(19) Japan Patent Office (JP)
`
`(12) Japanese Unexamined Patent
`Application Publication (A)
`
`(51) Int. Cl.5
`C03C 1/02
`
`Identification codes
`
`JPO file numbers
`6791-4G
`
` FI
`
`(11) Japanese Unexamined Patent
`Application Publication Number
`H4-219340
`(43) Publication date August 10, 1992
`
`Technical indications
`
`Request for examination: Not yet requested: Number of claims: 11 (Total of 5 pages)
`
`(21) Application number
`(22) Date of application
`
`H2-402553
`December 15, 1990
`
`(71) Applicant
`
`(72) Inventor
`
`(72) Inventor
`
`(74) Agent
`
`000253503
`KIRIN BREWERY COMPANY, LIMITED
`6-26-1 JINGUMAE, SHIBUYA-KU, TOKYO
`NAKAMURA, KOJI
`℅ KIRIN BREWERY COMPANY, LIMITED
`6-26-1 JINGUMAE, SHIBUYA-KU, TOKYO
`YOKOKURA, SHUICHI
`℅ KIRIN BREWERY COMPANY, LIMITED
`6-26-1 JINGUMAE, SHIBUYA-KU, TOKYO
`Patent attorney SATO, KAZUO (AND 2 OTHERS)
`
`(54) [TITLE OF THE INVENTION]
`Decoloring Method for Amber Glass
`[ABSTRACT]
`[OBJECT]
`The object of the present invention is to provide a
`method wherein decoloring of the amber color of amber
`glass can be achieved through a temperature that is
`remarkably
`lower
`in comparison with
`that of
`the
`conventional oxidation method, for example, a temperature
`of between about 700 and 900°C.
`[STRUCTURE]
`The present invention is a decoloring method for amber
`glass including heating the amber glass together with a zinc
`compound and/or an antimony compound. Additionally, the
`present invention is a decoloring method for colored glass,
`including heating, together with an antimony compound,
`colored glass that is colored with iron.
`
`[VERTICAL AXIS] Reflectivity (%)
`[HORIZONTAL AXIS] Beam Wavelength (nm)
`[IN FIGURE] Embodiment 1
`Embodiment 2
`Control (No decoloring agent added)
`
`O-I Glass, Inc.
`Exhibit 1036
`Page 001
`
`

`

`[PATENT CLAIMS]
`[CLAIM 1]
`A decoloring method for amber glass, including:
`heating the amber glass together with a zinc compound.
`[CLAIM 2]
`A decoloring method for amber glass as set forth in
`claim 1, wherein:
`the zinc compound is zinc carbonate, zinc nitrate, zinc
`sulfate, zinc chloride, zinc hydroxide, or zinc phosphate.
`[CLAIM 3]
`A decoloring method for amber glass as set forth in
`claim 1 and [sic – "or"?] 2, wherein:
`the amount of the zinc compound is between 2 and 15
`parts by weight in respect to 100 parts by weight of the
`amber glass.
`[CLAIM 4]
`A decoloring method for amber glass as set forth in [any
`one of] claims 1 through 3, wherein:
`an antimony compound is also added.
`[CLAIM 5]
`A decoloring method for colored glass, including:
`heating, together with an antimony compound, a colored
`glass that has been colored with iron.
`[CLAIM 6]
`A decoloring method for colored glass as set forth in
`claim 5, wherein:
`the colored glass that is colored with iron is amber glass
`wherein an amber color that is derived from a sulfide
`colloid is decolored.
`[CLAIM 7]
`A decoloring method for colored glass as set forth in
`claims 4 through 6, wherein:
`the antimony compound is antimony oxide, antimony
`trichloride, or antimony pentachloride.
`[CLAIM 8]
`A decoloring method for colored glass as set forth in
`claims 4 through 7, wherein:
`the amount of antimony compound present is between 1
`and 5 parts by weight in respect to 100 parts by weight of
`amber glass.
`[CLAIM 9]
`A decoloring method for colored glass as set forth in
`claims 1 through 8, heated [sic] to a temperature of no less
`than the glass transition point of the glass that is to be
`decolored.
`[CLAIM 10]
`A decoloring method for colored glass as set forth in
`claims 1 through 9, wherein:
`a heating temperature is no less than 700°C, and a
`heating time is no less than 30 minutes.
`[CLAIM 11]
`Glass that has been decolored through a method as set
`forth in Claims 1 through 10.
`[DETAILED EXPLANATION OF THE INVENTION]
`[0001]
`[BACKGROUND OF THE INVENTION]
`[INDUSTRIAL FIELD OF APPLICATION]
`The present invention relates to a decoloring method for
`amber glass.
`[0002]
`[PRIOR ART]
`
`Japanese Unexamined Patent Application Publication H4-219340
`(2)
`
`Glass that is broadly used in various types of beverage
`bottles, such as for beer, sake, and the like, that is currently
`available commercially includes so-called "amber glass,"
`that is colored brown through a sulfide colloid. After this
`amber glass has been used in the market, it is ultimately
`recycled as cullet (refuse glass). However, the fields or
`applications wherein glass that has been colored, such as
`amber glass, is used are limited. For example, when
`recycled as a glass raw material, it is recycled only in glass
`of the same color tone, and reusing in glass with a different
`color tone has been difficult. If the amber color of the
`amber glass could be decolored, this could enlarge the
`scope of reuse.
`[0003]
`Conventionally, several methods for decoloring amber
`glass have been proposed. For example, there is a method
`wherein Na2SO4, NaNO3, As2O3, or the like, is added, as an
`oxidizing agent, to amber glass that has been pulverized
`into microparticles, and melted by heating to at least
`1200°C after mixing. (This method may be termed the
`"oxidizing method," below.) In this method, the result of
`heating and mixing is that the sulfur, which is the substance
`that is the primary cause for the coloration, is oxidized, or
`is eliminated (evaporated) from the glass melt as sulfurous
`acid gas. However, in this oxidizing method, decoloring
`requires melting through heating the glass to no less than
`1200°C, and thus there is a drawback in that the thermal
`energy cost is large.
`[0004]
`Moreover, the amber glass that is used today typically
`includes iron content of between about 0.2 and 0.3% by
`weight as, for example, Fe2O3. The result is that the glass
`that has been decolored through the oxidizing method,
`described above, may have coloration (light blue-green)
`caused by this iron content. Decoloring this coloration
`conventionally has been performed through a method of
`heating after adding a coloring agent
`that has a
`complementary color relationship with blue-green (for
`example, Mn, Co, Se, or the like). However, the coloring
`agents used conventionally require melting of the glass
`through heating to at least 1200°C after addition of the
`coloring agent, or else no decoloring effect would be
`produced. That
`is,
`in
`the conventional amber glass
`decoloring methods, heating to a high temperature of no
`less than 1200°C is required in order to appear to the eye as
`completely decolored (whitened).
`[0005]
`[SUMMARY OF THE INVENTION]
`[PROBLEM SOLVED BY THE PRESENT INVENTION]
`The object of the present invention is to provide a
`method that enables decoloring of the amber color of a
`carbon-sulfur amber glass (termed simply "amber glass" in
`this specification) at a temperature of, for example,
`between 700 and 900 °C, which is remarkably low when
`compared to that of the conventional oxidizing method.
`Moreover, an object of the present invention is to provide a
`method for achieving decoloring of the color derived from
`iron in colored glass that is colored with iron, and,
`specifically, of an amber color that is derived from a sulfide
`colloid, similarly at a low temperature, for example, the
`temperature of between 790°C. Moreover, an object of the
`present invention is to provide a decoloring method for
`
`O-I Glass, Inc.
`Exhibit 1036
`Page 002
`
`

`

`decoloring (whitening) amber glass in its appearance to the
`eye.
`[0006]
`[MEANS FOR SOLVING THE PROBLEM]
`SUMMARY
`That is, the decoloring method for amber glass according
`to the present invention includes heating the amber glass
`together with a zinc compound.
`[0007]
`Moreover, in another aspect of the present invention, the
`decoloring method for colored glass according to the
`present
`invention
`includes heating,
`together with an
`antimony compound, colored glass that is colored with iron,
`and, in particular, amber glass wherein the amber color
`derived from the sulfide colloid has been decolored.
`[0008]
`The amber color of the amber glass that is used in typical
`beer bottles, and the like, at present is colored through a
`sulfide colloid
`that exists
`therein, and, specifically,
`complexes of sulfur chains and iron. Given the decoloring
`method according the present invention, the amber color
`can be decolored through heating the amber glass and the
`sulfur compounds to a low temperature, for example, a
`temperature in excess of 700°C, at the highest. The
`decoloring mechanism is believed to be that the amber
`color is removed through chemically breaking the sulfur
`chains simultaneously with the reaction between sulfur and
`zinc ions. On the other hand, given that the zinc sulfide
`(ZnS) that is generated is white, the glass after decoloring
`will be substantially white or light blue-green, greatly
`removing the limits the applications due to the color thereof,
`so a broad range of recycling applications can be
`anticipated. In this way, it is believed that the sulfur and the
`zinc ions in the molten glass can be reacted to form zinc
`sulfide, to break the sulfur chains, and that that this reaction
`can be achieved at a low temperature has not been
`anticipated.
`[0009]
`Moreover, in the decoloring method according the
`present invention, the blue-green caused by the iron content
`that remains after decoloring of the color caused by the
`sulfur chains in the amber glass can be decolored through
`heating to, for example, no more than 700°C. That is, when
`an antimony compound is heated together with the amber
`glass, antimony sulfide (Sb2S3) is generated. The antimony
`sulfide
`is
`red, which has a complementary color
`relationship with blue-green, enabling decoloring of the
`amber glass. It had not been anticipated that, in molten
`glass, antimony ions and sulfur can be reacted to form
`antimony sulfide at a low temperature, enabling amber
`glass to be decolored (whitened) in its appearance of the
`eye.
`[0010]
`[DETAILED EXPLANATION OF THE INVENTION]
`The colored glass to which the decoloring method
`according to the present invention can be applied is that
`which is colored brown through a sulfide colloid, known as
`"amber glass." Here "amber glass" is not simply a literal
`descriptor, but rather is used to mean glass that is actually
`colored through a sulfide colloid, for example, a sulfur
`chain, such as, for example, soda lime glass, or the like.
`[0011]
`
`Japanese Unexamined Patent Application Publication H4-219340
`(3)
`
`In the method according the present invention, there is
`no particular limitation on the zinc compound that is added
`to the colored glass, insofar as it can produce zinc ions in
`the molten glass. Specific examples include zinc carbonate
`(ZnCO3), zinc oxide (ZnO), zinc nitrate (ZnNO3), zinc
`sulfate (ZnSO4), zinc chloride (ZnCl2), and zinc hydroxide
`(Zn(OH)2), zinc phosphate (Zn(PO4) · 4 H2O), and the like.
`Zinc carbonate is preferred in particular.
`[0012]
`The amount of this zinc compound added is dependent
`on the amount of sulfur that exists in the glass bottle that is
`to be decolored, and, of course,
`is determined as
`appropriate. For example, in the case of glass that is used
`broadly today for beer bottles, sulfur is included at about
`0.1% by weight (calculated SO3 equivalent). Between 2 and
`15 parts by weight in respect to 100 parts by weight glass is
`preferred, and between 5 and 10 parts by weight is more
`preferred. At 2 parts by weight the discoloring effect would
`be inadequate, and if more than 15 parts by weight, this
`could cause a reduction in strength of the decolored glass,
`and would not be useful in terms of cost as well.
`[0013]
`The decoloring is carried out through heating the glass
`together with a zinc compound. Preferably it is performed
`as described below. First the amber glass that is to be
`decolored is pulverized roughly, and then is subjected to
`fine pulverization through a ball mill, or the like. The finer
`the pulverized particle size, the greater the surface area,
`which is useful in achieving a reduction in the reaction time
`required for decoloring. However, there is no impediment
`to decoloring in normal practical application as long as it is
`no greater than about a 100 mesh. A zinc compound,
`described above, is added to the finely pulverized glass
`powder that has been prepared, and mixing is followed by
`melted through heating. In practice, the heating temperature
`should be no less than the glass transition point of the glass
`that is to be decolored. However, given the relationship
`with the reaction speed, generally 700°C or more is
`preferred. Moreover, when the heating temperature is
`between about 700 and 800°C, parts may be seen wherein
`the decoloring is inadequate in the form of blotchy points,
`albeit small, depending on the pulverization grain size of
`the pulverized glass powder.
`However, with a heating temperature of 800°C or more,
`or preferably 850°C or more, the blotchy points are
`eliminated. The glass is decolorized through heating and
`melting for preferably no less than 30 minutes, and more
`preferably no less than 1 hour , at the temperature described
`above.
`[0014]
`The amber color is decolored through a reaction with the
`zinc compound, described above, where the resulting glass
`will appear white or light blue-green. As described above,
`when iron content exists in the glass, light blue-green will
`remain, even if the amber color is decolored. However,
`depending on the application, the decolored glass obtained
`through the decoloring operation described above can be
`reused directly.
`[0015]
`If iron content exists in the amber glass, a light blue-
`green, derived from the iron content (which typically exists
`as Fe2O3) will remain in the glass. In the present invention,
`
`O-I Glass, Inc.
`Exhibit 1036
`Page 003
`
`

`

`this coloration [sic?] can be achieved through heating the
`amber glass together with an antimony compound. In the
`method according to the present invention, there is no
`particular limitation to the antimony compound insofar as it
`can produce antimony ions in the melted glass. Specific
`examples
`include antimony oxide (Sb2O3), antimony
`trichloride (SbCl3), antimony pentchloride (SbCl5), and the
`like. Antimony oxide is preferred particularly .
`[0016]
`The amount with which these antimony compounds are
`added depends on the amount of iron content that exists in
`the glass bottle to be decolored, and of course is determined
`as appropriate. For example, in the case of the glass that is
`broadly used in beer bottles of today, iron content is
`included at between about 0.2 and 0.3% by weight as Fe2O3.
`The amount of antimony compounds to be added to this
`glass preferably is between 0.5 and 5 parts by weight, and
`more preferably between 1 and 3 parts by weight, in respect
`to 100 parts by weight of the amber glass. If less than 0.5
`parts by weight, the decoloring effect would be inadequate,
`and if greater than 5 parts by weight, the glass would be
`colored excessively red, which would be undesirable.
`[0017]
`The addition of the antimony compound preferably is
`carried out simultaneously when heating the amber glass
`together with the zinc compound, described above. The
`heating temperature and time conditions at this time are the
`same as those for the zinc compound alone, described
`above. Moreover, in the method described above the
`antimony compound may be added anew to the glass after
`decoloring of the amber color, and then caused to react
`under the same heating temperature and time conditions as
`for the zinc compound alone. Moreover, the decoloring
`through addition of the antimony compound may, of course,
`be applied also to glass wherein the amber color has been
`decolored through an amber color decoloring method other
`than that of the present invention, such as, for example, the
`oxidizing method.
`[0018]
`[EMBODIMENTS]
`EMBODIMENT 1
`A beer bottle made from carbon-sulfur amber glass
`(including 0.25% by weight Fe2O3) was pulverized to
`produce a powder of no greater than 100 mesh. After
`adding 5 g zinc carbonate (ZnCO3) and 2 g antimony oxide
`(Sb2O3) to 100 g of this glass powder and mixing, the
`material was placed in a crucible and heated for one hour at
`900°C in an electric furnace, followed by gradually cooling.
`The glass was polished to a mirror surface, and the
`reflectivity of the surface was measured in accordance with
`JIS Z 8722 (Measurement Method for an Object Color with
`a 2° Field of View). The measurement was carried out
`using a spectral photometer UV-2100 (Model S, with an
`integrating spherical reflector, manufactured by Shimadzu).
`The result was as shown in FIG. 1. As can be appreciated
`from FIG. 1, the decoloring effect was obvious, and
`appeared essentially pure white to the eye.
`[0019]
`EMBODIMENT 2
`Decoloring was performed through an identical method
`as in Embodiment 1, except for the addition of 3 g of zinc
`carbonate and 1.5 g of antimony oxide to 100 g of the same
`
`Japanese Unexamined Patent Application Publication H4-219340
`(4)
`
`glass powder as in Embodiment 1. For the decolored glass
`produced, the surface reflectivity was measured using the
`same method as in Embodiment 1. The result is as shown in
`FIG. 1.
`[0020]
`EMBODIMENT 3
`Decoloring was performed through an identical method
`as in Embodiment 1, except for the addition of 10 g of zinc
`carbonate and 2 g of antimony oxide to 100 g of the same
`glass powder as in Embodiment 1. For the decolored glass
`produced, the surface reflectivity was measured using the
`same method as in Embodiment 1. The result is as shown in
`FIG. 2.
`[0021]
`EMBODIMENT 4
`Decoloring was performed through an identical method
`as in Embodiment 1, except for the addition of 10 g of zinc
`carbonate and 3 g of antimony oxide to 100 g of the same
`glass powder as in Embodiment 1. For the decolored glass
`produced, the surface reflectivity was measured using the
`same method as in Embodiment 1. The result is as shown in
`FIG. 2.
`[0022]
`EMBODIMENT 5
`Decoloring was performed through an identical method
`as in Embodiment 1, except for the addition of 2 g of zinc
`carbonate and 1.5 g of antimony oxide to 100 g of the same
`glass powder as in Embodiment 1 and using the heating
`temperature of 800°C for the electric furnace. For the
`decolored glass produced, the surface reflectivity was
`measured using the same method as in Embodiment 1. The
`result is as shown in FIG. 3.
`[0023]
`EMBODIMENT 6
`Decoloring was performed through an identical method
`as in Embodiment 1, except for the addition of 5 g of zinc
`carbonate and 2 g of antimony oxide to 100 g of the same
`glass powder as in Embodiment 1 and using the heating
`temperature of 800°C for the electric furnace. For the
`decolored glass produced, the surface reflectivity was
`measured using the same method as in Embodiment 1. The
`result is as shown in FIG. 3.
`[0024]
`EMBODIMENT 7
`Decoloring was performed through an identical method
`as in Embodiment 5, except using a heating temperature of
`750°C for the electric furnace. For the decolored glass
`produced, the surface reflectivity was measured using the
`same method as in Embodiment 1. The result is as shown in
`FIG. 4.
`[0025]
`EMBODIMENT 8
`Decoloring was performed through an identical method
`as in Embodiment 6, except using a heating temperature of
`750°C for the electric furnace. For the decolored glass
`produced, the surface reflectivity was measured using the
`same method as in Embodiment 1. The result is as shown in
`FIG. 4.
`[0026]
`EMBODIMENT 9
`Decoloring was performed through an identical method
`as in Embodiment 1, except for varying the amounts of zinc
`
`O-I Glass, Inc.
`Exhibit 1036
`Page 004
`
`

`

`carbonate and of antimony oxide added to the same glass
`powder as in Embodiment 1. The relationship between the
`decoloring effect and the amounts added were investigated
`through observing visually the glass obtained as a result.
`The results are shown in FIG. 5.
`[BRIEF DESCRIPTIONS OF THE DRAWINGS]
`FIG. 1 is a diagram depicting the surface reflectivity of
`glass decolored by the decoloring method according to the
`present invention.
`FIG. 2 is a diagram depicting the surface reflectivity of
`glass decolored by the decoloring method according to the
`present invention.
`
`Japanese Unexamined Patent Application Publication H4-219340
`(5)
`
`FIG. 3 is a diagram depicting the surface reflectivity of
`glass decolored by the decoloring method according to the
`present invention.
`FIG. 4 is a diagram depicting the surface reflectivity of
`glass decolored by the decoloring method according to the
`present invention.
`FIG. 5 is a diagram depicting the relationship between
`the amount of zinc carbonate and antimony oxide added
`and the decoloring effect
`in the decoloring method
`according the present invention.
`
`[FIG. 1]
`
`[FIG. 3]
`
`[VERTICAL AXIS] Reflectivity (%)
`[HORIZONTAL AXIS] Beam Wavelength (nm)
`[IN FIGURE]
`Embodiment 1
`Embodiment 2
`Control (No decoloring agent added)
`
`[FIG. 2]
`
`[VERTICAL AXIS] Reflectivity (%)
`[HORIZONTAL AXIS] Beam Wavelength (nm)
`[IN FIGURE]
`Embodiment 5
`Embodiment 6
`Control (No decoloring agent added)
`
`[FIG. 4]
`
`[VERTICAL AXIS] Reflectivity (%)
`[HORIZONTAL AXIS] Beam Wavelength (nm)
`[IN FIGURE]
`Embodiment 3
`Embodiment 4
`Control (No decoloring agent added)
`
`[VERTICAL AXIS] Reflectivity (%)
`[HORIZONTAL AXIS] Beam Wavelength (nm)
`[IN FIGURE]
`Embodiment 7
`Embodiment 8
`Control (No decoloring agent added)
`
`O-I Glass, Inc.
`Exhibit 1036
`Page 005
`
`

`

`[FIG. 5]
`
`Japanese Unexamined Patent Application Publication H4-219340
`(6)
`
`[VERTICAL AXIS] Zinc Oxide (%)
`[HORIZONTAL AXIS] Antimony Oxide (%)
`[LEFT] Blue-Green Color
`[MIDDLE] Decolored Region
`[BOTTOM RIGHT] Pink Color
`
`O-I Glass, Inc.
`Exhibit 1036
`Page 006
`
`

`

`Japanese-English
`Technology
`Services
`
`Dr. Warren Smith
`
`27 Sandy Brook Dr.
`Durham, NH 03824
`1.603.674.2227
`Warren.Smith@Comcast.net
`
`JETS
`
`Serving the Global Technical and Legal Communities Since 1984
`
`5/27/2020
`
`CERTIFICATION OF TRANSLATION
`
`I, Dr. Warren Smith of JETS: Japanese-English Technology Services, 27 Sandy
`Brook Drive, Durham, NH 03824 hereby declare and certify:
`I am well acquainted with and knowledgeable regarding both the Japanese and
`English languages;
`I am the translator of the English translation of the document titled
`"JP4219340(A)," attached above.
`To the best of my knowledge and belief, the attached English translation is a true,
`correct, accurate and complete translation.
`I further declare and certify that all statements made herein of my own knowledge
`are true and that all statements made on information and belief are believed to be true;
`and further that these statements were made with the knowledge that willful false
`statements and the like so made are punishable by fine or imprisonment, or both, under
`18 U.S.C. § 1001.
`Pursuant to 28 U.S.C. § 1746, I declare and certify under penalty of perjury that
`the foregoing is true and correct.
`Date: 5/27/2020
`
`_____________
`Dr. Warren W. Smith
`JETS: Japanese-English Technology Services
`Durham, NH 03824
`Warren.Smith@comcast.net
`603-674-2227
`
`O-I Glass, Inc.
`Exhibit 1036
`Page 007
`
`

`

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`O—l Glass, Inc.
`Exhibit 1036
`Page 008
`
`O-I Glass, Inc.
`Exhibit 1036
`Page 008
`
`

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`
`—252—
`
`O—l Glass, Inc.
`Exhibit 1036
`Page 009
`
`O-I Glass, Inc.
`Exhibit 1036
`Page 009
`
`

`

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`
`—253—
`
`O—l Glass, Inc.
`Exhibit 1036
`Page010
`
`O-I Glass, Inc.
`Exhibit 1036
`Page 010
`
`

`

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