CA2231264A1 - Method for producing coloured concrete bodies - Google Patents
Method for producing coloured concrete bodies Download PDFInfo
- Publication number
- CA2231264A1 CA2231264A1 CA002231264A CA2231264A CA2231264A1 CA 2231264 A1 CA2231264 A1 CA 2231264A1 CA 002231264 A CA002231264 A CA 002231264A CA 2231264 A CA2231264 A CA 2231264A CA 2231264 A1 CA2231264 A1 CA 2231264A1
- Authority
- CA
- Canada
- Prior art keywords
- pigment
- concrete
- pigments
- added
- coloured
- 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.)
- Abandoned
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00586—Roofing materials
- C04B2111/00594—Concrete roof tiles
Abstract
The invention relates to a method for producing coloured concrete bodies, particularly coloured concrete roof tiles, whereby pigment is added to the unprocessed concrete mix. In order to provide a method which makes possible the production of permanently coloured concrete bodies with reasonably priced pigments which are stable in outdoor exposure and are resistant to light, particularly UV, alkalis and heat, it is proposed that a cement compatible aqueous polymer dispersion in which organic pigment is dispersed be added to the unprocessed concrete mix. Suitable cement compatible polymer dispersions are aqueous polymer dispersions based on styrol and/or pure acrylate.
Phthalocyanine or China acridon pigments are particularly suitable as organic pigments.
Phthalocyanine or China acridon pigments are particularly suitable as organic pigments.
Description
CA 02231264 1998-03-0~
Description Method for producing coloured concrete bodies The invention relates to a method for producing coloured concrete bodies, particularly coloured concrete roof tiles, whereby pigment is added to the unprocessed concrete mix.
Coloured concrete bodies are used, for example, as roof tiles, pavers, slabs, etc. Normally, such concrete bodies are coloured with inorganic, preferably mineral, pigments. Iron oxides, but also chromium oxides or spinel compounds such as cobalt aluminium oxide, are used. These types of pigment have been well established for many years and have proved to be durable. However, relatively expensive inorganic pigments are needed, in particular for the production of blue shades.
Moreover, the colour intensity of these pigments is relatively low.
The purpose of this invention is to provide a method which makes it possible to produce permanently coloured concrete bodies with reasonably priced pigments which are stable in outdoor exposure and resistant to light, particularly W, alkalis and heat.
The invention serves this purpose in that a cement compatible aqueous polymer dispersion, in which organic pigment is dispersed, is added to the unprocessed concrete mix.
The unprocessed concrete mix can then be shaped into bodies and cured in the usual way.
Organic pigments were hitherto considered unsuitable for colouring concrete bodies, as is stated by A.M. Veit in his article "Proposed ways of improving coloured concrete products" in the periodical "Betonwerk + Fertigteil-Technik", volume 11/1994, pp 92 - lOo. organic pigments cannot be properly bound into the hydraulically hardening matrix.
CA 02231264 1998-03-0~
Consequently, these pigments are gradually elutriated, and the concrete body fades with time, inevitably giving rise to complaints.
However, because of their binding into a cement compatible polymer dispersion, the method as per the invention makes it possible to incorporate organic pigments permanently in the matrix of the concrete body, so that elutriation does not occur. What is crucial for the success of the method as per the invention is that a dispersion is produced which contains at least dispersed organic polymer and colouring. If the colouring is dispersed as pigment in an aqueous polymer dispersion, polymer particles are deposited on the surface of the pigment particles and ultimately surround the latter.
Hence the pigment particles are surrounded and protected by polymer particles. When the dispersion desiccates, the pigment particles are bound into the plastic matrix. This also applies to chemically bound pigment. In the case of aqueous dispersions, the dispersion is non redispersible and of high molecular weight. In other words, following desiccation of the original dispersion, a plastic results which cannot be converted back into a dispersion with the addition of more water. Hence the purpose of the invention is achieved, i.e. the production of permanently coloured concrete bodies.
Some organic pigments have a colouring power up to 20 times that of the same colour inorganic pigments. In other words, a much smaller amount of organic pigment is needed to produce the same intensity of colour.
In addition, a much greater colour intensity of the concrete body can be achieved at far lower cost than with mineral pigments.
Furthermore, shades can be achieved which are not possible with mineral pigments. As a suitable cement compatible polymer dispersion, preference is given to an aqueous polymer CA 02231264 1998-03-0~
dispersion whose polymer contains styrol and/or pure acrylate.
However, any polymer dispersion which is of high molecular weight, stable in cement and non redispersible is suitable.
The molar mass of the typical high molecular weight polymer is about 106 g/Mol.
It is advantageous for the polymer dispersion to contain 5 - 30% by weight of the organic pigment.
In order to increase the colour intensity, a wetting and/or dispersing agent can be added to the preparation; also possible are admixtures to prevent the pigment from precipitating.
It is advantageous for the polymer dispersion to be added to the unprocessed concrete mix in such a quantity that the pigmentlcement ratio is between 0.002 and 0.05.
A light-fast substance such as phthalocyanine or China acridon pigment is particularly suitable as organic pigment.
Phthalocyanine pigment in particular can be produced in various colours, from blue copper phthalocyanine to green hexadecachlorophthalocyanine.
The pigment preparation can of course also contain a blend of various organic pigments, and mineral pigment can be added if required. In the method as per the invention, it is also possible to permanently bind pigment such as carbon blac~ into concrete.
The organic colouring molecules can contain substituents which, for example, make possible a copolymerisation with the dispersion polymer, so that the organic pigment is bound chemically in the polymer chain.
The method as per the invention is explained below using four embodiments.
CA 02231264 1998-03-0~
W O 97/09284 PCT~P96/03875 Embodiment 1 50 g of copper phthalocyanine was dispersed in a dissolver for 15 minutes with 950 g of a styrol acrylate dispersion (LDM
6880, 50% proportion, Hoechst). 16.8 g of this preparation was added to an unprocessed concrete mix of 1350 g of sand with a grain size of 0 to 3 mm, 420 g of cement CEM I 42.5 R
and 135 g of water. The coloured concrete mix was shaped into a body. Following curing of the shaped body, a light blue concrete body was obtained.
Embodiment 2 300 g of copper phthalocyanine was dispersed in a dissolver for 15 minutes with 700 g of a pure acrylate dispersion (B60A, 50% proportion, Rohm & Haas). 70 g of this preparation was added to an unprocessed concrete mix of 1350 g of sand with a grain size of 0 to 3 mm, 420 g of cement CEM I 42.5 R and 120 g of water. Concrete bodies made from this mix had an intense blue colour.
Embodiment 3 100 g of China acridon pigment was dispersed in a dissolver for 15 minutes with 600 g of a styrol acrylate dispersion (LDM
6880, 50% proportion, Hoechst). 43 g of this preparation was added to an unprocessed concrete mix of 1350 g of sand with a grain size of 0 to 3 mm, 420 g of cement CEM I 42.5 R and 109 g of water. After shaping and curing, a light violet concrete body was obtained.
Embodiment 4 150 g of China acridon pigment was dispersed in a dissolver for 15 minutes with 300 g of a styrol acrylate dispersion (LDM
6880, 50% proportion, Hoechst). 63.3 g of this preparation was added to an unprocessed concrete mix of 1350 g of sand with a grain size of 0 to 3 mm, 420 g of cement CEM I 42.5 R
and 109 g of water. After shaping and curing, an intense violet concrete body was obtained.
Description Method for producing coloured concrete bodies The invention relates to a method for producing coloured concrete bodies, particularly coloured concrete roof tiles, whereby pigment is added to the unprocessed concrete mix.
Coloured concrete bodies are used, for example, as roof tiles, pavers, slabs, etc. Normally, such concrete bodies are coloured with inorganic, preferably mineral, pigments. Iron oxides, but also chromium oxides or spinel compounds such as cobalt aluminium oxide, are used. These types of pigment have been well established for many years and have proved to be durable. However, relatively expensive inorganic pigments are needed, in particular for the production of blue shades.
Moreover, the colour intensity of these pigments is relatively low.
The purpose of this invention is to provide a method which makes it possible to produce permanently coloured concrete bodies with reasonably priced pigments which are stable in outdoor exposure and resistant to light, particularly W, alkalis and heat.
The invention serves this purpose in that a cement compatible aqueous polymer dispersion, in which organic pigment is dispersed, is added to the unprocessed concrete mix.
The unprocessed concrete mix can then be shaped into bodies and cured in the usual way.
Organic pigments were hitherto considered unsuitable for colouring concrete bodies, as is stated by A.M. Veit in his article "Proposed ways of improving coloured concrete products" in the periodical "Betonwerk + Fertigteil-Technik", volume 11/1994, pp 92 - lOo. organic pigments cannot be properly bound into the hydraulically hardening matrix.
CA 02231264 1998-03-0~
Consequently, these pigments are gradually elutriated, and the concrete body fades with time, inevitably giving rise to complaints.
However, because of their binding into a cement compatible polymer dispersion, the method as per the invention makes it possible to incorporate organic pigments permanently in the matrix of the concrete body, so that elutriation does not occur. What is crucial for the success of the method as per the invention is that a dispersion is produced which contains at least dispersed organic polymer and colouring. If the colouring is dispersed as pigment in an aqueous polymer dispersion, polymer particles are deposited on the surface of the pigment particles and ultimately surround the latter.
Hence the pigment particles are surrounded and protected by polymer particles. When the dispersion desiccates, the pigment particles are bound into the plastic matrix. This also applies to chemically bound pigment. In the case of aqueous dispersions, the dispersion is non redispersible and of high molecular weight. In other words, following desiccation of the original dispersion, a plastic results which cannot be converted back into a dispersion with the addition of more water. Hence the purpose of the invention is achieved, i.e. the production of permanently coloured concrete bodies.
Some organic pigments have a colouring power up to 20 times that of the same colour inorganic pigments. In other words, a much smaller amount of organic pigment is needed to produce the same intensity of colour.
In addition, a much greater colour intensity of the concrete body can be achieved at far lower cost than with mineral pigments.
Furthermore, shades can be achieved which are not possible with mineral pigments. As a suitable cement compatible polymer dispersion, preference is given to an aqueous polymer CA 02231264 1998-03-0~
dispersion whose polymer contains styrol and/or pure acrylate.
However, any polymer dispersion which is of high molecular weight, stable in cement and non redispersible is suitable.
The molar mass of the typical high molecular weight polymer is about 106 g/Mol.
It is advantageous for the polymer dispersion to contain 5 - 30% by weight of the organic pigment.
In order to increase the colour intensity, a wetting and/or dispersing agent can be added to the preparation; also possible are admixtures to prevent the pigment from precipitating.
It is advantageous for the polymer dispersion to be added to the unprocessed concrete mix in such a quantity that the pigmentlcement ratio is between 0.002 and 0.05.
A light-fast substance such as phthalocyanine or China acridon pigment is particularly suitable as organic pigment.
Phthalocyanine pigment in particular can be produced in various colours, from blue copper phthalocyanine to green hexadecachlorophthalocyanine.
The pigment preparation can of course also contain a blend of various organic pigments, and mineral pigment can be added if required. In the method as per the invention, it is also possible to permanently bind pigment such as carbon blac~ into concrete.
The organic colouring molecules can contain substituents which, for example, make possible a copolymerisation with the dispersion polymer, so that the organic pigment is bound chemically in the polymer chain.
The method as per the invention is explained below using four embodiments.
CA 02231264 1998-03-0~
W O 97/09284 PCT~P96/03875 Embodiment 1 50 g of copper phthalocyanine was dispersed in a dissolver for 15 minutes with 950 g of a styrol acrylate dispersion (LDM
6880, 50% proportion, Hoechst). 16.8 g of this preparation was added to an unprocessed concrete mix of 1350 g of sand with a grain size of 0 to 3 mm, 420 g of cement CEM I 42.5 R
and 135 g of water. The coloured concrete mix was shaped into a body. Following curing of the shaped body, a light blue concrete body was obtained.
Embodiment 2 300 g of copper phthalocyanine was dispersed in a dissolver for 15 minutes with 700 g of a pure acrylate dispersion (B60A, 50% proportion, Rohm & Haas). 70 g of this preparation was added to an unprocessed concrete mix of 1350 g of sand with a grain size of 0 to 3 mm, 420 g of cement CEM I 42.5 R and 120 g of water. Concrete bodies made from this mix had an intense blue colour.
Embodiment 3 100 g of China acridon pigment was dispersed in a dissolver for 15 minutes with 600 g of a styrol acrylate dispersion (LDM
6880, 50% proportion, Hoechst). 43 g of this preparation was added to an unprocessed concrete mix of 1350 g of sand with a grain size of 0 to 3 mm, 420 g of cement CEM I 42.5 R and 109 g of water. After shaping and curing, a light violet concrete body was obtained.
Embodiment 4 150 g of China acridon pigment was dispersed in a dissolver for 15 minutes with 300 g of a styrol acrylate dispersion (LDM
6880, 50% proportion, Hoechst). 63.3 g of this preparation was added to an unprocessed concrete mix of 1350 g of sand with a grain size of 0 to 3 mm, 420 g of cement CEM I 42.5 R
and 109 g of water. After shaping and curing, an intense violet concrete body was obtained.
Claims (8)
1. Method for producing coloured concrete bodies, particularly coloured roof tiles, whereby pigment is added to the unprocessed concrete mix, characterised in that a cement compatible aqueous polymer dispersion is added in which an organic pigment is dispersed.
2. Method as in claim 1, characterised in that the polymer of the polymer dispersion contains styrol and/or pure acrylate.
3. Method as in claim 1 or 2, characterised in that the polymer dispersion contains 5 - 30% by weight of the organic pigment.
4. Method as in one of claims 1 to 3, characterised in that the polymer dispersion contains a wetting and/or dispersing agent.
5. Method as in one of claims 1 to 4, characterised in that the ratio of the pigment to cement in the unprocessed concrete mix is between 0.002 and 0.05.
6. Method as in one of claims 1 to 5, characterised in that the organic pigment is a phthalocyanine pigment.
7. Method as in one of claims 1 to 6, characterised in that the organic pigment is a China acridon pigment.
8. Method as in one of claims 1 to 7, characterised in that the organic pigment is chemically bound in the polymer chain.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19533081.1 | 1995-09-07 | ||
| DE19533081A DE19533081C2 (en) | 1995-09-07 | 1995-09-07 | Process for the production of colored concrete bodies |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2231264A1 true CA2231264A1 (en) | 1997-03-13 |
Family
ID=7771522
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002231264A Abandoned CA2231264A1 (en) | 1995-09-07 | 1996-09-04 | Method for producing coloured concrete bodies |
Country Status (19)
| Country | Link |
|---|---|
| US (2) | US6090329A (en) |
| EP (1) | EP0848691B1 (en) |
| JP (1) | JP3263398B2 (en) |
| CN (1) | CN1092159C (en) |
| AT (1) | ATE188197T1 (en) |
| AU (1) | AU695856B2 (en) |
| BR (1) | BR9610124A (en) |
| CA (1) | CA2231264A1 (en) |
| DE (2) | DE19533081C2 (en) |
| DK (1) | DK0848691T3 (en) |
| ES (1) | ES2142609T3 (en) |
| GR (1) | GR3032756T3 (en) |
| HU (1) | HUP9901178A2 (en) |
| MY (1) | MY118355A (en) |
| NO (1) | NO980977L (en) |
| NZ (1) | NZ318392A (en) |
| PL (1) | PL187414B1 (en) |
| PT (1) | PT848691E (en) |
| WO (1) | WO1997009284A1 (en) |
Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19533081C2 (en) * | 1995-09-07 | 1998-11-26 | Braas Gmbh | Process for the production of colored concrete bodies |
| CA2263667C (en) * | 1999-03-15 | 2002-02-26 | Axel J. Societe En Commandite | Processes for manufacturing pigment granules used in the colouring of concrete |
| DE60027460T2 (en) * | 1999-12-03 | 2006-10-12 | Sun Chemical Corp. | ORGANIC PIGMENT DISPERSION FOR STAINING BUILDING MATERIALS |
| KR20010057252A (en) * | 1999-12-21 | 2001-07-04 | 최철 | A coloring composition having a good compatibility with cement |
| CA2389885A1 (en) * | 2002-06-19 | 2003-12-19 | Smart Landscape Colors Inc. | Process of colouring concrete with syringe-type metering system for liquid colours |
| US20040121082A1 (en) * | 2002-10-22 | 2004-06-24 | Jack Dunnous | Method and apparatus for producing multi-color concrete |
| US7241500B2 (en) | 2003-10-06 | 2007-07-10 | Certainteed Corporation | Colored roofing granules with increased solar heat reflectance, solar heat-reflective shingles, and process for producing same |
| US7815728B2 (en) * | 2008-05-02 | 2010-10-19 | L. M. Scofield Company | High SRI cementitious systems for colored concrete |
| DE102010003999A1 (en) | 2009-05-12 | 2011-01-05 | Harold Scholz & Co. Gmbh | New pigment systems for coloring cementitious systems, in particular concrete |
| CA2808378A1 (en) | 2009-08-20 | 2011-02-24 | Certain Teed Corporation | Roofing granules, roofing products including such granules, and process for preparing same |
| US8637116B2 (en) * | 2009-08-20 | 2014-01-28 | Certainteed Corporation | Process for preparing roofing granules comprising organic colorant, with improved luster, and roofing products including such granules |
| US20130266370A1 (en) * | 2012-03-16 | 2013-10-10 | Intecrete, Llc | Multi-layered cement compositions containing photocatalyst particles and method for creating multi-layered cement compositions containing photocatalyst particles |
| CN107903787A (en) * | 2017-12-15 | 2018-04-13 | 苏州金润新材料科技有限公司 | A kind of concrete penetrating colorants and its application |
| CN111039582B (en) * | 2019-12-19 | 2021-10-22 | 深圳市点绿科技有限公司 | Preparation method of yellow rust purple quartz sand |
Family Cites Families (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2315400C2 (en) * | 1973-03-28 | 1982-09-16 | Hoechst Ag, 6000 Frankfurt | Method of coloring mineral granular material |
| JPS5943437B2 (en) * | 1981-06-16 | 1984-10-22 | 成雄 安藤 | Method for producing cementitious molded product with protective covering layer |
| NL8105814A (en) * | 1981-12-23 | 1983-07-18 | Anjap Nv | Granulate particles with coloured layer of synthetic resin - compatible with heat hardening resin. esp. for flooring |
| US4548968A (en) * | 1983-04-06 | 1985-10-22 | Ciba Geigy Corporation | Manufacture of resin extended pigments |
| GB2164288B (en) * | 1984-09-12 | 1988-06-02 | Redland Roof Tiles Ltd | Method and apparatus for manufacturing roof tiles and tiles made thereby |
| US5223200A (en) * | 1985-06-26 | 1993-06-29 | Braas Gmbh | Method for producing concrete roof tiles |
| DE3619363A1 (en) * | 1986-06-09 | 1987-12-10 | Brockhues Chem Werke Ag | METHOD FOR COLORING CONCRETE |
| JP2610980B2 (en) * | 1987-12-30 | 1997-05-14 | トーメンコンストラクション株式会社 | Compounds for the production of heavy concrete and methods for producing heavy concrete |
| JP2626016B2 (en) * | 1987-12-30 | 1997-07-02 | トーメンコンストラクション株式会社 | Compounds for the production of heavy concrete and methods for producing heavy concrete |
| CA2047787A1 (en) * | 1991-07-24 | 1993-01-25 | Z. Grant Kafarowski | Decorative concrete slab |
| DE4212768A1 (en) * | 1992-04-16 | 1993-10-21 | Huels Chemische Werke Ag | Process for the preparation of aqueous polymer dispersions |
| JPH0657148A (en) * | 1992-08-11 | 1994-03-01 | Sumika Color Kk | Surface course material for colored pavement and its production |
| US5401313A (en) * | 1993-02-10 | 1995-03-28 | Harcros Pigments, Inc. | Surface modified particles and method of making the same |
| US5298076A (en) * | 1993-03-23 | 1994-03-29 | Ciba-Geigy Corporation | Carbazole dioxazine-pigmented plastics and coatings |
| US5406766A (en) * | 1993-07-29 | 1995-04-18 | Monier Roof Tile Inc. | Multi-color concrete tiles and method and apparatus for making same |
| DE4419574A1 (en) * | 1994-06-03 | 1995-12-07 | Bayer Ag | Coating materials for waterproofing building materials, etc. |
| DE19533081C2 (en) * | 1995-09-07 | 1998-11-26 | Braas Gmbh | Process for the production of colored concrete bodies |
-
1995
- 1995-09-07 DE DE19533081A patent/DE19533081C2/en not_active Expired - Fee Related
-
1996
- 1996-09-04 BR BR9610124A patent/BR9610124A/en not_active IP Right Cessation
- 1996-09-04 AT AT96931014T patent/ATE188197T1/en not_active IP Right Cessation
- 1996-09-04 EP EP96931014A patent/EP0848691B1/en not_active Expired - Lifetime
- 1996-09-04 CN CN96196680A patent/CN1092159C/en not_active Expired - Fee Related
- 1996-09-04 NZ NZ318392A patent/NZ318392A/en unknown
- 1996-09-04 PL PL96325238A patent/PL187414B1/en not_active IP Right Cessation
- 1996-09-04 HU HU9901178A patent/HUP9901178A2/en unknown
- 1996-09-04 ES ES96931014T patent/ES2142609T3/en not_active Expired - Lifetime
- 1996-09-04 AU AU69868/96A patent/AU695856B2/en not_active Ceased
- 1996-09-04 PT PT96931014T patent/PT848691E/en unknown
- 1996-09-04 JP JP51086097A patent/JP3263398B2/en not_active Expired - Fee Related
- 1996-09-04 DK DK96931014T patent/DK0848691T3/en active
- 1996-09-04 DE DE69605930T patent/DE69605930T2/en not_active Expired - Fee Related
- 1996-09-04 WO PCT/EP1996/003875 patent/WO1997009284A1/en active IP Right Grant
- 1996-09-04 CA CA002231264A patent/CA2231264A1/en not_active Abandoned
- 1996-09-06 MY MYPI96003692A patent/MY118355A/en unknown
-
1998
- 1998-03-06 NO NO980977A patent/NO980977L/en not_active Application Discontinuation
- 1998-03-06 US US09/036,463 patent/US6090329A/en not_active Expired - Fee Related
-
2000
- 2000-02-14 US US09/503,672 patent/US6268410B1/en not_active Expired - Fee Related
- 2000-02-24 GR GR20000400456T patent/GR3032756T3/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| PL187414B1 (en) | 2004-07-30 |
| DE69605930T2 (en) | 2001-04-26 |
| HUP9901178A2 (en) | 1999-08-30 |
| WO1997009284A1 (en) | 1997-03-13 |
| EP0848691A1 (en) | 1998-06-24 |
| NO980977D0 (en) | 1998-03-06 |
| US6090329A (en) | 2000-07-18 |
| US6268410B1 (en) | 2001-07-31 |
| CN1195335A (en) | 1998-10-07 |
| EP0848691B1 (en) | 1999-12-29 |
| NZ318392A (en) | 1998-09-24 |
| AU695856B2 (en) | 1998-08-27 |
| CN1092159C (en) | 2002-10-09 |
| JPH11510139A (en) | 1999-09-07 |
| AU6986896A (en) | 1997-03-27 |
| PL325238A1 (en) | 1998-07-06 |
| ES2142609T3 (en) | 2000-04-16 |
| DE19533081C2 (en) | 1998-11-26 |
| NO980977L (en) | 1998-03-06 |
| JP3263398B2 (en) | 2002-03-04 |
| ATE188197T1 (en) | 2000-01-15 |
| GR3032756T3 (en) | 2000-06-30 |
| BR9610124A (en) | 1999-05-04 |
| PT848691E (en) | 2000-06-30 |
| MY118355A (en) | 2004-10-30 |
| DK0848691T3 (en) | 2000-05-15 |
| DE19533081A1 (en) | 1997-03-13 |
| DE69605930D1 (en) | 2000-02-03 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| FZDE | Discontinued |