WO2014171561A1 - Composition de production de fibre de verre et fibre de verre biosoluble produite à partir de celle-ci - Google Patents

Composition de production de fibre de verre et fibre de verre biosoluble produite à partir de celle-ci Download PDF

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Publication number
WO2014171561A1
WO2014171561A1 PCT/KR2013/003160 KR2013003160W WO2014171561A1 WO 2014171561 A1 WO2014171561 A1 WO 2014171561A1 KR 2013003160 W KR2013003160 W KR 2013003160W WO 2014171561 A1 WO2014171561 A1 WO 2014171561A1
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WO
WIPO (PCT)
Prior art keywords
composition
glass fiber
fiber
weight
glass
Prior art date
Application number
PCT/KR2013/003160
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English (en)
Korean (ko)
Inventor
우봉기
이병원
이남수
허균용
정원식
주석재
강성호
Original Assignee
주식회사 케이씨씨
Priority date (The priority date 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 date listed.)
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Application filed by 주식회사 케이씨씨 filed Critical 주식회사 케이씨씨
Priority to PCT/KR2013/003160 priority Critical patent/WO2014171561A1/fr
Publication of WO2014171561A1 publication Critical patent/WO2014171561A1/fr

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Classifications

    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
    • 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
    • C03C13/06—Mineral fibres, e.g. slag wool, mineral wool, rock wool
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • 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
    • C03C2213/00—Glass fibres or filaments
    • C03C2213/02—Biodegradable glass fibres

Definitions

  • the present invention relates to a composition for producing glass fibers and a biosoluble glass fibers prepared therefrom, and more particularly, SiO 2 , Al 2 O 3 , CaO, MgO, Na 2 O, K 2 O, B 2 O 3 and P
  • a glass fiber composition and a bio-soluble glass prepared therefrom which makes it possible to easily produce a glass fiber having excellent biodegradability, water resistance, processability, etc. by a conventional rotary process. It is about a fiber.
  • Glass fiber is an amorphous artificial mineral inorganic fiber manufactured by melting raw materials at high temperature of 1400 °C or higher and processing them into 3 ⁇ 10 ⁇ m thick fibrous material. It is used for thermal insulation, heat insulation, cold storage, sound absorption, sound insulation, and many other uses. to be.
  • glass fiber insulation is prepared by combining a mixed soda lime alumina borosilicate glass fiber with a binder.
  • a binder a phenol-formaldehyde resin or a urea formaldehyde resin is usually used.
  • Glass fibers can be produced using a high speed centrifugal method, an example of which is a rotary process that produces fibers from a rotating device, commonly called a spinner.
  • the liquidus temperature of the glass fiber is 100 ° C. above the fiber draw viscosity temperature (also called the fiberization working temperature) (log ⁇ 3) to prevent the glass fiber from crystallizing in the spinner during de-emulsification. It is preferable that it is lower than the above.
  • glass fiber is related to human diseases, but if it is broken down and accumulated in the lungs by breathing as fine fibers, it may cause harm to the human body. At the same time, it is possible to minimize the possibility of fiberization, and research on the glass fiber composition having sufficient durability and thermal insulation during use is actively underway (for example, Korean Patent Publication No. 2011-0097010).
  • KI [Na 2 O + K 2 O + CaO + MgO + B 2 O 3 + BaO] content-2 ⁇ Al 2 O 3 content
  • the content of each oxide here is expressed in weight percent of the material in the glass composition.
  • the KI value can be increased by increasing the content of Na 2 O, K 2 O, CaO, MgO, B 2 O 3 , BaO or reducing the content of Al 2 O 3 in the composition.
  • this method has advantages in the manufacturing process due to the reduction of the melting point of the glass and the jeomseom temperature, but also has the adverse effect such as lowered heat resistance, water resistance, devitrification phenomenon during the jeseomyeon, increase in manufacturing raw material cost, and may be difficult or impossible to fiberize Can be generated.
  • the present invention has been made to solve the above problems of the prior art, it is possible to manufacture a glass fiber with improved biodegradability greatly improved without the heat resistance, water resistance, heat insulation, while using a relatively inexpensive raw material, glass fiber It is a technical problem to provide a composition for preparation and a biosoluble glass fiber prepared therefrom.
  • the present invention to achieve the above technical problem, SiO 2 62-65 wt%, Al 2 O 3 0.2-2 wt%, CaO 6.5-8.5 wt%, MgO 2.5-4.5 wt%, Na 2 O + K 2 O 15.5-18.7 weight%, B 2 O 3 4-7 wt% and P 2 O 5 It provides the composition for glass fiber manufacture containing 0.2-2 weight%.
  • the KI index of the composition for producing glass fibers is less than 40.
  • CaO / MgO in the composition for producing glass fibers is 1.6 to 2.5, MgO + CaO is 9.2 to 12.5% by weight.
  • B 2 O 3 / P 2 O 5 in the composition for producing glass fibers is 3-7, and B 2 O 3 + P 2 O 5 is 5.5-8.6 wt%.
  • biosoluble glass fiber which is produced from the composition for producing glass fibers of the present invention.
  • an insulation product comprising the biosoluble glass fibers of the invention.
  • a glass fiber having improved biodegradability can be manufactured by a conventional rotary process without using heat in a relatively low cost and without deteriorating heat resistance, water resistance, and thermal insulation, and can save energy required for melting and fiberizing fiber production.
  • SiO 2 serves as a network former forming the basic structure of the glass.
  • Glass fiber-producing composition of the present invention is a SiO 2 containing 62-65% by weight, and more preferably contains 63.5 to 64.5% by weight. If the content of SiO 2 in the composition is less than 62% by weight, the mechanical properties such as heat resistance and water resistance of the produced fiber are lowered, and the raw material cost is increased due to the increase of alkali earth metal oxide or alkali metal oxide. On the contrary, if the content exceeds 65% by weight, the melting temperature and the fiberization working temperature of the molten composition are increased, which makes it difficult to fiberize and there is a problem in that the diameter of the manufactured fiber is increased.
  • Al 2 O 3 is an intermediate oxide to increase the viscosity of the glass melt near the liquid line to control the crystallization of the glass and improve the water resistance of the fiber.
  • Glass fiber-producing composition of the present invention is an Al 2 O 3 containing 0.2 to 2% by weight, more preferably 1 to 2% by weight. When the Al 2 O 3 content in the composition is less than 0.2% by weight, the effect of adjusting the viscosity of the composition and the water resistance of the glass fiber may be lowered, and when it exceeds 2% by weight, the biodegradability may be lowered.
  • CaO and MgO increases the biodegradability of the glass fiber prepared as a modifier oxide (Modifier oxide) and serves to help the fiberization by reducing the viscosity of the glass melt. It also has the effect of improving the chemical durability lowered by the introduction of alkali metal oxides. MgO also reduces the temperature at which crystallization occurs and contributes more to biodegradability than CaO.
  • the composition for producing glass fibers of the present invention contains 6.5 to 8.5 wt% CaO, 2.5 to 4.5 wt% MgO, more preferably 7.0 to 7.5 wt% CaO, 3.5 to 4.0 wt% MgO.
  • the content of CaO and MgO in the composition is less than the above-mentioned level, there is a problem that the melting temperature is increased to increase the heat consumption required for melting, and if it exceeds this, there is a problem that the possibility of crystallization during fiberization increases.
  • MgO + CaO is preferably 9.2 to 12.5% by weight, more preferably 10.5 to 11.5% by weight. If the total amount of MgO and CaO in the composition is less than 9.2% by weight, the melt viscosity may be increased or the biodegradability may be decreased. If the total amount of MgO and CaO is less than 12.5% by weight, the glass melt crystallinity may be increased, resulting in process troubles or fiber quality. Can be reduced.
  • the CaO / MgO in the composition is preferably 1.6 to 2.5, more preferably 1.75 to 2.5, if the ratio is less than 1.6 may lead to an increase in the manufacturing cost, if the ratio exceeds 2.5 will increase the degree of crystallinity during the fiberization Can be.
  • the biosolubility and the water resistance of the glass fiber can be further improved by appropriately adjusting the CaO / MgO ratio without changing the CaO + MgO amount.
  • compositions of the present invention include Na 2 O and K 2 O as another modified oxide. They act as a melting agent for smoothly advancing melting during glass melting by producing non-crosslinked oxygen of the glass, and also serve to improve the biodegradability of the fibers.
  • Glass fiber-producing composition of the present invention contains 15.5 ⁇ 18.7% by weight of the total amount of Na 2 O + K 2 O, and more preferably contain Na 2 O + K 2 O 16.0 to 17.0% by weight.
  • the content of each of Na 2 O and K 2 O may be freely selected within a range satisfying the above range of total amounts.
  • the content of each of Na 2 O and K 2 O may be in the range of 0 to 18.7 weight percent (eg, 0.1 to 18.6 weight percent), but the total amount thereof is as described above.
  • B 2 O 3 included in the composition of the present invention contributes to the improvement of biodegradability of the produced glass fibers, and is a component that helps glass melting as a flux during glass melting.
  • B 2 O 3 serves to increase the resilience of the fiber product by improving the elasticity of the glass fiber, and also serves to reduce the brittleness of the fiber that can occur due to the addition of the alkali metal oxide.
  • the composition for producing glass fibers of the present invention contains 4 to 7% by weight of B 2 O 3 , more preferably 5.5 to 6.5% by weight. If the B 2 O 3 content in the composition is less than 4% by weight, the biodegradability and mechanical properties of the glass fiber may be lowered. If the B 2 O 3 content is more than 7% by weight, melt instability may be caused, and manufacturing costs may increase.
  • P 2 O 5 included in the compositions of the present invention may compensate for the melt instability and raw materials and cost problems due to contribute to the biodegradable improvement of fibers, in particular the use of B 2 O 3 together with B 2 O 3.
  • Glass fiber-producing composition of the present invention and the P 2 O 5 containing 0.2 to 2% by weight, more preferably from 0.5 to 1.5% by weight. If the P 2 O 5 content in the composition is less than 0.2% by weight, the biodegradability of the glass fiber may be lowered. If the P 2 O 5 content is more than 2% by weight, the crystallinity of the glass fiber may be increased to cause process trouble and fiber quality.
  • the present invention is characterized in that both biodegradability and melt stability are improved by adding P 2 O 5 instead of reducing the amount of B 2 O 3 which is very positive for biodegradability but is highly volatile in the melting process and causes melt instability.
  • B 2 O 3 + P 2 O 5 in the composition for producing glass fibers is preferably 5.5 to 8.6 wt%, more preferably 6.0 to 8.0 wt%.
  • the total amount of B 2 O 3 and P 2 O 5 in the composition is less than 5.5% by weight, there may be a problem of lowering biodegradability, and when it exceeds 8.6% by weight, there may be a problem of melt instability, an increase in manufacturing cost, or a decrease in heat resistance. .
  • B 2 O 3 / P 2 O 5 in the composition is preferably 3-7, more preferably 3.7 to 6.5, if the ratio is less than 3, there may be a problem of an increase in the degree of crystallinity when fiberglass is fiberized If it exceeds 7, it may cause melt instability due to the excess of B 2 O 3 .
  • the case of the composition within the B 2 O 3 and P 2 O 5 and the total amount of B 2 O 3 / P 2 O 5 in the ratio satisfying the above-described level may be the best in terms of melt stability and raw material costs.
  • the sum of P 2 O 5 and B 2 O 3 is 7% by weight, of which P 2 O 5 is 1% by weight and B 2 O 3 is 6% by weight.
  • the composition for producing glass fibers according to the present invention may include components such as TiO 2 , Fe 2 O 3 , BaO, etc., as impurities, depending on the raw materials used, but if the total amount thereof is maintained at a level of 2% by weight or less in the total composition Therefore, the physical property of a fiber does not fall.
  • the following KI index of the composition for producing glass fibers is less than 40.
  • KI [Na 2 O + K 2 O + CaO + MgO + B 2 O 3 + BaO] content-2 ⁇ Al 2 O 3 content
  • the method for producing the composition for producing glass fibers according to the present invention can be prepared by a method for producing a composition for ordinary glass fibers using the above components in the content range.
  • it may be prepared by the same method as the electric melting method, but is not limited thereto.
  • the viscosity of the composition required in the fiberization operation in using this fiberization method is preferably log ⁇ 3, that is, around 1000 poise viscosity.
  • the viscosity of the melt is a function of temperature and the corresponding composition, and the viscosity of the melt having the same composition will depend on the temperature. When the temperature of the melt is high during the fiberization, the viscosity is lowered. On the contrary, when the fiberization temperature is low, the viscosity is increased to affect the fiberization.
  • the length of the produced fiber is short and thin, as well as a lot of fine microfiber shots are generated, resulting in a low fiberization yield and a high diameter even when the fiber composition is too high. There is a problem that the fibers are formed and the coarse microfiber material (shot) is increased.
  • biosoluble glass fiber which is produced from the composition for producing glass fibers of the present invention as described above.
  • the glass fiber of the present invention is preferably 1) 300 ng / cm 2 ⁇ hr or more, more preferably 400 ng / cm 2 ⁇ hr or more, the dissolution rate constant for the artificial body fluid, 2) 1000 ° C. or less, more preferably Liquidus temperature of 950 ° C or lower, 3) fibrous working temperature higher than 100 ° C, more preferably 110 ° C or higher (log ⁇ 3), 4) 3% or less, more preferably 2.7% or less Satisfies one or more of the reduction rate conditions in the water resistance test (maintained at 100 ° C./5 hours), more preferably two or more, even more preferably three or more, and most preferably all of these conditions .
  • the preferable fiber average particle diameter of the biosoluble glass fiber of this invention is 3-10 micrometers.
  • an insulation product comprising the glass fiber of the invention as described above.
  • the specific form of the insulation product for example, plate, board, blanket, pipe cover, or any other form is possible.
  • composition for producing glass fibers having the components and contents shown in the following Table 1 (Example) and Table 2 (Comparative Example) by the electric current melting method using a three-phase electrode rod, and then a conventional rotary process for manufacturing glass (melt)
  • the glass fiber was manufactured by dropping onto a spinner surface in the form of a centrifugal rotation to tension the fiber, and at the same time spraying a high pressure air from the rear side to finely fiber the fiber (fiber diameter: about 4 to 8 ⁇ m).
  • EDS and ICP analysis equipment was used for the content analysis of each component.
  • the dissolution rate constant (K dis ) value, the liquidus temperature (liquidus temperature), the fiberization working temperature (log ⁇ 3), and the reduction ratio in the water resistance test for the artificial body fluid were measured. It measured and calculated by the following method, and is shown to following Table 1 (Example) and Table 2 (Comparative Example).
  • the solubility in artificial body fluid was obtained by the following method.
  • the biodegradability of the ceramic fiber in the body was evaluated based on the solubility of the fiber in the artificial body fluid, and after comparing the residence time based on the solubility, the dissolution rate constant (K dis ) was calculated using the following equation.
  • d 0 is the initial average fiber diameter ( ⁇ m)
  • ⁇ is the initial density of the fiber (g / cm 3 )
  • M 0 is the mass of the initial fiber (mg)
  • M is the mass of the remaining dissolved fiber (mg)
  • t represents the experiment time (hr).
  • the fiber to be measured was placed between thin layers between 0.2 ⁇ m polycarbonate membrane filters fixed with a plastic filter support, and the dissolution rate was measured by filtering artificial fluid between the filters.
  • the temperature of the artificial fluid was continuously controlled at 37 ° C. and the flow rate was 135 mL / day, and the pH was maintained at 7.4 ⁇ 0.1 using CO 2 / N 2 (5% / 95%) gas.
  • the content (g) of the composition contained in 1 L of the artificial fluid (gamble solution) used to measure the dissolution rate of the fiber was as follows.
  • the liquidus temperature can be defined as the maximum temperature at which crystals can be produced in the glass fiber and measured according to ASTM C829-81.
  • the fiberization operation temperature is a temperature at which the viscosity of the glass melt becomes approximately 1000 poise, and the fiberization operation takes place near this temperature.
  • the fiberization working temperature was measured by melting the glass composition in the platinum bushing while measuring the viscosity with the platinum spindle under temperature control. This method is commonly used in glass industry and glass fiber industry.
  • the glass fiber prepared according to the present invention exhibited excellent biodegradability of K dis value of 300 ng / cm 2 h or more and at the same time excellent water resistance (ie, low loss ratio), and fiberization.
  • the difference between the working temperature (log ⁇ 3) and the liquidus temperature was also over 100 °C, and the fiber could be safely produced without any process problems such as the formation of crystallization in the spinner.
  • Comparative Example 1 it can be seen that the biosolubility was very poor in a composition similar to the conventional general glass fiber products.
  • Comparative Example 2 it was impossible to apply to the heat insulating material due to the poor water resistance.
  • Comparative Example 3 the energy cost was increased due to the high liquidus temperature, and the crystallinity was increased during the fiberization process because the difference between the liquidus temperature and the fiberization working temperature was not large. As a result, the fiber quality was degraded.
  • Comparative Examples 4 and 5 the difference between the liquidus temperature and the fiberization working temperature was not large, and thus the crystallinity was increased during the fiberization process, and thus the fiber quality was lowered.

Abstract

La présente invention concerne une composition de production de fibre de verre et une fibre de verre biosoluble fabriquée à partir de celle-ci et concerne plus particulièrement : une composition de production de fibre de verre qui permet à la fibre de verre de présenter d'excellentes biosolubilité, résistance à l'eau, propriétés de travail et similaires et qui peut être produite selon un procédé rotatif existant, par ajout de SiO2, Al2O3, CaO, MgO, Na2O, K2O, B2O3 et P2O5 dans des proportions ajustées ; et une fibre de verre biosoluble produite à partir de celle-ci.
PCT/KR2013/003160 2013-04-15 2013-04-15 Composition de production de fibre de verre et fibre de verre biosoluble produite à partir de celle-ci WO2014171561A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/KR2013/003160 WO2014171561A1 (fr) 2013-04-15 2013-04-15 Composition de production de fibre de verre et fibre de verre biosoluble produite à partir de celle-ci

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/KR2013/003160 WO2014171561A1 (fr) 2013-04-15 2013-04-15 Composition de production de fibre de verre et fibre de verre biosoluble produite à partir de celle-ci

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WO2014171561A1 true WO2014171561A1 (fr) 2014-10-23

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995032926A1 (fr) * 1994-05-28 1995-12-07 Isover Saint-Gobain Compositions de fibres de verre
KR0167763B1 (ko) * 1989-08-11 1999-01-15 이소베 생-고벵 생리학적 매질 속에서 분해가능한 유리섬유
KR20030058921A (ko) * 2001-12-29 2003-07-07 주식회사 금강고려화학 인공체액에 대한 용해도가 우수한 고온단열재용 생분해성세라믹 섬유조성물
US6852656B1 (en) * 1999-09-30 2005-02-08 Techint Compagnia Tecnica Internazionale S.P.A. Glass fiber composition
KR20110107816A (ko) * 2008-12-30 2011-10-04 쌩-고벵 이조베르 내화 광물성 면 절연 제품, 그 제작 방법 및 적합한 결합 조성물

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR0167763B1 (ko) * 1989-08-11 1999-01-15 이소베 생-고벵 생리학적 매질 속에서 분해가능한 유리섬유
WO1995032926A1 (fr) * 1994-05-28 1995-12-07 Isover Saint-Gobain Compositions de fibres de verre
US6852656B1 (en) * 1999-09-30 2005-02-08 Techint Compagnia Tecnica Internazionale S.P.A. Glass fiber composition
KR20030058921A (ko) * 2001-12-29 2003-07-07 주식회사 금강고려화학 인공체액에 대한 용해도가 우수한 고온단열재용 생분해성세라믹 섬유조성물
KR20110107816A (ko) * 2008-12-30 2011-10-04 쌩-고벵 이조베르 내화 광물성 면 절연 제품, 그 제작 방법 및 적합한 결합 조성물

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