US20010042493A1 - Dispersions containing pyrogenic oxides - Google Patents

Dispersions containing pyrogenic oxides Download PDF

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Publication number
US20010042493A1
US20010042493A1 US09/829,014 US82901401A US2001042493A1 US 20010042493 A1 US20010042493 A1 US 20010042493A1 US 82901401 A US82901401 A US 82901401A US 2001042493 A1 US2001042493 A1 US 2001042493A1
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Prior art keywords
dispersion
doped
oxide
pyrogenic oxide
pyrogenic
Prior art date
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Abandoned
Application number
US09/829,014
Inventor
Thomas Scharfe
Rainer Golchert
Helmut Mangold
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Evonik Operations GmbH
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Degussa GmbH
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Filing date
Publication date
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Assigned to DEGUSSA AG reassignment DEGUSSA AG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GOLCHERT, RAINER, SCHARFE, THOMAS, MANGOLD, HELMUT
Publication of US20010042493A1 publication Critical patent/US20010042493A1/en
Priority to US10/295,895 priority Critical patent/US6695907B2/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/50—Recording sheets characterised by the coating used to improve ink, dye or pigment receptivity, e.g. for ink-jet or thermal dye transfer recording
    • B41M5/52—Macromolecular coatings
    • B41M5/5218—Macromolecular coatings characterised by inorganic additives, e.g. pigments, clays
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/141—Preparation of hydrosols or aqueous dispersions
    • C01B33/1415—Preparation of hydrosols or aqueous dispersions by suspending finely divided silica in water
    • C01B33/1417—Preparation of hydrosols or aqueous dispersions by suspending finely divided silica in water an aqueous dispersion being obtained
    • 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
    • C09D17/00—Pigment pastes, e.g. for mixing in paints
    • C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
    • C09D17/007—Metal oxide

Definitions

  • the present invention is directed to dispersions, a process for preparing these dispersions and their use in the preparation of coating mixtures for inkjet media.
  • dispersions for example water-based dispersions
  • Aqueous dispersions can be used to prepare coating mixtures which are applied to paper or films.
  • the coated films may then be printed using an inkjet printer.
  • one objective is to obtain dispersions which are filled as highly as possible (high solids content) but with a low viscosity.
  • the invention provides dispersions which are characterised in that they consist of a liquid phase, preferably water, and a solid phase.
  • the solid phase consists of a pyrogenic oxide, doped using an aerosol, the BET surface area of which is between 5 and 600 m 2 /g.
  • the pyrogenic oxide preferably comprises silica prepared by the method of flame hydrolysis or flame oxidation and which has been doped with one or more doping component(s).
  • the doping component is an aluminium oxide, and doping is accomplished by the method of aerosol application, in which the amount of doped material is between 1 and 200,000 ppm and the doping component(s) are applied via a salt or a salt mixture.
  • the solid phase in the dispersion should be present in a proportion by weight between 0.001 and 80 wt. %.
  • the invention also provides a process for preparing chemical dispersions in which a pyrogenic oxide, doped using an aerosol, is introduced into a liquid, preferably water, in a proportion by weight of between 0.001 and 80 wt. %.
  • a liquid preferably water
  • 85 kg/h of SiCl 4 are evaporated, mixed with 51 Nm 3 /h of hydrogen and with 70 Nm 3 /h of a nitrogen/oxygen mixture (containing 35 vol. % O 2 , remainder N 2 ) and fed into the central tube in the burner.
  • the gas mixture flows out of a nozzle and bums in a water-cooled combustion chamber.
  • 4 Nm 3 /h of (jacket) hydrogen flows out of the jacket nozzle which surrounds the central nozzle, in order to avoid incrustations.
  • 70 Nm 3 /h of secondary air are also introduced into the combustion chamber.
  • An aerosol flows into the central tube out of an axial tube located therein.
  • the aerosol is produced by atomising a 15% aqueous AlCl 3 solution using a two-fluid nozzle.
  • An aerosol flow of 1 kg/h (aqueous salt solution) is produced in which a carrier gas stream of 16 Nm 3 /h of air conveys the aerosol through a heating section.
  • the air/aerosol gas mixture then enters the central tube from the axial tube at about 180° C.
  • the aerosol is burned together with the air/SiCl 4 mixture.
  • the reaction gases and the pyrogenically prepared silica doped with aluminium oxide are removed under suction through a cooling system, and cooled by applying a reduced pressure.
  • the solid material (doped pyrogenic oxide) is separated from the gas stream in a filter or a cyclone.
  • the doped pyrogenically prepared silica is produced as a white, finely divided powder. Adhering residues of hydrochloric acid are removed by treatment at elevated temperature with air which contains water vapour.
  • the pyrogenic silicon dioxide doped using an aerosol has the following physico-chemical characteristics: BET: 60 m 2 /g pH (4% aqu. disp.): 3.9 Compacted bulk density: 142 g/l Chloride content: 180 ppm Al 2 O 3 content 0.19 wt. % DBP absorption: 73 g/100 g
  • An aqueous dispersion is prepared with the doped pyrogenic oxide.
  • a commercially available Aerosils pyrogenically prepared silica provided by Degussa-Hüls AG/Frankfurt, OX 50 and Aerosil 90, are used as comparison examples.
  • Table 1 gives the characteristics of the oxides: TABLE 1 Physico-chemical characteristics of the doped pyrogenic oxide Doped pyrogenic oxide according to example OX 50 Aerosil 90 BET m 2 /g 60 50 90 pH (4% aqu. disp.) 3.9 3.8-4.8 3.7-4.7 Compacted bulk density 142 130 80 g/l Chloride content 180 ⁇ 250 ⁇ 250 ppm Al 2 O 3 content wt. % 0.19 ⁇ 0.08 0.05 SiO 2 content wt. % 99.8 >99.8 >99.8
  • the viscosity of the dispersions prepared in this way is measured after 2 h with a Brookfield viscometer. TABLE 2 Viscosity of the 40% aqueous dispersion
  • Doped pyrogenic Aerosil 90 oxide according not possible to prepare a 40% to example 1 OX 50 dispersion using Ultra-Turrax 5 rpm 2420 2320 >10,000 l0 rpm 1520 1320 20 rpm 970 745 50 rpm 554 372 100 rpm 370 256
  • Inkjet coating mixtures are prepared from these 40% aqueous dispersions.
  • Dispersion B is a 10% (with respect to PVA) aqueous dispersion of polyvinyl alcohol (solid, abbreviated as PVA), Mowiol 26-88 from the Clariant Co.
  • PVA polyvinyl alcohol
  • the two dispersions A and B are combined over the course of 10 minutes by stirring at 500 rpm with a dissolver disc to give a dispersion C.
  • Dispersions A and B are mixed in such a way that a ratio by weight of Aerosil (or doped pyrogenic oxide) to PVA of 100:20 is produced in subsequent dispersion C. In the case of a 40% dispersion A, this is mixed with dispersion B in the ratio by weight of 1.25:1 in order to achieve the required ratio by weight (100:20 for the solids).
  • These coating mixtures are applied to an untreated polyester film (thickness 100 micrometers) with the aid of a shaped spreading rod.
  • the wet film thickness of the coating mixture is 120 micrometers.
  • the coating is dried at 105° C. for 8 minutes. The also very good.
  • dispersions made with Aerosil OX 50 also have a relatively low viscosity, the print quality of the coating mixtures, or coatings, prepared therefrom is not acceptable.

Abstract

Dispersions of pyrogenic oxides, doped using an aerosol, are prepared by mixing the oxide with a suspending agent and milling. The dispersions can be used to prepare inkjet paper.

Description

    CROSS REFERENCE TO RELATED APPLICATIONS
  • The present application claims priority to Europen application 00107817.9 filed on Apr. 12, 2000, the subject matter of which is hereby incorporated by reference. [0001]
    • FIELD OF THE INVENTION
  • The present invention is directed to dispersions, a process for preparing these dispersions and their use in the preparation of coating mixtures for inkjet media. [0002]
    • BACKGROUND OF THE INVENTION
  • It is known that dispersions, for example water-based dispersions, can be prepared from pyrogenically prepared oxides. Aqueous dispersions can be used to prepare coating mixtures which are applied to paper or films. The coated films may then be printed using an inkjet printer. In this case, one objective is to obtain dispersions which are filled as highly as possible (high solids content) but with a low viscosity. [0003]
    • SUMMARY OF THE INVENTION
  • The invention provides dispersions which are characterised in that they consist of a liquid phase, preferably water, and a solid phase. The solid phase consists of a pyrogenic oxide, doped using an aerosol, the BET surface area of which is between 5 and 600 m[0004] 2/g. The pyrogenic oxide preferably comprises silica prepared by the method of flame hydrolysis or flame oxidation and which has been doped with one or more doping component(s). Preferably the doping component is an aluminium oxide, and doping is accomplished by the method of aerosol application, in which the amount of doped material is between 1 and 200,000 ppm and the doping component(s) are applied via a salt or a salt mixture. The solid phase in the dispersion should be present in a proportion by weight between 0.001 and 80 wt. %.
    •
  • The invention also provides a process for preparing chemical dispersions in which a pyrogenic oxide, doped using an aerosol, is introduced into a liquid, preferably water, in a proportion by weight of between 0.001 and 80 wt. %. This dispersion is then that patent, 85 kg/h of SiCl[0005] 4 are evaporated, mixed with 51 Nm3/h of hydrogen and with 70 Nm3/h of a nitrogen/oxygen mixture (containing 35 vol. % O2, remainder N2) and fed into the central tube in the burner. The gas mixture flows out of a nozzle and bums in a water-cooled combustion chamber. 4 Nm3/h of (jacket) hydrogen flows out of the jacket nozzle which surrounds the central nozzle, in order to avoid incrustations. 70 Nm3/h of secondary air are also introduced into the combustion chamber.
  • An aerosol flows into the central tube out of an axial tube located therein. The aerosol is produced by atomising a 15% aqueous AlCl[0006] 3 solution using a two-fluid nozzle. An aerosol flow of 1 kg/h (aqueous salt solution) is produced in which a carrier gas stream of 16 Nm3/h of air conveys the aerosol through a heating section. The air/aerosol gas mixture then enters the central tube from the axial tube at about 180° C. The aerosol is burned together with the air/SiCl4 mixture. The reaction gases and the pyrogenically prepared silica doped with aluminium oxide are removed under suction through a cooling system, and cooled by applying a reduced pressure. The solid material (doped pyrogenic oxide) is separated from the gas stream in a filter or a cyclone.
  • The doped pyrogenically prepared silica is produced as a white, finely divided powder. Adhering residues of hydrochloric acid are removed by treatment at elevated temperature with air which contains water vapour. The pyrogenic silicon dioxide doped using an aerosol has the following physico-chemical characteristics: [0007]
    BET: 60 m2/g
    pH (4% aqu. disp.): 3.9
    Compacted bulk density: 142 g/l
    Chloride content: 180 ppm
    Al2O3 content 0.19 wt. %
    DBP absorption: 73 g/100 g
  • An aqueous dispersion is prepared with the doped pyrogenic oxide. A commercially available Aerosils (pyrogenically prepared silica) provided by Degussa-Hüls AG/Frankfurt, OX 50 and Aerosil 90, are used as comparison examples. [0008]
  • Table 1 gives the characteristics of the oxides: [0009]
    TABLE 1
    Physico-chemical characteristics of the doped pyrogenic oxide
    Doped pyrogenic oxide
    according to example OX 50 Aerosil 90
    BET m2/g 60 50 90
    pH (4% aqu. disp.) 3.9 3.8-4.8 3.7-4.7
    Compacted bulk density 142 130 80
    g/l
    Chloride content 180 <250 <250
    ppm
    Al2O3 content wt. % 0.19 <0.08 0.05
    SiO2 content wt. % 99.8 >99.8 >99.8
  • An aqueous dispersion is prepared using these three different pyrogenic oxides. This is achieved using a rotor-stator system (Ultra-Turrax™) with a dispersion time of 30 minutes in a double-walled vessel with water cooling. It is attempted to prepare a 40% (with respect to solids) dispersion (w=0.40). This dispersion may also be prepared using other equipment, e.g., ball mills or pearl mills or various types of jet or high-pressure mills (jets of liquid directed towards each other). It is shown that it is not possible to produce a 40% dispersion with Aerosil 90 using this system because the system is too highly viscous. The viscosity of the dispersions prepared in this way (doped oxide and Aerosil OX 50) is measured after 2 h with a Brookfield viscometer. [0010]
    TABLE 2
    Viscosity of the 40% aqueous dispersion
    Doped pyrogenic Aerosil 90:
    oxide according not possible to prepare a 40%
    to example 1 OX 50 dispersion using Ultra-Turrax
    5 rpm 2420 2320 >10,000
    l0 rpm 1520 1320
    20 rpm 970 745
    50 rpm 554 372
    100 rpm 370 256
  • Inkjet coating mixtures are prepared from these 40% aqueous dispersions. Formulation for preparing an inkjet coating mixture is as follows. Two dispersions, A and B, are prepared. Dispersion A is a 40% (w=0.40 ) aqueous dispersion which contains the pyrogenic oxide (or the doped pyrogenic oxide). This is made by dispersing the pyrogenic oxide or doped oxide for 30 minutes with an Ultra-Turrax system in a water-cooled double-jacket system. [0011]
  • Dispersion B is a 10% (with respect to PVA) aqueous dispersion of polyvinyl alcohol (solid, abbreviated as PVA), Mowiol 26-88 from the Clariant Co. The two dispersions A and B are combined over the course of 10 minutes by stirring at 500 rpm with a dissolver disc to give a dispersion C. Dispersions A and B are mixed in such a way that a ratio by weight of Aerosil (or doped pyrogenic oxide) to PVA of 100:20 is produced in subsequent dispersion C. In the case of a 40% dispersion A, this is mixed with dispersion B in the ratio by weight of 1.25:1 in order to achieve the required ratio by weight (100:20 for the solids). Furthermore (if required) enough water is added to produce a 24% dispersion C, with respect to the sum of the solids (progenic oxide+ PVA). The viscosity of this dispersion C, the inkjet coating mixture, is measured after 24 h using a Brookfield viscometer. [0012]
    TABLE 3
    Viscosity of the coating mixture measured after 24 h
    Doped oxide according
    to example 1 OX 50 Aerosil 90
    Solids content of the 24 24 22.5
    coating mixture
    (pyrogenic oxide +
    PVA) wt. %
    Viscosity [mPas] 3244 685 3352
    at 100 rpm
  • (Note: In the case of preparing the coating mixture from Aerosil 90, a 30% aqueous dispersion is used initially.) [0013]
  • These coating mixtures are applied to an untreated polyester film (thickness 100 micrometers) with the aid of a shaped spreading rod. The wet film thickness of the coating mixture is 120 micrometers. The coating is dried at 105° C. for 8 minutes. The also very good. Although dispersions made with Aerosil OX 50 also have a relatively low viscosity, the print quality of the coating mixtures, or coatings, prepared therefrom is not acceptable. [0014]

Claims (18)

What is claimed is:
1. A dispersion comprising a liquid phase and a solid phase, wherein the solid phase comprises a pyrogenic oxide, and wherein said pyrogenic oxide:
a) is doped with one or more doping components; and
b) has a BET surface area of between 5 and 600 m2/g.
2. The dispersion of
claim 1
, wherein said pyrogenic oxide is silica.
3. The dispersion of
claim 1
, wherein said liquid phase is water.
4. The dispersion of any one of claims 1-3, wherein said pyrogenic oxide is prepared by the method of flame hydrolysis or flame oxidation.
5. The dispersion of any one of claims 1-3, wherein said pyrogenic oxide is doped using an aerosol.
6. The dispersion of any one of claims 1-3, wherein said pyrogenic oxide is doped with aluminum oxide.
7. The dispersion of any one of claims 1-3, wherein the amount of doped material in said pyrogenic oxide is between 1 and 200,000 ppm.
8. The dispersion of
claim 6
, wherein the amount of doped material in said pyrogenic oxide is between 1 and 200,000 ppm.
9. The dispersion of
claim 8
, wherein said doped material is applied as a salt or a salt mixture.
10. The dispersion of any one of claims 1-3, wherein the solid phase in the dispersion is present in a proportion by weight of between 0.001 and 80 wt. %.
11. The dispersion of
claim 6
, wherein the solid phase in the dispersion is present in a proportion by weight of between 0.001 and 80 wt. %.
12. A process for preparing a dispersion according to
claim 1
, comprising:
a) mixing a doped pyrogenic oxide with a liquid; and
b) milling the mixture produced in step a).
13. The process of
claim 12
, wherein said liquid is water and said pyrogenic oxide is silica.
14. The process of
claim 12
, wherein said pyrogenic oxide is present in said liquid in a proportion by weight of between 0.001 and 80 wt. %.
15. The process of
claim 12
, wherein said milling procedure is performed using an ball mill.
16. The process of
claim 12
, wherein said milling procedure is performed using a pearl mill.
17. The process of
claim 12
, wherein said milling procedure is performed using a high pressure milling mixture.
18. A coating mixture for an inkjet paper or inkjet film comprising the dispersion of
claim 1
.
US09/829,014 2000-04-12 2001-04-10 Dispersions containing pyrogenic oxides Abandoned US20010042493A1 (en)

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Application Number Priority Date Filing Date Title
EP00107817.9A EP1148026B1 (en) 2000-04-12 2000-04-12 Dispersions
EP00107817.9 2000-04-12

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US20020121156A1 (en) * 2001-02-22 2002-09-05 Degussa Ag Aqueous dispersion, process for its production and use
US20030095905A1 (en) * 2001-07-20 2003-05-22 Thomas Scharfe Pyrogenically produced aluminum-silicon mixed oxides
US20030150838A1 (en) * 2002-02-07 2003-08-14 Degussa Ag Dispersion for chemical mechanical polishing
US6676719B2 (en) 2000-12-23 2004-01-13 Degussa Ag Aqueous dispersion, a process for the preparation and the use thereof
WO2004089816A1 (en) * 2003-04-14 2004-10-21 Degussa Ag Process for the production of metal oxide and metalloid oxide dispersions
WO2006002085A1 (en) 2004-06-15 2006-01-05 W. R. Grace & Co.-Conn. Chemically assisted milling of silicas
WO2006002773A1 (en) * 2004-07-01 2006-01-12 Degussa Ag Silicon dioxide dispersion comprising polyol
US20080045411A1 (en) * 2002-12-17 2008-02-21 Degussa Ag Pyrogenic Silicon Dioxide and a Dispersion Thereof

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JP5566723B2 (en) * 2010-03-01 2014-08-06 古河電気工業株式会社 Fine particle mixture, active material aggregate, positive electrode active material, positive electrode, secondary battery, and production method thereof

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US6676719B2 (en) 2000-12-23 2004-01-13 Degussa Ag Aqueous dispersion, a process for the preparation and the use thereof
US20020121156A1 (en) * 2001-02-22 2002-09-05 Degussa Ag Aqueous dispersion, process for its production and use
US7169322B2 (en) * 2001-02-22 2007-01-30 Degussa Ag Aqueous dispersion, process for its production and use
US20030095905A1 (en) * 2001-07-20 2003-05-22 Thomas Scharfe Pyrogenically produced aluminum-silicon mixed oxides
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US6905632B2 (en) 2002-02-07 2005-06-14 Degussa Ag Dispersion for chemical mechanical polishing
US20030150838A1 (en) * 2002-02-07 2003-08-14 Degussa Ag Dispersion for chemical mechanical polishing
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US20080045411A1 (en) * 2002-12-17 2008-02-21 Degussa Ag Pyrogenic Silicon Dioxide and a Dispersion Thereof
US20060104881A1 (en) * 2003-04-14 2006-05-18 Degussa Ag Process for the produciton of metal oxide and metalloid oxide dispersions
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US20110155951A1 (en) * 2003-04-14 2011-06-30 Evonik Degussa Gmbh Process for the production of metal oxide and metalloid oxide dispersions
US8529651B2 (en) 2003-04-14 2013-09-10 Evonik Degussa Gmbh Process for the production of metal oxide and metalloid oxide dispersions
WO2006002085A1 (en) 2004-06-15 2006-01-05 W. R. Grace & Co.-Conn. Chemically assisted milling of silicas
US20110094418A1 (en) * 2004-06-15 2011-04-28 David Monroe Chapman Chemically assisted milling of silicas
US20090261309A1 (en) * 2004-07-01 2009-10-22 Degussa Ag Silicon dioxide dispersion comprising polyol
WO2006002773A1 (en) * 2004-07-01 2006-01-12 Degussa Ag Silicon dioxide dispersion comprising polyol
CN1980861B (en) * 2004-07-01 2012-08-29 赢创德固赛有限公司 Silicon dioxide dispersion comprising polyol
US8911638B2 (en) 2004-07-01 2014-12-16 Degussa Ag Silicon dioxide dispersion comprising polyol

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ZA200103011B (en) 2001-10-18
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CA2343831A1 (en) 2001-10-12
PL347019A1 (en) 2001-10-22
NO333429B1 (en) 2013-06-03
JP2002020650A (en) 2002-01-23
JP3909217B2 (en) 2007-04-25
EP1148026A1 (en) 2001-10-24
US6695907B2 (en) 2004-02-24
NO20011872D0 (en) 2001-04-11
NO20011872L (en) 2001-10-15
BR0101455A (en) 2001-12-04
EP1148026B1 (en) 2016-08-10
TW527317B (en) 2003-04-11
IL142506A0 (en) 2002-03-10
KR100459963B1 (en) 2004-12-04

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