viscosity of the molten glass as SiO 2, there is work to lower the high temperature viscosity rather .
  • the content of B 2 O 3 is preferably 3 to 6.3%, 4 to 6%, and particularly preferably 4.5 to 5.5%.
  • B 2 content of O 3 is too small, it increased high temperature viscosity, the melting property tends to deteriorate.
  • foreign glass such as scum is likely to be generated in the melting process.
  • MgO is a component that acts as a flux that makes it easy to melt glass raw materials, and at the same time is very effective in reducing high-temperature viscosity. It is a useful ingredient.
  • the MgO content is preferably 0 to 5%, 1 to 4%, particularly preferably 1.5 to 3%. If the MgO content is too large, the phase separation of the molten glass increases and ⁇ T XL decreases, which is not preferable.
  • CaO is a component that lowers the high temperature viscosity together with MgO.
  • the CaO content is preferably 18 to 28%, 20 to 25%, particularly preferably 22 to 25%.
  • the content of CaO is too large, the phase separation of the molten glass is increased, and ⁇ T XL is decreased, which is not preferable.
  • Li 2 O, Na 2 O and K 2 O which are alkali metal oxide components facilitate the production of a glass melt when heated in a mixed state of a plurality of glass raw materials to form a glass melt. It acts as a so-called flux. It also has the function of reducing the high temperature viscosity.
  • the total amount of Li 2 O, Na 2 O and K 2 O (content of Li 2 O + Na 2 O + K 2 O) is preferably 0 to 2%, 0 to 1%, particularly preferably 0 to 0.8%. .
  • P 2 O 5 is an ingredient that has the effect of preventing the formation of fine crystal nuclei in the molten glass and can lower the liquidus temperature. However, if added in a large amount, the liquidus temperature is increased.
  • the content of P 2 O 5 is preferably 0.1 to 2%, more preferably 0.1 to 1%, still more preferably 0.1 to 0.5%. If the P 2 O 5 content is too small, the above effect cannot be obtained.
  • SrO and BaO may be contained.
  • the SrO content is preferably 0 to 2%, more preferably 0.1 to 2%, and still more preferably 0.1 to 1.5%.
  • the content of BaO is preferably 0 to 2%, more preferably 0.05 to 1%, and still more preferably 0.05% to 0.5%. If the content of SrO or BaO is too large, the phase separation of the molten glass is increased, and ⁇ T XL is decreased, which is not preferable.
  • One or more clarifiers may be included to reduce foam in the product glass.
  • the clarifier for example, SO 3 , Cl, SnO 2 , Sb 2 O 3 , As 2 O 3 and the like can be used. In this case, the total amount of standard fining agents added is within 0.5%.
  • 3 components each of Cr 2 O 3 , PbO, La 2 O 3 , WO 3 , Nb 2 O 5 , Y 2 O 3 , F, etc. % May be contained.
  • H 2 , CO 2 , CO, H 2 O, He, Ne, Ar, and N 2 may be contained up to 0.1% as impurities.
  • Pt, Rh, and Au may be contained up to 0.05% or less as impurities.
  • the glass fiber produced by the method of the present invention preferably has a melting temperature T melt (temperature at which the viscosity of the glass becomes 10 2.0 dPa ⁇ s) is 1400 ° C. or lower, 1380 ° C. or lower, particularly 1360 ° C. or lower. If the melting temperature T melt is too high, the glass must be melted at a high temperature, which increases the consumption of heavy oil, gas, and electricity, leading to an increase in manufacturing costs.
  • T melt temperature at which the viscosity of the glass becomes 10 2.0 dPa ⁇ s
  • the molding temperature T X (the temperature at which the glass has a viscosity of 10 3.0 dPa ⁇ s) is preferably 1210 ° C. or less, particularly preferably 1190 ° C. or less.
  • T X is too high, since the glass fiber must be spun at a high temperature occurs, bushing life tends shortened deformed, leading to increase in manufacturing cost.
  • melting temperature T melt and shaping temperature T X can be measured using a platinum ball pulling method.
  • the liquidus temperature TL is preferably 1080 ° C. or lower, particularly preferably 1060 ° C. or lower.
  • ⁇ T LX becomes small and spinnability deteriorates. That is, devitrified substances are easily generated in the glass melt, and yarn breakage is likely to occur.
  • the liquid phase temperature TL is measured by filling a crushed sample in a platinum boat and placing it in an electric furnace having a temperature gradient for 16 hours. Can be determined by the method of
  • the temperature difference ⁇ T XL between the molding temperature T X and the liquidus temperature TL is preferably 100 ° C. or higher, 110 ° C. or higher, and particularly preferably 120 ° C. or higher. If ⁇ T XL is too small, spinnability deteriorates.
  • Table 1 shows examples (sample Nos. 1 to 5) and comparative examples (sample No. 6) of the present invention.
  • Table 2 shows the composition of the B-containing glass cullet (glass cullet ad).
  • the sample No. In Nos. 1 to 5 the molding temperature T X was 1183 ° C. or lower, and ⁇ T XL was 102 ° C. or higher.
  • sample No. which is a comparative example. 6 was as small as 80 ° C.
  • the molding temperature T X (the temperature at which the viscosity of the glass becomes 10 3.0 dPa ⁇ s) was performed as follows. The massive glass sample was crushed to an appropriate size, and put into an alumina crucible so that bubbles were not caught as much as possible. Subsequently, the alumina crucible is heated to bring the sample into a molten state, and the measured value of the viscosity of the glass at a plurality of temperatures is obtained by a platinum ball pulling method, and the viscosity curve is created by calculating the constant of the Vogel-Fulcher equation. The glass was measured by a method of calculating the temperature at which the viscosity of the glass becomes 10 3.0 dPa ⁇ s and the temperature at which the viscosity becomes 10 2.0 dPa ⁇ s.
  • the liquid phase temperature TL is measured by filling a crushed sample in a platinum boat of about 120 ⁇ 20 ⁇ 10 mm and placing it in an electric furnace having a linear temperature gradient for 16 hours. Calculated from the temperature gradient graph of the electric furnace, this temperature was defined as the liquidus temperature TL .
  • the massive glass sample was put into a noble metal pot equipped with a bushing, and remelted by energization heating. Thereafter, various treatment agents were applied to the monofilament continuously drawn out in a filament form from the bushing nozzle, and the glass fibers were obtained by focusing each monofilament.
  • various treatment agents were applied to the monofilament continuously drawn out in a filament form from the bushing nozzle, and the glass fibers were obtained by focusing each monofilament.
  • a method of once producing a lump glass sample and remelting and spinning it was adopted.
  • the molten glass was directly supplied to the bushing for spinning. It is preferable to adopt the method to do.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Glass Compositions (AREA)

Abstract

L'invention fournit un procédé de fabrication de fibres de verre qui permet une fabrication bon marché et avec une faible quantité de B émis dans l'atmosphère. Plus précisément, l'invention concerne un procédé de fabrication de fibres de verre selon lequel un lot de matières premières constitué d'un mélange de matière première de verre et de calcins de verre est fondu dans un four de fusion du verre, et un verre fondu est étiré en continu à partir d'une filière et moulé sous forme de fibres. Ce procédé est caractéristique en ce qu'il met en œuvre le lot de matières premières, lequel comprend en tant que calcins de verre plus de 25% en masse de calcins de verre à teneur en B (bore).
PCT/JP2017/019826 2016-06-23 2017-05-29 Procédé de fabrication de fibres de verre Ceased WO2017221637A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2016-124756 2016-06-23
JP2016124756A JP2017226582A (ja) 2016-06-23 2016-06-23 ガラス繊維の製造方法

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2020070218A (ja) * 2018-11-01 2020-05-07 日本電気硝子株式会社 ガラスの製造方法及びガラス用混合原料
CN115335557A (zh) * 2020-03-24 2022-11-11 新日本繊维株式会社 纤维、纤维制造方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7900738B2 (ja) * 2020-06-25 2026-08-05 日本電気硝子株式会社 低アルカリガラス板の製造方法及び低アルカリガラス板

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0337136A (ja) * 1989-06-30 1991-02-18 Nippon Electric Glass Co Ltd 長繊維用ガラス組成物
JPH09263422A (ja) * 1996-03-28 1997-10-07 Nitto Boseki Co Ltd 防かび性ガラス繊維
JPH1179780A (ja) * 1997-08-28 1999-03-23 Nitto Boseki Co Ltd 耐水性高ホウ酸ガラス繊維の製造方法および耐水性高ホウ酸ガラス繊維
JPH11228164A (ja) * 1998-02-12 1999-08-24 Asahi Fiber Glass Co Ltd 有機物で被覆されている繊維状ガラス物の処理方法
JP2003267753A (ja) * 2000-10-11 2003-09-25 Paramount Glass Kogyo Kk 無機質繊維製造用硝子組成物及びその成型物
JP2007217280A (ja) * 2007-04-27 2007-08-30 Nippon Sheet Glass Co Ltd カレットを原料としたガラス短繊維の製造方法
JP2011011969A (ja) * 2009-06-04 2011-01-20 Nippon Electric Glass Co Ltd ガラス繊維製造方法及びガラス繊維

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0337136A (ja) * 1989-06-30 1991-02-18 Nippon Electric Glass Co Ltd 長繊維用ガラス組成物
JPH09263422A (ja) * 1996-03-28 1997-10-07 Nitto Boseki Co Ltd 防かび性ガラス繊維
JPH1179780A (ja) * 1997-08-28 1999-03-23 Nitto Boseki Co Ltd 耐水性高ホウ酸ガラス繊維の製造方法および耐水性高ホウ酸ガラス繊維
JPH11228164A (ja) * 1998-02-12 1999-08-24 Asahi Fiber Glass Co Ltd 有機物で被覆されている繊維状ガラス物の処理方法
JP2003267753A (ja) * 2000-10-11 2003-09-25 Paramount Glass Kogyo Kk 無機質繊維製造用硝子組成物及びその成型物
JP2007217280A (ja) * 2007-04-27 2007-08-30 Nippon Sheet Glass Co Ltd カレットを原料としたガラス短繊維の製造方法
JP2011011969A (ja) * 2009-06-04 2011-01-20 Nippon Electric Glass Co Ltd ガラス繊維製造方法及びガラス繊維

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2020070218A (ja) * 2018-11-01 2020-05-07 日本電気硝子株式会社 ガラスの製造方法及びガラス用混合原料
CN115335557A (zh) * 2020-03-24 2022-11-11 新日本繊维株式会社 纤维、纤维制造方法

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