Classifications

• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09G—POLISHING COMPOSITIONS; SKI WAXES
  • C09G1/00—Polishing compositions
  • C09G1/02—Polishing compositions containing abrasives or grinding agents
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
  • C01B13/14—Methods for preparing oxides or hydroxides in general
  • C01B13/145—After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
• • 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
  • C01—INORGANIC CHEMISTRY
  • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
  • C01F7/00—Compounds of aluminium
  • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
  • C01F7/021—After-treatment of oxides or hydroxides
  • C01F7/026—Making or stabilising dispersions
• • C—CHEMISTRY; METALLURGY
  • C03—GLASS; MINERAL OR SLAG WOOL
  • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
  • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
  • C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
  • C09K3/00—Materials not provided for elsewhere
  • C09K3/14—Anti-slip materials; Abrasives
  • C09K3/1454—Abrasive powders, suspensions and pastes for polishing
  • C09K3/1463—Aqueous liquid suspensions
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2002/00—Crystal-structural characteristics
  • C01P2002/50—Solid solutions
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2006/00—Physical properties of inorganic compounds
  • C01P2006/12—Surface area
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2006/00—Physical properties of inorganic compounds
  • C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability

Definitions

• the invention provides a process for the production of low-viscosity, highly filled dispersions of pyrogenic metal oxides and metalloid oxides.
• silica and aluminium dioxide dispersions are used in polishing processes (chemical-mechanical polishing) or in the paper industry for the production of a paper coating.
• highly filled silica dispersions or dispersions of silicon-titanium mixed oxide are used for the production of shaped glass articles.
• U.S. Pat. No. 5,116,535, U.S. Pat. No. 5,246,624 and U.S. Pat. No. 6,248,144 all describe processes for the production of low-viscosity dispersions of pyrogenic silicon dioxide powder (fumed silica).
• Fumed silica powders are produced like other pyrogenic oxide powders, e.g. alumina or titanium dioxide, preferably by flame hydrolysis.
• a homogeneous mixture of a vaporous starting material of the subsequent oxide e.g. silicon tetrachloride or aluminium chloride, is burnt with hydrogen, oxygen and an inert gas using a burner in a cooled combustion chamber.
• water is produced by the reaction of hydrogen and oxygen, and in a second step, this water hydrolyses the starting material with the formation of the pyrogenic oxide.
• primary particles are initially formed, which can coalesce into aggregates as the reaction progresses.
• Aggregates here are primary particles that have fused together.
• the aggregates can cluster together further to form agglomerates.
• the agglomerates are first separated. With higher dispersing energies, larger aggregates are also converted to small aggregates.
• the content of silica powder in these processes is reduced to values of less than 40 wt. %, the effectiveness of the dispersing is reduced to such an extent that only incomplete destructuring of the silica powder takes place and larger aggregates remain in dispersion. This can lead to sedimentation or gelation of the dispersion.
• the dispersion is then adjusted to the desired solids content by dilution.
• a disadvantage of these processes is the time- and energy-intensive incorporation of the pyrogenically produced silica powder to achieve the required viscosity.
• an aqueous predispersion is divided into two partial streams, which are brought together again under high pressure.
• the particles grind one another during this process.
• the predispersion is also placed under high pressure, but the collision of the particles takes place against armoured wall regions.
• Dispersion can take place over the entire pH range, the alkaline range being preferred. If a dispersion with a high solids content in the acidic range is desired, it is advantageous to reduce the viscosity by means of suitable additives.
• the object of the invention is to provide a process for the production of finely dispersed dispersions containing pyrogenically produced metal oxides as the solid phase, which avoids the disadvantages of the prior art.
• the object is achieved by a process for the production of an aqueous dispersion of pyrogenically produced metal oxide or metalloid oxide powders with a BET surface area of between 5 and 600 m 2 /g, with a metal oxide or metalloid oxide content in the dispersion of between 5 and 25 wt. %, which comprises the following steps:
• the shear rate can be between 20000 and 30000 s ⁇ 1 .
• the process according to the invention can preferably be carried out with silica powder, alumina powder, doped silica powder, described e.g. in DE-A-19847161 or DE-A-10065028, or with silicon-aluminium mixed oxide powder, described e.g. in DE-A-4226711, DE-A-10135452, DE-A19919635 or US-A-2003/22081.
• bases and/or acids may be added to the dispersion and/or predispersion.
• bases for example ammonia, ammonium hydroxide, tetramethylammonium hydroxide, primary, secondary or tertiary organic amines, sodium hydroxide solution or potassium hydroxide solution may be used.
• acids for example phosphoric acid, sulfuric acid, hydrochloric acid, nitric acid or carboxylic acids may be used.
• cationic polymers and/or aluminium salts may be added to the dispersion and/or predispersion.
• Suitable cationic polymers may be those with at least one quaternary ammonium group, a phosphonium group, an acid adduct of a primary, secondary or tertiary amine group, polyethylene imines, polydiallylamines or polyallylamines, polyvinylamines, dicyandiamide condensates, dicyandiamide-polyamine co-condensates or polyamide-formaldehyde condensates.
• aluminium compounds in the production of silica dispersions is already described in the German patent application with application number DE10238463.0.
• a surface-active substances which is of a non-ionic, cationic, anionic or amphoteric nature.
• preservatives can also be added to the process according to the invention.
• These can, for example, be compounds that are available under the trade names Preventol® from Bayer or Acticide® from Thor.
• the viscosity of the dispersions produced was determined using a rotary rheometer from Physica, model 300, and the CC 27 measuring cup at 25° C. The viscosity value was determined at a shear rate of 10 s ⁇ 1 and 100 s ⁇ 1 .
• the particle size present in the dispersion is determined by dynamic light scattering.
• the instrument used is the Zetasizer 3000 HSa (Malvern Instruments, UK).
• the median value of the volume distribution d 50(V) is given.
• the shear rate in the process according to the invention is expressed as the peripheral speed divided by the distance between the surfaces.
• the peripheral speeds can be calculated from the speed of the rotor and the rotor diameter.
• the distance between rotor and stator is approx. 1 mm in the dispersing devices used.
• Dispersing devices used the rotor/stator machines Conti-TDS 3 and Conti-TDS 4 from Ystral are used for dispersing.
• the pH of the predispersion can be between 2 and 4.5, as a result of the acidic nature of the pyrogenically produced silica and depending on the quality of the raw materials. If desired, the pH can be adjusted to be constant throughout the different silica batches by adding acid, e.g. aqueous hydrochloric acid, or base, e.g. aqueous ammonia solution, in order to achieve a constant grinding output.
• acid e.g. aqueous hydrochloric acid
• base e.g. aqueous ammonia solution
• a pH value of the predispersion close to the isoelectric point is advantageous, since the particles to be ground can be more readily ground in this case without having to overcome reciprocal electrostatic repelling forces.
• alkaline pH values When alkaline pH values are being adjusted, it can be useful to pass through the area around pH 7 by rapid addition of the alkaline component.
• a heating of the dispersion by the high energy input is countered by a heat exchanger, which limits the temperature increase to no more than 40° C.
• the suction nozzle is closed and shearing continues at 3000 rpm for a further 10 min.
• deionised water is used to dilute to a concentration slightly higher than the desired end concentration to be able to take into account the quantities of additives still to be added.
• the pH is adjusted to 5.3 with ammonia solution. On reaching the desired pH, the remainder of the water needed is metered in to achieve the exact silica end concentration of the dispersion of 12 wt. %. Using the Conti TDS 3, homogenisation is performed for a few more minutes.
• the pH is adjusted to 5.0 with ammonia solution. More deionised water is used to adjust the concentration of the dispersion to 12 wt. % silica and, using the Conti TDS 4, homogenisation is performed for a few more minutes.
• the thorough mixing/homogenisation is additionally supported by a jetstream mixer from Ystral installed in the mixing tank.
• the pH is adjusted to 9.5 by rapidly adding ammonia solution.
• the thorough mixing/homogenisation is additionally supported by a jetstream mixer from Ystral installed in the mixing tank.
• a jetstream mixer from Ystral installed in the mixing tank.
• more deionised water is used to adjust the concentration of the dispersion to 15 wt. % silica and, using the Conti TDS 4, homogenisation is performed for a few more minutes.
• the suction nozzle is closed and the 35 wt. %-predispersion is sheared at 3000 rpm for a further 10 min (Example 14: 30 min).
• deionised water is used to dilute to a concentration slightly higher than the desired end concentration to be able to take into account the quantities of additives still to be added.
• the pH is adjusted to the desired level using sodium hydroxide or ammonia solution. On reaching the desired pH, the remainder of the water needed is metered in to achieve the exact silica end concentration.
• an aqueous aluminium chloride solution is added (10 wt. %, based on Al 2 O 3 ), so that, based on the quantity of AEROSIL® 200 used, a concentration of 0.01 mg Al 2 O 3 per m 2 silica surface area is obtained.
• the pH of the dispersion is kept at a pH of between 3.8 and 4.5 by simultaneously adding 25 wt. % sodium hydroxide solution.
• the pH is adjusted to 5.0 with the sodium hydroxide solution, the remainder of the deionised water needed is added to adjust the concentration of the dispersion to 20 wt. % and dispersing is continued for a further 5 minutes.
• 35.75 kg of deionised water are initially charged into a 60 l stainless steel mixing tank. Then, with the aid of the suction tube of the Ystral Conti-TDS 3 (stator slot: 4 mm ring and 1 mm ring) under shear conditions, 19.25 kg of AEROSIL® 200 are sucked in. Once the intake is complete, the suction nozzle is closed and the 35 wt. % predispersion is sheared at 3000 rpm for a further 10 min.
• an aqueous aluminium chloride solution is added (10 wt. %, based on Al 2 O 3 ), so that, based on the quantity of AEROSIL® 200 used, a concentration of 0.01 mg Al 2 O 3 per m 2 silica surface area is obtained.
• the pH of the dispersion is kept at a pH of between 3.8 and 4.5 by simultaneously adding 25% sodium hydroxide solution. After adding the required aluminium chloride solution, the pH is adjusted to 5.0 with the sodium hydroxide solution, the remainder of the deionised water needed is added to adjust the concentration of the dispersion to 20 wt. % and dispersing is continued for a further 5 minutes.
• Examples 1, 2, 3 and 6 show the importance of a high filling level during grinding.
• a high filling level during grinding with a rotor/stator set leads to a reduction in the viscosity of the dispersion.
• Examples 3, 4 and 6 show the importance of the shear rate for successful grinding. At a higher shear rate, even with a low concentration of the predispersion, an equivalent product, or even a product with a slightly lower viscosity, can be achieved.
• Examples 10, 11 and 12 show that, with a higher concentration of the silica, a higher viscosity is obtained.
• Examples 13, 14 and 15 show that, in addition to the shear rate and the filling level during grinding, the period of grinding and the pH of the predispersion also have an influence. A longer grinding period brings about a lower viscosity of the dispersion. A reduction from pH 4.4 to 3.5 brings about a marked reduction in viscosity for the same grinding period.
• Examples 16 and 17 show that the addition of aluminium salts clearly reduces the viscosity of dispersions containing silica.
• the viscosity of the dispersion can be reduced surprisingly markedly. This can be seen particularly clearly from Example 17.
• TAB. 1 Dispersing parameters and physico-chemical data of the silica dispersions Predispersion Predispersion Shear rate (approx.) Dispersion d 50(v) Visc. 10 s ⁇ 1 Visc. 100 s ⁇ 1 Ex. AEROSIL wt. % pH s ⁇ 1 wt.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Engineering & Computer Science (AREA)
• Life Sciences & Earth Sciences (AREA)
• Dispersion Chemistry (AREA)
• Materials Engineering (AREA)
• Geology (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Geochemistry & Mineralogy (AREA)
• Silicon Compounds (AREA)
• Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
• Oxygen, Ozone, And Oxides In General (AREA)
• Colloid Chemistry (AREA)

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• 2003
  • 2003-04-14 DE DE10317066A patent/DE10317066A1/de not_active Ceased
• 2004
  • 2004-04-01 JP JP2006504942A patent/JP4768601B2/ja not_active Expired - Lifetime
  • 2004-04-01 PL PL04725037T patent/PL1611054T3/pl unknown
  • 2004-04-01 ES ES04725037T patent/ES2353501T3/es not_active Expired - Lifetime
  • 2004-04-01 CN CN2004800093265A patent/CN1771192B/zh not_active Expired - Lifetime
  • 2004-04-01 EP EP04725037A patent/EP1611054B1/en not_active Expired - Lifetime
  • 2004-04-01 US US10/546,893 patent/US20060104881A1/en not_active Abandoned
  • 2004-04-01 AT AT04725037T patent/ATE485238T1/de active
  • 2004-04-01 DE DE602004029659T patent/DE602004029659D1/de not_active Expired - Lifetime
  • 2004-04-01 WO PCT/EP2004/003445 patent/WO2004089816A1/en not_active Ceased
• 2010
  • 2010-09-30 US US12/894,539 patent/US8529651B2/en not_active Expired - Fee Related

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