WO2014193387A1 - White inkjet ink - Google Patents
White inkjet ink Download PDFInfo
- Publication number
- WO2014193387A1 WO2014193387A1 PCT/US2013/043369 US2013043369W WO2014193387A1 WO 2014193387 A1 WO2014193387 A1 WO 2014193387A1 US 2013043369 W US2013043369 W US 2013043369W WO 2014193387 A1 WO2014193387 A1 WO 2014193387A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- white
- inkjet ink
- anionic surfactant
- white pigment
- particle size
- Prior art date
Links
- 239000002245 particle Substances 0.000 claims abstract description 88
- 239000012463 white pigment Substances 0.000 claims abstract description 51
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 27
- 239000004816 latex Substances 0.000 claims abstract description 19
- 229920000126 latex Polymers 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims description 19
- 239000000049 pigment Substances 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 14
- 230000003287 optical effect Effects 0.000 claims description 10
- 238000010296 bead milling Methods 0.000 claims description 9
- 238000007639 printing Methods 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000007641 inkjet printing Methods 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 229940088417 precipitated calcium carbonate Drugs 0.000 claims description 5
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 2
- 238000007865 diluting Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims 1
- 239000000976 ink Substances 0.000 description 36
- 239000006185 dispersion Substances 0.000 description 24
- 239000004094 surface-active agent Substances 0.000 description 10
- 238000003801 milling Methods 0.000 description 8
- 230000002776 aggregation Effects 0.000 description 7
- 238000004220 aggregation Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000002296 dynamic light scattering Methods 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 125000000129 anionic group Chemical group 0.000 description 4
- 239000011324 bead Substances 0.000 description 4
- 239000003906 humectant Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 125000006850 spacer group Chemical group 0.000 description 4
- 230000003115 biocidal effect Effects 0.000 description 3
- 239000003139 biocide Substances 0.000 description 3
- 239000006184 cosolvent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 235000001892 vitamin D2 Nutrition 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- BCMCBBGGLRIHSE-UHFFFAOYSA-N 1,3-benzoxazole Chemical class C1=CC=C2OC=NC2=C1 BCMCBBGGLRIHSE-UHFFFAOYSA-N 0.000 description 1
- ATIAIEWDRRJGSL-UHFFFAOYSA-N 1,3-bis(2-hydroxyethyl)-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(CCO)C(=O)N(CCO)C1=O ATIAIEWDRRJGSL-UHFFFAOYSA-N 0.000 description 1
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 description 1
- JYCQQPHGFMYQCF-UHFFFAOYSA-N 4-tert-Octylphenol monoethoxylate Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(OCCO)C=C1 JYCQQPHGFMYQCF-UHFFFAOYSA-N 0.000 description 1
- PIGKXHAIBGNREV-UHFFFAOYSA-N C1=CC=CC=C1C1=CC=CC=C1.C=1C=CC=CC=1C=CC1=CC=CC=C1 Chemical class C1=CC=CC=C1C1=CC=CC=C1.C=1C=CC=CC=1C=CC1=CC=CC=C1 PIGKXHAIBGNREV-UHFFFAOYSA-N 0.000 description 1
- WTKZEGDFNFYCGP-UHFFFAOYSA-N Pyrazole Chemical class C=1C=NNC=1 WTKZEGDFNFYCGP-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- -1 alumina) Chemical compound 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N benzo-alpha-pyrone Natural products C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 235000001671 coumarin Nutrition 0.000 description 1
- 150000004775 coumarins Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002462 imidazolines Chemical class 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 229920002113 octoxynol Polymers 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000010951 particle size reduction Methods 0.000 description 1
- 238000004375 physisorption Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- KBVBZJLGCBJUSU-UHFFFAOYSA-N stilbene;triazine Chemical class C1=CN=NN=C1.C=1C=CC=CC=1C=CC1=CC=CC=C1 KBVBZJLGCBJUSU-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/322—Pigment inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D121/00—Coating compositions based on unspecified rubbers
- C09D121/02—Latex
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/21—Ink jet for multi-colour printing
- B41J2/2107—Ink jet for multi-colour printing characterised by the ink properties
- B41J2/211—Mixing of inks, solvent or air prior to paper contact
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/21—Ink jet for multi-colour printing
- B41J2/2107—Ink jet for multi-colour printing characterised by the ink properties
- B41J2/2114—Ejecting specialized liquids, e.g. transparent or processing liquids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/21—Ink jet for multi-colour printing
- B41J2/2107—Ink jet for multi-colour printing characterised by the ink properties
- B41J2/2114—Ejecting specialized liquids, e.g. transparent or processing liquids
- B41J2/2117—Ejecting white liquids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
Definitions
- Inkjet printing is a non-impact printing method that utilizes electronic signals to control and direct droplets or a stream of ink to be deposited on media.
- Some commercial and industrial inkjet printers utilize fixed printheads and a moving substrate web in order to achieve high speed printing.
- Current inkjet printing technology involves forcing the ink drops through small nozzles by thermal ejection, piezoelectric pressure or oscillation onto the surface of the media. This technology has become a popular way of recording images on various media surfaces (e.g., paper), for a number of reasons, including, low printer noise, capability of high-speed recording and multicolor recording.
- Fig. 1 is a flow diagram illustrating an example of a method of making an example of a white inkjet ink
- Fig. 2 is a graph illustrating the particle size of white pigments ground with a variety of different surfactants
- Fig. 3 is a graph illustrating the pigment aggregation stability of the white pigments.
- Some water-based white inks used in inkjet printing have been found to suffer from dispersion instability. It is believed that dispersion instability may be due to aggregation and/or sedimentation of the white pigment that is used. As an example, white inks containing titanium dioxide particles may exhibit instability. The stability may be increased when titanium dioxide particles of a smaller size (e.g., sub-50 nm) are utilized; however, smaller particles may also result in an undesirable reduction in opacity of the white ink.
- a smaller size e.g., sub-50 nm
- Examples of the white inkjet ink disclosed herein exhibit stability.
- stability it is meant that the white pigment particles experience little, if any, aggregation (i.e., the particle size of the white pigment remains substantially consistent for a predetermined time) and sedimentation.
- the material system used in the white inkjet ink creates repulsion (e.g., electrostatic repulsion) between the pigment particles in the dispersion environment.
- This material system includes a low density (i.e., less than 3 g/cm 3 ) white pigment and an anionic surfactant having a molecular weight (number average) less than 10,000.
- the anionic surfactant interacts with surface group(s) (e.g., a hydroxyl group) of the white pigment in such a manner that the negatively charged anionic groups face away from the surface of the white pigment particle.
- the positioning of the negatively charged anionic groups causes the white pigment particles to repel one another, thereby avoiding agglomeration or aggregation into larger pigment specks.
- the low density of the white pigment particles is believed to contribute to the reduction in sedimentation.
- Examples of the white inkjet ink disclosed herein also exhibit a desirable white opacity (i.e., at least 50%). This percentage of opacity may be achieved by including a suitable white pigment loading as well as a latex particle.
- the latex particle affects the reflective intensity of the white inkjet ink by acting as an optical spacer.
- the latex particles act as spacers between the white pigments, facilitating a larger change in refractive index between the pigments and the latex. This leads to enhanced light scattering and higher opacity.
- the white inkjet ink disclosed herein is an aqueous based ink including the white pigment, the anionic surfactant, the latex particle, and a balance of water.
- the white inkjet ink includes no other components.
- the white inkjet ink includes additives, such as an optical brightener, a biocide, another surfactant, a co-solvent, and/or a humectant.
- Fig. 1 illustrates an example of a method 10 for making the white inkjet ink.
- the method 10 begins with a bead milling process (reference numeral 12). This process is performed in order to obtain white pigment particles having an average size that is suitable for obtaining white opacity and for achieving good jettability.
- the desired average particle size for the white pigment particles ranges from about 200 nm to about 300 nm.
- the white pigment particles Prior to bead milling, the white pigment particles may be in the form of agglomerates having an average particle size that is greater than 300 nm. In an example, the particle agglomerates may be larger than 0.5 ⁇ .
- the white pigment is selected from a class of white filler pigments that have an effective density that is less than 3 g/cm 3 . Examples of the white pigment include precipitated calcium carbonate (PCC), aluminum silicate, aluminum oxide (i.e., alumina), mica-based pigments coated with thin layer(s) of white pigment (such as TiO 2 ), or combinations thereof.
- PCC precipitated calcium carbonate
- aluminum silicate aluminum oxide
- aluminum oxide i.e., alumina
- mica-based pigments coated with thin layer(s) of white pigment such as TiO 2
- a slurry of water and the selected white pigment is prepared.
- the slurry includes about 25 wt% of the white pigment particles and a remaining balance of water.
- the slurry may contain from about 10 wt% to about 50 wt% of the white pigment particles.
- the slurry is mixed with milling media, and this mixture is added to a bead mill, an attritor, or another type of particle size reduction equipment.
- a bead mill is a UAM015 bead mill from Kotobuki Industries, Japan.
- 100 ⁇ zirconium oxide (ZrO 2 ) beads are used as the milling media.
- the ratio of the slurry to the milling media may range from about 2:3 (v/v) to about 3:1 (v/v).
- Bead milling is then accomplished using suitable conditions (e.g., speed, temperature, etc.) for a suitable time to achieve the desired reduced particle size.
- suitable conditions e.g., speed, temperature, etc.
- the speed may be about 3,000 rpm
- the temperature may range from about 10°C to about 80°C.
- milling may be
- the milling cycle is about 30 minutes.
- the number of cycles utilized may depend, at least in part, on the original size and the desirable reduced size of the white pigment particles. In an example, anywhere from one cycle to four cycles are performed. This process causes the original white pigment particles/agglomerates to deagglomerate into discrete particles. For instance, during bead milling, the impact from the milling media disintegrates the pigment agglomerates into the discrete particles, which have an average pigment particle size at or below 300 nm.
- the particle size may be monitored, e.g., via dynamic light scattering (DLS) and/or scanning electron microscopy (SEM).
- DLS dynamic light scattering
- SEM scanning electron microscopy
- the milling media is separated from the white pigment particles using, for example, a mesh sieve or some other suitable filter.
- the slurry (now including the reduced size white pigment particles) is diluted with water.
- the slurry is diluted to contain about 5 wt% of the white pigment particles.
- the diluted slurry may include anywhere from about 5 wt% to about 30 wt% of the white pigment particles.
- anionic surfactant is then selected for the white inkjet ink, as shown at reference numeral 16.
- the anionic surfactant is selected so that it interacts with the white pigment in a desirable manner. More particularly, the anionic surfactant is selected so that when the anionic surfactant is mixed with the white pigment particles, the surfactant will migrate toward the discrete pigment particles, and attach themselves onto the surfaces thereof (via physisorption and/or chemisorption). It is believed that the anionic groups of the surfactant orient themselves so that the negative charges are facing away from the pigment particle surface. It is further believed that this creates repulsive forces within the ink environment that keep the particles from agglomerating. This enables the white pigment particles to maintain a substantially constant particle size over time.
- substantially consistent particle size it is meant that the average particle size of the white pigment particles (after the reduction in size takes place and after incorporation into the inkjet ink) remains within a predetermined range or below a predetermined number for a predetermined period of time.
- the particle size stays within the range of from about 100 nm to about 250 nm.
- about 90% of the particles remain substantially consistent in size.
- the predetermined time period may be at least 3 months at ambient conditions (e.g., a temperature ranging from about 20°C to about 25°C).
- the particle size of the white pigment particles stays below 300 nm or within a range of 200 nm to 300 nm for at least 6 days.
- anionic surfactants have a molecular weight that is less than 10,000.
- anionic surfactant include a 50% active alkylphenol ethoxylate-free polymeric dispersant in water (e.g.,
- the white inkjet ink is then prepared by mixing the diluted slurry with the anionic surfactant, a latex particle, and a balance of water. This is shown at reference numeral 18 in Fig. 1 .
- the anionic surfactant, the latex particle, any other additives, and water may be added sequentially to the diluted slurry after milling to afford the final dispersion.
- the components may be added and processed via another mixing process, such ultrasonication, low-shear mixing, etc.
- the amount of anionic surfactant utilized will depend, at least in part, on the amount of white pigment particles that is utilized. In an example, the anionic surfactant is present in an amount up to 20% of an amount of the white pigment. In an example, the anionic surfactant is present in an amount up to 10% of an amount of the white pigment. In the example including 5 wt% of white pigment particles, up to 0.5 wt% of the anionic surfactant may be included.
- the latex particle enhances the opacity of the white inkjet ink by acting as an optical spacer.
- Optical spacers enhance reflective intensity, which in turn enhances the opacity.
- Suitable latex particles include polyurethane-based particles, styrene based particles, and methacrylic based latex particles.
- the average particle size of the latex particles is less than 200 nm. In an example, the average particle size of the latex particles ranges from about 100 nm to about 200 nm.
- the latex particles may be present in the white inkjet ink in an amount ranging from about 2 wt% with respect to the pigment wt% to about 50 wt% with respect to the pigment wt%. The higher amounts may be incorporated to further increase the opacity.
- the white inkjet ink may, in some examples, include other additives, such as an optical brightener.
- the optical brightener may further enhance the opacity of the ink. Examples of suitable optical brighteners include
- Suitable additives include a biocide, another surfactant, a co-solvent, and/or a humectant.
- the biocide may be used in any amount that is less than 1 wt% of the total wt% of the ink.
- the other surfactants include TERGITOLTM (The Dow Chemical Co.), ZONYL® FSO (E. I. du Pont de Nemours and Company), CRODAFOSTM (Croda International),
- the surfactant may be used in any amount that is less than 5 wt% of the total wt% of the ink.
- the co-solvent is included in addition to water, and may be used in any amount that is less than 20 wt% of the total wt% of the ink. Examples of suitable co-solvents include propanol and its variants.
- the humectant may be used in an amount that is less than 15 wt% of the total wt% of the ink.
- An example humectant is DANTOCOL® DHE (di- (2-hydroxyethyl)-5,5-dimethylhydantoin) (Lonza).
- the amount of water included makes up the balance of the ink.
- the white inkjet inks disclosed herein are printable from a thermal inkjet printhead, such as 10 ng to 40 ng thermal inkjet pens.
- the white ink may also be printed with piezoelectric printheads.
- the printing method involves jetting the white inkjet ink onto a suitable substrate, such as colored cellulose-based substrates, plastics, glass, foils, etc.
- a suitable substrate such as colored cellulose-based substrates, plastics, glass, foils, etc.
- examples of the white inkjet ink disclosed herein are capable of being thermally jetted in a reliable manner at a relatively high drop velocity, with desirable directionality and nozzle health.
- Table 1 illustrates the formulations of the various dispersions.
- the white pigment was precipitated calcium carbonate (PCC) particles in the form of a slurry.
- PCC precipitated calcium carbonate
- the average particle size of the white pigment in each of the white dispersion samples was determined by dynamic light scattering (DLS). The results are shown in Fig. 2. As illustrated, both white dispersions 2 and 5 had an average particle size of about 250 nm, while
- comparative white inks 0, 1 , 3, and 4 each had an average particle size over 300 nm.
- the dispersions were then allowed to sit for 6 days.
- the particle size was measured using DLS after 2 days, 4 days, and 6 days. These results are shown in Fig. 3.
- the particle size of the white dispersions 2 and 5 remains at about 250 nm over the time period, with very little change.
- the particle size in comparative white dispersion 0 increased by about 200 nm
- the particle size in comparative white dispersion 1 increased by about 350 nm
- the particle size in comparative dispersion 3 increased in size by about 250 nm
- the particle size in comparative dispersion 4 increased in size by about 125 nm.
- the increase in particle size in each of the comparative dispersions is indicative of pigment particle aggregation.
- both white dispersions 2 and 5 exhibited pigment aggregation stability.
- the average drop velocity was desirable (>10 m/s) for both white dispersions 2 and 5. It was also observed that these dispersions exhibited relatively good decap performance (the term "decap,” as referred to herein, means the ability of the dispersion composition to readily eject from the print head, upon prolonged exposure to air), and an absence of nozzle plate puddling with extended firing. [0033] It is to be understood that the ranges provided herein include the stated range and any value or sub-range within the stated range.
- a range from about 0.5 wt.% to about 5 wt.% should be interpreted to include not only the explicitly recited limits of about 0.5 wt.% to about 5 wt.%, but also to include individual values, such as 0.75 wt.%, 3 wt.%, 4.5 wt.%, etc., and sub-ranges, such as from about 0.8 wt.% to about 4 wt.%, etc.
- “about” is utilized to describe a value, this is meant to encompass minor variations (up to +/- 10%) from the stated value.
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
A white inkjet ink includes an anionic surfactant having a molecular weight less than 10,000, a white pigment, a latex particle, and a balance of water. The white pigment has i) a density less than 3 g/cm3, and ii) a substantially constant particle size over a predetermined time period. The substantially constant particle size ranges from about 100 nm to about 300 nm.
Description
WHITE INKJET INK
BACKGROUND
[0001 ] In addition to home and office usage, inkjet technology has been expanded to high-speed, commercial and industrial printing. Inkjet printing is a non-impact printing method that utilizes electronic signals to control and direct droplets or a stream of ink to be deposited on media. Some commercial and industrial inkjet printers utilize fixed printheads and a moving substrate web in order to achieve high speed printing. Current inkjet printing technology involves forcing the ink drops through small nozzles by thermal ejection, piezoelectric pressure or oscillation onto the surface of the media. This technology has become a popular way of recording images on various media surfaces (e.g., paper), for a number of reasons, including, low printer noise, capability of high-speed recording and multicolor recording.
BRIEF DESCRIPTION OF THE DRAWINGS
[0002] Features and advantages of examples of the present disclosure will become apparent by reference to the following detailed description and the drawings, in which like reference numerals correspond to similar, though perhaps not identical, components. For the sake of brevity, reference numerals or features having a previously described function may or may not be described in connection with other drawings in which they appear.
[0003] Fig. 1 is a flow diagram illustrating an example of a method of making an example of a white inkjet ink;
[0004] Fig. 2 is a graph illustrating the particle size of white pigments ground with a variety of different surfactants; and
[0005] Fig. 3 is a graph illustrating the pigment aggregation stability of the white pigments.
DETAILED DESCRIPTION
[0006] Some water-based white inks used in inkjet printing have been found to suffer from dispersion instability. It is believed that dispersion instability may be due to aggregation and/or sedimentation of the white pigment that is used. As an example, white inks containing titanium dioxide particles may exhibit instability. The stability may be increased when titanium dioxide particles of a smaller size (e.g., sub-50 nm) are utilized; however, smaller particles may also result in an undesirable reduction in opacity of the white ink.
[0007] Examples of the white inkjet ink disclosed herein exhibit stability. By "stability", it is meant that the white pigment particles experience little, if any, aggregation (i.e., the particle size of the white pigment remains substantially consistent for a predetermined time) and sedimentation. Without being bound to any theory, it is believed that the material system used in the white inkjet ink creates repulsion (e.g., electrostatic repulsion) between the pigment particles in the dispersion environment. This material system includes a low density (i.e., less than 3 g/cm3) white pigment and an anionic surfactant having a molecular weight (number average) less than 10,000. It is believed that the anionic surfactant interacts with surface group(s) (e.g., a hydroxyl group) of the white pigment in such a manner that the negatively charged anionic groups face away from the surface of the white pigment particle. The positioning of the negatively charged anionic groups causes the white pigment particles to repel one another, thereby avoiding agglomeration or aggregation into larger pigment specks. The low density of the white pigment particles is believed to contribute to the reduction in sedimentation.
[0008] Examples of the white inkjet ink disclosed herein also exhibit a desirable white opacity (i.e., at least 50%). This percentage of opacity may be achieved by including a suitable white pigment loading as well as a latex particle. The latex particle affects the reflective intensity of the white inkjet ink by acting as an optical spacer. The latex particles act as spacers between the white pigments, facilitating a larger change in refractive index between the pigments and the latex. This leads to enhanced light scattering and higher opacity.
[0009] The white inkjet ink disclosed herein is an aqueous based ink including the white pigment, the anionic surfactant, the latex particle, and a balance of water. In some instances, the white inkjet ink includes no other components. In other instances, the white inkjet ink includes additives, such as an optical brightener, a biocide, another surfactant, a co-solvent, and/or a humectant. The various components of examples of the white inkjet will be described further in reference to Fig. 1 , which illustrates an example of a method 10 for making the white inkjet ink.
[0010] As illustrated in Fig. 1 , the method 10 begins with a bead milling process (reference numeral 12). This process is performed in order to obtain white pigment particles having an average size that is suitable for obtaining white opacity and for achieving good jettability. In an example, the desired average particle size for the white pigment particles ranges from about 200 nm to about 300 nm.
[001 1 ] Prior to bead milling, the white pigment particles may be in the form of agglomerates having an average particle size that is greater than 300 nm. In an example, the particle agglomerates may be larger than 0.5 μιτι. The white pigment is selected from a class of white filler pigments that have an effective density that is less than 3 g/cm3. Examples of the white pigment include precipitated calcium carbonate (PCC), aluminum silicate, aluminum oxide (i.e., alumina), mica-based pigments coated with thin layer(s) of white pigment (such as TiO2), or combinations thereof.
[0012] In the bead milling process, a slurry of water and the selected white pigment is prepared. In an example, the slurry includes about 25 wt% of the white
pigment particles and a remaining balance of water. The slurry may contain from about 10 wt% to about 50 wt% of the white pigment particles.
[0013] The slurry is mixed with milling media, and this mixture is added to a bead mill, an attritor, or another type of particle size reduction equipment. One example of a bead mill is a UAM015 bead mill from Kotobuki Industries, Japan. In an example, 100 μιτι zirconium oxide (ZrO2) beads are used as the milling media. The ratio of the slurry to the milling media may range from about 2:3 (v/v) to about 3:1 (v/v).
[0014] Bead milling is then accomplished using suitable conditions (e.g., speed, temperature, etc.) for a suitable time to achieve the desired reduced particle size. In an example, the speed may be about 3,000 rpm, and the temperature may range from about 10°C to about 80°C. In one example, milling may be
accomplished for about 5 minutes to about 60 minutes per cycle. In an example, the milling cycle is about 30 minutes. The number of cycles utilized may depend, at least in part, on the original size and the desirable reduced size of the white pigment particles. In an example, anywhere from one cycle to four cycles are performed. This process causes the original white pigment particles/agglomerates to deagglomerate into discrete particles. For instance, during bead milling, the impact from the milling media disintegrates the pigment agglomerates into the discrete particles, which have an average pigment particle size at or below 300 nm.
[0015] During the bead milling process, the particle size may be monitored, e.g., via dynamic light scattering (DLS) and/or scanning electron microscopy (SEM).
[0016] After bead milling is complete, the milling media is separated from the white pigment particles using, for example, a mesh sieve or some other suitable filter.
[0017] As shown at reference numeral 14 in Fig. 1 , the slurry (now including the reduced size white pigment particles) is diluted with water. In an example, the slurry is diluted to contain about 5 wt% of the white pigment particles. The diluted
slurry may include anywhere from about 5 wt% to about 30 wt% of the white pigment particles.
[0018] An anionic surfactant is then selected for the white inkjet ink, as shown at reference numeral 16. As previously mentioned, the anionic surfactant is selected so that it interacts with the white pigment in a desirable manner. More particularly, the anionic surfactant is selected so that when the anionic surfactant is mixed with the white pigment particles, the surfactant will migrate toward the discrete pigment particles, and attach themselves onto the surfaces thereof (via physisorption and/or chemisorption). It is believed that the anionic groups of the surfactant orient themselves so that the negative charges are facing away from the pigment particle surface. It is further believed that this creates repulsive forces within the ink environment that keep the particles from agglomerating. This enables the white pigment particles to maintain a substantially constant particle size over time.
[0019] By "substantially consistent particle size", it is meant that the average particle size of the white pigment particles (after the reduction in size takes place and after incorporation into the inkjet ink) remains within a predetermined range or below a predetermined number for a predetermined period of time. In an example, the particle size stays within the range of from about 100 nm to about 250 nm. In another example, about 90% of the particles remain substantially consistent in size. The predetermined time period may be at least 3 months at ambient conditions (e.g., a temperature ranging from about 20°C to about 25°C). In still another example, after the white pigment particles are incorporated into the white inkjet ink, the particle size of the white pigment particles stays below 300 nm or within a range of 200 nm to 300 nm for at least 6 days.
[0020] Examples of suitable anionic surfactants have a molecular weight that is less than 10,000. Some particular examples of the anionic surfactant include a 50% active alkylphenol ethoxylate-free polymeric dispersant in water (e.g.,
SOLSPERSE® 46000 from Lubrizol, Ltd., United Kingdom) and sodium dodecyl sulfate (SDS).
[0021 ] Once the anionic surfactant is selected, the white inkjet ink is then prepared by mixing the diluted slurry with the anionic surfactant, a latex particle, and a balance of water. This is shown at reference numeral 18 in Fig. 1 . The anionic surfactant, the latex particle, any other additives, and water may be added sequentially to the diluted slurry after milling to afford the final dispersion.
Alternatively, the components may be added and processed via another mixing process, such ultrasonication, low-shear mixing, etc.
[0022] The amount of anionic surfactant utilized will depend, at least in part, on the amount of white pigment particles that is utilized. In an example, the anionic surfactant is present in an amount up to 20% of an amount of the white pigment. In an example, the anionic surfactant is present in an amount up to 10% of an amount of the white pigment. In the example including 5 wt% of white pigment particles, up to 0.5 wt% of the anionic surfactant may be included.
[0023] As mentioned above, the latex particle enhances the opacity of the white inkjet ink by acting as an optical spacer. Optical spacers enhance reflective intensity, which in turn enhances the opacity. Suitable latex particles include polyurethane-based particles, styrene based particles, and methacrylic based latex particles. The average particle size of the latex particles is less than 200 nm. In an example, the average particle size of the latex particles ranges from about 100 nm to about 200 nm. The latex particles may be present in the white inkjet ink in an amount ranging from about 2 wt% with respect to the pigment wt% to about 50 wt% with respect to the pigment wt%. The higher amounts may be incorporated to further increase the opacity.
[0024] The white inkjet ink may, in some examples, include other additives, such as an optical brightener. The optical brightener may further enhance the opacity of the ink. Examples of suitable optical brighteners include
benzoxazolines, biphenyl-stilbenes, triazoles, diazoles, imidazolines, coumarins, and triazine-stilbenes. The optical brightener may range from about 0.5 wt% to about 5 wt% of the total wt% of the ink.
[0025] As mentioned above, other suitable additives include a biocide, another surfactant, a co-solvent, and/or a humectant. The biocide may be used in any amount that is less than 1 wt% of the total wt% of the ink. Examples of the other surfactants include TERGITOL™ (The Dow Chemical Co.), ZONYL® FSO (E. I. du Pont de Nemours and Company), CRODAFOS™ (Croda International),
SURFYNOL® (Air Products and Chemicals). The surfactant may be used in any amount that is less than 5 wt% of the total wt% of the ink. The co-solvent is included in addition to water, and may be used in any amount that is less than 20 wt% of the total wt% of the ink. Examples of suitable co-solvents include propanol and its variants. The humectant may be used in an amount that is less than 15 wt% of the total wt% of the ink. An example humectant is DANTOCOL® DHE (di- (2-hydroxyethyl)-5,5-dimethylhydantoin) (Lonza).
[0026] The amount of water included makes up the balance of the ink.
[0027] The white inkjet inks disclosed herein are printable from a thermal inkjet printhead, such as 10 ng to 40 ng thermal inkjet pens. The white ink may also be printed with piezoelectric printheads. The printing method involves jetting the white inkjet ink onto a suitable substrate, such as colored cellulose-based substrates, plastics, glass, foils, etc. As will be illustrated in the Example section below, examples of the white inkjet ink disclosed herein are capable of being thermally jetted in a reliable manner at a relatively high drop velocity, with desirable directionality and nozzle health.
[0028] To further illustrate the present disclosure, examples are given herein. It is to be understood that these examples are provided for illustrative purposes and are not to be construed as limiting the scope of the present disclosure.
EXAMPLE
[0029] Six white milled dispersions were prepared by ball milling the white pigments in the presence of various surfactants, and then diluting with water.
Table 1 below illustrates the formulations of the various dispersions. In the
dispersion formulations, the white pigment was precipitated calcium carbonate (PCC) particles in the form of a slurry.
Table 1
* a nonionic, octylphenol ethoxylate surfactant, available from The Dow Chemical Co., Midland, Ml ** a nonionic alkyl EO/PO copolymer surfactant, available from The Dow Chemical Co., Midland, Ml *** a nonionic, 100% active polymeric dispersion, available from Lubrizol, Ltd., United Kingdom **** an anionic, 50% active polymeric dispersant in water, available from Lubrizol, Ltd., United Kingdom
[0030] After the dispersions were prepared, the average particle size of the white pigment in each of the white dispersion samples was determined by dynamic light scattering (DLS). The results are shown in Fig. 2. As illustrated, both white dispersions 2 and 5 had an average particle size of about 250 nm, while
comparative white inks 0, 1 , 3, and 4 each had an average particle size over 300 nm. The dispersions were then allowed to sit for 6 days. The particle size was measured using DLS after 2 days, 4 days, and 6 days. These results are shown in Fig. 3. As illustrated, the particle size of the white dispersions 2 and 5 remains at about 250 nm over the time period, with very little change. In contrast, the particle size in comparative white dispersion 0 increased by about 200 nm; the particle size in comparative white dispersion 1 increased by about 350 nm; the particle size in comparative dispersion 3 increased in size by about 250 nm; and the particle size
in comparative dispersion 4 increased in size by about 125 nm. The increase in particle size in each of the comparative dispersions is indicative of pigment particle aggregation. In contrast, both white dispersions 2 and 5 exhibited pigment aggregation stability.
[0031 ] The jetting performance of white dispersion samples 2 and 5 was evaluated using an HP thermal printhead. Typical firing conditions were utilized, as shown in Tables 2 and 3 below.
Table 2: Jetting Conditions/Performance for White Dispersion 2
[0032] As depicted in Tables 2 and 3, the average drop velocity was desirable (>10 m/s) for both white dispersions 2 and 5. It was also observed that these dispersions exhibited relatively good decap performance (the term "decap," as referred to herein, means the ability of the dispersion composition to readily eject from the print head, upon prolonged exposure to air), and an absence of nozzle plate puddling with extended firing.
[0033] It is to be understood that the ranges provided herein include the stated range and any value or sub-range within the stated range. For example, a range from about 0.5 wt.% to about 5 wt.% should be interpreted to include not only the explicitly recited limits of about 0.5 wt.% to about 5 wt.%, but also to include individual values, such as 0.75 wt.%, 3 wt.%, 4.5 wt.%, etc., and sub-ranges, such as from about 0.8 wt.% to about 4 wt.%, etc. Furthermore, when "about" is utilized to describe a value, this is meant to encompass minor variations (up to +/- 10%) from the stated value.
[0034] In describing and claiming the examples disclosed herein, the singular forms "a", "an", and "the" include plural referents unless the context clearly dictates otherwise.
[0035] Reference throughout the specification to "one example", "another example", "an example", and so forth, means that a particular element (e.g., feature, structure, and/or characteristic) described in connection with the example is included in at least one example described herein, and may or may not be present in other examples. In addition, it is to be understood that the described elements for any example may be combined in any suitable manner in the various examples unless the context clearly dictates otherwise.
[0036] While several examples have been described in detail, it will be apparent to those skilled in the art that the disclosed examples may be modified. Therefore, the foregoing description is to be considered non-limiting.
Claims
1 . A white inkjet ink, comprising:
an anionic surfactant having a molecular weight less than 10,000;
a white pigment having i) a density less than 3 g/cm3, and ii) a substantially constant particle size over a predetermined time period, the substantially constant particle size ranging from about 100 nm to about 300 nm;
a latex particle; and
a balance of water.
2. The white inkjet ink as defined in claim 1 wherein the predetermined time period is at least 3 months at ambient temperature.
3. The white inkjet ink as defined in claim 1 wherein the anionic surfactant is selected from a 50% active alkylphenol ethoxylate-free polymeric dispersant in water and sodium dodecyl sulfate.
4. The white inkjet ink as defined in claim 3 wherein the anionic surfactant is present in an amount up to 20% of an amount of the white pigment.
5. The white inkjet ink as defined in claim 1 wherein the white pigment is present in an amount ranging from about 5 wt% to about 30 wt% of a total wt% of the inkjet ink.
6. The white inkjet ink as defined in claim 1 wherein the white pigment is selected from precipitated calcium carbonate, aluminum silicate, aluminum oxide, a mica pigment coated with titanium dioxide, and combinations thereof.
7. The white inkjet ink as defined in claim 1 wherein an amount of the latex particle ranges from about 2 wt% with respect to white pigment wt% to about 50 wt% with respect to white pigment wt%.
8. The white inkjet ink as defined in claim 1 , further comprising an optical brightener.
9. A method of making a white inkjet ink, the method comprising:
bead milling a slurry including about 25 wt% of a white pigment having a density less than 3 g/cm3;
diluting the slurry to include about 5 wt% of the white pigment;
selecting an anionic surfactant that will interact with the white pigment such that the white pigment exhibits, in the white inkjet ink, a substantially constant particle size over a predetermined time period, the substantially constant particle size ranging from about 100 nm to about 300 nm; and
mixing the diluted slurry with the selected anionic surfactant, a latex particle, and a balance of water.
10. The method as defined in claim 9 wherein the selecting of the anionic surfactant includes selecting the anionic surfactant from a 50% active alkylphenol ethoxy late-free polymeric dispersant in water and sodium dodecyl sulfate.
1 1 . The method as defined in claim 9, further comprising increasing an opacity of the white inkjet ink by any of:
increasing an amount of the latex particle included in the white inkjet ink; or introducing an optical brightener into the white inkjet ink.
12. The method as defined in claim 9 wherein bead milling is accomplished at a predetermined speed for a predetermined time to reduce an initial size of the white pigment to the substantially constant particle size.
13. A printing method, comprising:
selecting a white inkjet ink, including:
an anionic surfactant having a molecular weight less than 10,000; a white pigment having i) a density less than 3 g/cm3, and ii) a substantially constant particle size over a predetermined time period, the substantially constant particle size ranging from about 100 nm to about 300 nm;
a latex particle; and
a balance of water; and
thermal inkjet printing the white inkjet ink onto a medium.
14. The printing method as defined in claim 13 wherein the anionic surfactant is sodium dodecyl sulfate, and wherein the printing method further comprises performing the thermal inkjet printing using a jetting condition selected from:
a voltage ranging from about 18 V to about 22 V;
a pulse width ranging from about 1 .8 s to about 2.2 s;
an energy ranging from about 1 .7 μϋ to about 2.6 μϋ; and
a temperature of about 35°C.
15. The printing method as defined in claim 13 wherein the anionic surfactant is a 50% active alkylphenol ethoxylate-free polymeric dispersant in water, and wherein the printing method further comprises performing the thermal inkjet printing using a jetting condition selected from:
a voltage ranging from about 20 V to about 22 V;
a pulse width ranging from about 1 .6 s to about 2.0 s;
an energy ranging from about 1 .9 μϋ to about 2.6 μϋ; and
a temperature of about 35°C.
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PCT/US2013/043369 WO2014193387A1 (en) | 2013-05-30 | 2013-05-30 | White inkjet ink |
US14/892,560 US9394453B2 (en) | 2013-05-30 | 2013-05-30 | White inkjet ink |
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CN108026400A (en) * | 2015-09-15 | 2018-05-11 | 惠普发展公司,有限责任合伙企业 | White ink |
EP3294819A4 (en) * | 2015-09-15 | 2018-03-21 | Hewlett-Packard Development Company, L.P. | White inks |
US10696859B2 (en) | 2015-09-15 | 2020-06-30 | Hewlett-Packard Development Company, L.P. | White inks |
CN108026400B (en) * | 2015-09-15 | 2021-12-31 | 惠普发展公司,有限责任合伙企业 | White ink |
EP3213925A3 (en) * | 2016-02-24 | 2017-09-27 | Laudert GmbH + Co. KG | Method for aligning two papers, device provided with means for executing the method and computer program comprising an implementation of the method |
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EP3004264A1 (en) | 2016-04-13 |
US9394453B2 (en) | 2016-07-19 |
US20160102217A1 (en) | 2016-04-14 |
EP3004264B1 (en) | 2020-03-04 |
CN105264024A (en) | 2016-01-20 |
CN105264024B (en) | 2017-04-26 |
EP3004264A4 (en) | 2017-01-04 |
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