WO2007141196A1 - Silice agglomérée - Google Patents

Silice agglomérée Download PDF

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Publication number
WO2007141196A1
WO2007141196A1 PCT/EP2007/055365 EP2007055365W WO2007141196A1 WO 2007141196 A1 WO2007141196 A1 WO 2007141196A1 EP 2007055365 W EP2007055365 W EP 2007055365W WO 2007141196 A1 WO2007141196 A1 WO 2007141196A1
Authority
WO
WIPO (PCT)
Prior art keywords
particles
silica
organic solvent
water
alcohol
Prior art date
Application number
PCT/EP2007/055365
Other languages
English (en)
Inventor
Lorenzo Costa
Björn BRAUN
Original Assignee
Degussa Novara Technology S.P.A.
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.)
Filing date
Publication date
Application filed by Degussa Novara Technology S.P.A. filed Critical Degussa Novara Technology S.P.A.
Priority to CA2653155A priority Critical patent/CA2653155C/fr
Priority to AU2007255488A priority patent/AU2007255488B2/en
Priority to JP2009512608A priority patent/JP2009538816A/ja
Priority to EP07729766A priority patent/EP2024286B1/fr
Priority to US12/301,744 priority patent/US20100003182A1/en
Priority to CN2007800205334A priority patent/CN101460400B/zh
Priority to KR1020087029435A priority patent/KR101089897B1/ko
Publication of WO2007141196A1 publication Critical patent/WO2007141196A1/fr
Priority to NO20084294A priority patent/NO20084294L/no

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • 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
    • C03C1/026—Pelletisation or prereacting of powdered raw materials
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3009—Physical treatment, e.g. grinding; treatment with ultrasonic vibrations
    • C09C1/3036—Agglomeration, granulation, pelleting
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3081—Treatment with organo-silicon compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the subject of the invention is pelletized silica particles, the method to produces them and their use.
  • step b) calcining the powder of step b) (US 5,516,350).
  • the particle size of the gel before the calcinaton step was adjusted to a diameter of 60 to 900 ⁇ m.
  • the reference is silent about the particle size of the sintered quartz glass powder and the feature on its flowability.
  • the spherical material shows in the case of monomodal distribution a diameter between lnm and 1.000 nm. It can be used as a support for catalysts for the polymerization and copolymerization of olefinically unsaturated compounds (EP 0 537 850 Al) .
  • step A mixing either the pure (step A) or the hybrid (step B) silica sol in an organic media constituted by monofunctional aliphatic alcohols R-OH or mixtures thereof
  • the spherical silica particles show a particle diameter within the range of from 10 to 100 micrometers (EP 0 653 378 Al) .
  • free flowing powder composition used throughout this specification is meant a powder (made by milling, micropelletizing, or similar technique) of which the particles consist of a composition as defined above and of which the particles do not adhere to one other.
  • the size of the powder particles is expressed in terms of the particles diameter. In general, this size is determined by sieving and is independent of the shape of the particle.
  • cohesive powder are those powders in which the cohesive forces among the particles are very important (strengthwise) .
  • a free flowing powder does not contains fines.
  • a conventional spray drying technique in which a spray dryer mixes a heated gas with an atomized (sprayed) liquid stream within a vessel (drying chamber) to accomplish evaporation and produce a free flowing dry powder with a controlled average particle size is that available for instance by SDS Spray Drying Limited. With such spray drier it is possible to produce particle with averaged dimension of 300 micron with rather narrow particle size distribution .
  • a) segregation mainly due to differences on size of the particles, and to a minor extend differences in particle density. More in detail the forces that drive the segregation are: Van der Walls forces, electrostatic forces, liquid bridges, solid matter bridges and entanglement.
  • silica When it comes to purity of the particle a major importance plays the silica. In fact nowadays there is a growing demand of silica with high purity grade for new high end applications, such as: the inner part of crucibles, optical fibers and components for microelectronics among the others. Unfortunately on the market there isn't a large availability of such a product, because of the very high costs and the very complex production procedures.
  • the subject of the invention are pelletized silica particles, which are characterized by a round shape and a monomodal particle size distribution.
  • Particles of silica according to the invention have the said silica as core with all around Si ⁇ 2 obtained via hydrolysis of liquid alkoxisilane .
  • the silica can be Si ⁇ 2 as fumed silica or natural quartz.
  • the natural quartz can be i. e. JOTA 4 Type from JOTA Corporation and natural quartz from Norwegian Crystallites.
  • the pelletized inorganic oxide particles can consist of natural quartz which is surrounded by silicondioxid, obtained via hydrolysis of liquid alkoxisilane.
  • the alkoxisilane can be preferably tetraalkolisilane like tetraethoxy silane.
  • the said pelletized inorganic oxide particles according to the invention can be characterized by a surface area exceeding 50 m 2 /g.
  • the said pelletized inorganic oxide particles can have a size by which at least 90% are bigger than 100 micron. At least 90% of the pores can have a diameter lying between 50 and 1000 Angstrom.
  • alkoxisilane can be mixed with a soluble salt in order to obtained pelletized inorganic oxide particles doped with metals.
  • the free-flowing value is in the range from to more preferably from 5 to 2 according to the method developed by
  • a further object of this invention is a method for the production of the pelletized silica particles having a round shape and a monomodal particle size distribution.
  • the invention which is characterized in that inorganic silica, to be palletized, is added under stirring in a vessel containing acidic water, when the dispersion is clearly homogeneous and without lumps liquid alkoxide silane such as i. e. tetramethoxisilane and/or tetraethoxysilane is then added very slowly to the mixture. As consequence of the exothermic reaction the temperature raises.
  • the so obtained dispersion is then transferred slowly by means, for example, of a cannula in a vessel containing an organic solvent or a silicon oil previously mixed with an ammonia derivatives kept under strong stirring.
  • the drops of silica dispersion in contact with the alkaline organic solution form gelly particles that are collected on the bottom of the reactor and then transferred to another vessel to be washed with an alcohol and/or an ester such as dioxane, propanol, acetone, ethanol or pure ethyl acetate among the others, finally the particles are then washed with acetone.
  • the organic solvent or the silicon oil is then used for further runs.
  • the particles are then filtered and then the solvent is extracted under supercritical or slightly subcritical conditions. Alternatively the solvent can be removed by control drying under controlled conditions (% humidity and T) .
  • the dried particles are then calcinated at high temperature with oxygen for at least 1 hour in order to eliminate traces of the solvents from the silica particles.
  • the pelletization can be obtained by using sol-gel techniques which has been partially described in the EP 0 537 850 Al.
  • the method can comprise the following features:
  • the solution is then poured in a vessel containing an organic solvent by means of a cannula.
  • the pH is then risen by addition of an amine such as the Primene type supplied by Rohm and Haas, till very alkaline conditions are created, for example pH for 10% in water solution.
  • the temperature further rises.
  • the particles are then removed in continuous from the reaction batch and the obtained particles are then washed abundantly with water, in order to eliminate the residual solvent.
  • the material so obtained is then calcinated in a vertical furnace at 600 ⁇ 150° C for 6 ⁇ 2 hours in order to eliminate residual solvents .
  • the treated particles have a size in at least 90% of the particle have a size higher than 100 micron.
  • the pelletization is obtained by using tetraethoxysilane as pelletizasing agent.
  • the solution is then poured in a vessel containing an organic solvent kept under strong stirring.
  • the pH is then risen by addition of an amine such as the Primene type supplied by Rohm and Haas, till very alkaline conditions are created, for example pH for 10% in water solution.
  • the temperature further rises.
  • the particles are then removed in continouos from obtained particles are then washed abundantly with water, in order to eliminate the residual solvent.
  • the material so obtained is then calcinated in a vertical furnace at 600 ⁇ 150° C for 6 ⁇ 2 hours in order to eliminate residual solvents.
  • Particles are characterized by the fact that there is an almost continuous phase between the pellettizasing agent (the hydrolised silica alkoxide like TEOS) and the core material, since the pelletisating agent is able to impregnate the inorganic oxide particles.
  • the pellettizasing agent the hydrolised silica alkoxide like TEOS
  • the glassy particles obtained with this method according to the invention are characterized in terms of: flowability, microporosity and size distribution. Elsewhere, when the said inorganic oxide is silica or silica quartz the method allows to obtain a higher purity of the final product when compared to that of the starting particles. The purity increases approximately as direct function of the quantity of pelletizasing agent silica alkoxide like TEOS used.
  • the starting pH of the aqueous solution with inorganic oxide particles can be in the rage 1 to 4.
  • the liquid alkoxi silane can be tetramethoxisilane (CH 3 O) 4 Si and/or tetraethoxysilane (CH 3 -CH 2 -O) 4 Si.
  • the organic solvent can be an apolar organic solvent, which has a dielectric constant lower than 60 at 20 0 C.
  • the salt to be added in order to obtain the doped silica particles can be inter alias, aluminum acetate, aluminum sulfate, aluminum ammonium sulfate, lead acetate, boric acid, ammonium fluoride sulfate, ammonium fluoride.
  • the apolar organic solvent can be a liquid alkane such as hexane, eptane, octane, nonane and alcohol such as: propanol, butanol, pentanol, hexanol, eptanol, octanol, nonanol, decanol and a aromatic compound like toluene, benzene, nitrobenzene, chlorobenzene, dichlorobenzene, quinoline, decaline and/or a mixture thereof.
  • a liquid alkane such as hexane, eptane, octane, nonane and alcohol
  • alcohol such as: propanol, butanol, pentanol, hexanol, eptanol, octanol, nonanol, decanol and a aromatic compound like toluene, benzene, nitrobenzene, chlorobenzene, dich
  • organic solvent silicon oil can be used.
  • the silicon oil can be polydimethylsiloxane fluids like Dimethicone from Wacker Chemie AG listed under the brand name Wacker AK 50.
  • the organic base ammonia derivative can be cyclohexyilamine, t-alkyl amine.
  • the pH after the addition of the organic base can be in the range from 8 to 13, more preferably from 10 to 11 expressed as 10% water solution.
  • the calcinations temperature can be between 300 and 700 0 C more preferably between 300 and 600°.
  • the pelletized silica particles are characterized by round shape and they are virtually without fines.
  • microporosity and surface area of the material have been determined according to the method DIN 66131 by means of ASAP 2010 instrument from Micromeritics; measurements are carried out in liquid nitrogen.
  • Solvents used to disperse the gelly particles during titration with ammonia derivatives are apolar, with dielectric constant not higher than 60.
  • the list of tested solvents includes: alkane such as hexane, eptane, octane, nonane and alcohol such as: propanol, butanol, pentanol, hexanol, eptanol, octanol, nonanol, decanol and a aromatic compound like toluene, benzene, nitrobenzene, chlorobenzene, dichlorobenzene, quinoline and decaline.
  • the pelletized silica particles purity has been checked via ICP-MAS.
  • the pelletized silica particles, according to the invention can significantly raise the yield of transportation of the material by reducing the quantity of fines and narrowing the particle size distribution.
  • Example 1 Example 1 :
  • hydrochloric acid 37 Gew.-% cone is added to 900 ml of water in a 4 1 vessel till pH 2 is reached. Under stirring are then added very slowly 65Og of fumed silica, Aerosil EG50 supplied by Degussa, to be pelletized. When the dispersion is clear and homogeneous and without lumps, 65Og TEOS (Dynasil 40 fom DEGUSSA AG) are then added very slowly to the mixture. As consequence of the exothermic hydrolysis reaction the temperature rises up to 24°C.
  • the solution is then poured slowly dropwise by means of a cannula in a 22 1 vessel containing 15 1 of silicon oil (Wacker AK 50 from Wacker Chemie) mixed with a tertiary amine that had given a pH of 11 (expressed for a 10% water solution) : Primene JM-T (supplied by Rohm and Haas) .
  • the temperature further rises up to 31°C.
  • the emulsion containing the gelly particles is then filtered and the so obtained particle are then washed abundantly with water/acetone solution, in order to eliminate the residual silicon oil.
  • the material so obtained is then calcinated in a vertical furnace at 600° C for 8 hour in order to eliminate residual solvents.
  • Particles size The material is characterized by monomodal size distribution
  • the averaged diameter is 430 micron
  • Porosity Pores diameter 60 Angstrom, surface area 99 m2/g which is almost twice of the surface area of the starting material . Elemental Analysis:
  • the pelletisation improves greatly the dimension of the particles and its dispersion as well (monomodal distribution) , not only, because the purity of the final material is much better than that of the starting particles .
  • starting material mark is 5 while the palletized silica has a mark of 2, which means the pelletization process has improved the free flowing behaviour.
  • the emulsion containing the gelly particles is then filtered and the so obtained particle are then washed abundantly with water, in order to eliminate the residual silicon oil.
  • the material so obtained is then calcinated in a vertical furnace at 600° C for 8 hour in order to eliminate residual solvents.
  • the averaged diameter is 500 micron
  • Porosity Surface area 74 m2/g which has to be compared with the almost indetectable low surface area of the natural quartz.
  • the pelletisation improves greatly the dimension of the particles and its dispersion as well (monomodal distribution) , not only, because the purity of the final material is much better than that of the starting particles .
  • starting material mark is 5 while the palletized natural quartz before the calcinations process has a mark of 4 whereas after the calcinations process the mark is between 2 and 3 which means that the pelletization process has improved the free flowing behaviour.
  • the averaged diameter is 300 micron

Abstract

La présente invention concerne des particules de silice agglomérée caractérisées par une forme ronde et une granulométrie monomode produites par dispersion de particules de silice dans l'eau, ajout d'eau à la dispersion, mélange avec un alcoxysilane, versement du mélange dans un solvant organique, filtrage et lavage des particules de silice obtenues. Les particules de silice agglomérée peuvent être utilisées pour produire des monolithes de verre.
PCT/EP2007/055365 2006-06-02 2007-05-31 Silice agglomérée WO2007141196A1 (fr)

Priority Applications (8)

Application Number Priority Date Filing Date Title
CA2653155A CA2653155C (fr) 2006-06-02 2007-05-31 Silice agglomeree
AU2007255488A AU2007255488B2 (en) 2006-06-02 2007-05-31 Pelletized silica
JP2009512608A JP2009538816A (ja) 2006-06-02 2007-05-31 ペレット化シリカ
EP07729766A EP2024286B1 (fr) 2006-06-02 2007-05-31 Silice agglomérée
US12/301,744 US20100003182A1 (en) 2006-06-02 2007-05-31 Pellitized silica
CN2007800205334A CN101460400B (zh) 2006-06-02 2007-05-31 粒状二氧化硅
KR1020087029435A KR101089897B1 (ko) 2006-06-02 2007-05-31 펠렛화된 실리카
NO20084294A NO20084294L (no) 2006-06-02 2008-10-14 Pelletisert silika

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EPPCT/EP2006/062883 2006-06-02
EP2006062883 2006-06-02

Publications (1)

Publication Number Publication Date
WO2007141196A1 true WO2007141196A1 (fr) 2007-12-13

Family

ID=37697918

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2007/055365 WO2007141196A1 (fr) 2006-06-02 2007-05-31 Silice agglomérée

Country Status (8)

Country Link
JP (1) JP2009538816A (fr)
KR (1) KR101089897B1 (fr)
CN (1) CN101460400B (fr)
AU (1) AU2007255488B2 (fr)
CA (1) CA2653155C (fr)
NO (1) NO20084294L (fr)
TW (1) TWI372139B (fr)
WO (1) WO2007141196A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2559608A (en) * 2017-02-13 2018-08-15 Sibelco Nederland N V Grains comprising silica and methods of forming grains comprising silica
WO2018231367A1 (fr) * 2017-06-16 2018-12-20 Owens-Brockway Glass Container Inc. Matériau de mélange vitrifiable et procédé de fabrication de verre

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111747417A (zh) * 2019-03-28 2020-10-09 福建通源硅业有限公司 一种二氧化硅颗粒的制备方法
CN110479954A (zh) * 2019-08-19 2019-11-22 安徽省含山县兴建铸造厂 一种熔模铸造精密铸件用型壳耐火涂层材料
CN111170344A (zh) * 2020-01-15 2020-05-19 珠海琴晟新材料有限公司 一种超高纯纳米材料的制备方法
CN111868159B (zh) * 2020-02-17 2022-07-26 浙江三时纪新材科技有限公司 一种球形二氧化硅粉体填料的制备方法、由此得到的粉体填料及其应用
CN111634915A (zh) * 2020-06-12 2020-09-08 将乐三晶新材料有限公司 熔融金属硅雾化制粉工艺
CN115974089B (zh) * 2023-02-17 2023-10-20 江苏海格新材料有限公司 一种活性硅微粉的生产方法

Citations (3)

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EP0725037A1 (fr) * 1995-02-04 1996-08-07 Degussa Ag Granules à base de silice pyrogène, procédé pour leur préparation et leur utilisation
EP1266864A1 (fr) * 2001-05-17 2002-12-18 Degussa AG Granules à base d'une silice pyrogénique dopée à l'alumine et obtenue au moyen d'un aérosol, leur procédé de préparation et leur utilisation
WO2005085135A1 (fr) * 2004-03-08 2005-09-15 Merck Patent Gmbh Procede de production de particules de sio2 monodispersees

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JPS62260712A (ja) * 1986-05-02 1987-11-13 Toray Ind Inc シリカ粒子の製造法
JPH08281095A (ja) * 1995-02-14 1996-10-29 Toyota Motor Corp ダイラタンシー性液体
DE10256267A1 (de) * 2002-12-03 2004-06-24 Degussa Ag Dispersion, Streichfarbe und Aufnahmemedium

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
EP0725037A1 (fr) * 1995-02-04 1996-08-07 Degussa Ag Granules à base de silice pyrogène, procédé pour leur préparation et leur utilisation
EP1266864A1 (fr) * 2001-05-17 2002-12-18 Degussa AG Granules à base d'une silice pyrogénique dopée à l'alumine et obtenue au moyen d'un aérosol, leur procédé de préparation et leur utilisation
WO2005085135A1 (fr) * 2004-03-08 2005-09-15 Merck Patent Gmbh Procede de production de particules de sio2 monodispersees

Non-Patent Citations (1)

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Title
CHANG S M ET AL: "Preparation of large monodispersed spherical silica particles using seed particle growth", JOURNAL OF COLLOID AND INTERFACE SCIENCE, ACADEMIC PRESS, NEW YORK, NY, US, vol. 286, no. 2, 15 June 2005 (2005-06-15), pages 536 - 542, XP004894856, ISSN: 0021-9797 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2559608A (en) * 2017-02-13 2018-08-15 Sibelco Nederland N V Grains comprising silica and methods of forming grains comprising silica
WO2018231367A1 (fr) * 2017-06-16 2018-12-20 Owens-Brockway Glass Container Inc. Matériau de mélange vitrifiable et procédé de fabrication de verre
US20180362380A1 (en) * 2017-06-16 2018-12-20 Owens-Brockway Glass Container Inc. Glass batch material and process for making glass
US10343941B2 (en) 2017-06-16 2019-07-09 Owens-Brockway Glass Container Inc. Glass batch material and process for making glass

Also Published As

Publication number Publication date
CN101460400B (zh) 2011-09-14
CN101460400A (zh) 2009-06-17
NO20084294L (no) 2009-01-09
TWI372139B (en) 2012-09-11
TW200815284A (en) 2008-04-01
AU2007255488B2 (en) 2011-01-27
AU2007255488A1 (en) 2007-12-13
JP2009538816A (ja) 2009-11-12
KR101089897B1 (ko) 2011-12-05
KR20090009290A (ko) 2009-01-22
CA2653155A1 (fr) 2007-12-13
CA2653155C (fr) 2012-01-24

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