USRE31602E - Coated titanium dioxide pigment and a process for the production of the same - Google Patents

Coated titanium dioxide pigment and a process for the production of the same Download PDF

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Publication number
USRE31602E
USRE31602E US06/501,502 US50150283A USRE31602E US RE31602 E USRE31602 E US RE31602E US 50150283 A US50150283 A US 50150283A US RE31602 E USRE31602 E US RE31602E
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pigment
titanium dioxide
coating
slurry
dioxide pigment
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Pekka I. Makinen
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3692—Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • 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
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values

Definitions

  • the present invention relates to a titanium dioxide pigment which, in order to improve its dispersibility, is coated with an inorganic substance, and to a process for coating titanium dioxide pigment with an inorganic substance.
  • Titanium dioxide pigments are used in many fields, for example in the paint, plastics and rubber industries. The effectiveness of the pigment used depends to a large extent on how evenly the pigment particles can be dispersed into the product. It is generally known that the wetting dispersing properties of titanium dioxide pigments can be improved by depositing inorganic metal oxide and/or metal hydroxide coatings on the surface of titanium dioxide crystals. It is also known that, by treating titanium dioxide pigments with organic compounds, the dispersing properties of the pigments can be further improved. The use of the pigment determines the after-treatment which is most advantageous.
  • extrusion coating paper, cardboard, laminate or the like is coated with a thin pigmented plastic film.
  • the temperature of the molten plastic is 300°-320° C. If a titanium dioxide pigment coated with an inorganic substance is used for pigmenting plastic, the water chemically bound in the inorganic coating is released at a high temperature, whereby holes are formed in the coating film (so-called lacing phenomenon).
  • the thickness of the plastic film is 25-50 ⁇ m and its TiO 2 concentration is 10-15%.
  • the object of the present invention is to provide a titanium dioxide pigment coated with an inorganic substance, eliminating the above-mentioned disadvantages.
  • the inorganic coating used for the after-treatment of calcinated titanium dioxide pigment is so thin that the water chemically bounds in it does not cause lacing.
  • the superiority of the pigment according to the invention over inorganically uncoated pigments previously used in extrusion coating lies in its better dispersibility.
  • the rate of production can be improved by using a well dispersing pigment for the production of so-called master batches.
  • the pigment according to the present invention also provides the advantage that the same pigment can be used not only for extrusion coating but also for other applications in which titanium dioxide pigment is used for coloring plastics.
  • the inorganic metal oxide and/or metal hydroxide coating of titanium dioxide pigment produced according to the invention is very thin compared with the coatings of titanium dioxide pigment commonly used.
  • the total amount of inorganic coating must not exceed 0.5% by weight, and an advantageous addition of coating, expressed as metal oxide, is 0.05-0.5% of the weight of the pigment.
  • the inorganic coating of pigment produced according to the invention can be deposited on the surface of the pigment crystals during the after-treatment stage from any water-soluble metal compound commonly used for the production of titanium dioxide pigment, such as water-soluble compounds of aluminum, zinc, titanium, zirconium or magnesium, or mixtures of the same.
  • a suitable aluminum compound is aluminum sulfate, but aluminate solutions can also be used.
  • Zinc, magnesium and zirconium can be added in the form of sulfates, but other water-soluble compounds are also possible. Titanium can be added as titanyl sulfate or titanium tetrachloride. Inorganic coating chemicals are usually added in the form of solutions, but they can also be added as solids, as long as they are in soluble form during at least one treatment stage.
  • the process according to the invention can be applied to titanium dioxide pigments produced by any process. They can be produced by highly different processes, such as the sulfate process or the chloride process. The process can be applied to both rutile and anatase.
  • organic substance can also be used for coating titanium dioxide pigments in addition to an inorganic coating. Such substances include large-molecule fatty acids and their salts, organic silicon compounds, alcohols, polyalcohols, and amines.
  • 10 g of pigment is weighed into a tared quartz crucible which has been annealed at 600° C.
  • the crucible with the pigment is transferred into an aging oven, in which it is kept at 105° C. for 16 h, then cooled in an exsiccator, and weighed. Thereafter the pigment is kept in the aging oven at 200°, 300°, 400° and 500° C. for 2 hours in such a manner that after each heating stage the crucible with the pigment is cooled in an exsiccator and weighed.
  • the weight loss of the pigment at the different temperatures is calculated in percent of the dry weight obtained at 105° C.
  • a PVC paste is prepared by adding 37.5 g of epoxy softener and 12.5 g of organic Sn stabilizer to 1150 g of dioctyl phthalate with the aid of a Lenart laboratory mixer (LENART mikromix, type EWTH, Paul Vollrath, Cologne). The mixture of dioctyl phthalate and stabilizer is cooled, and 2400 g of polyvinyl chloride powder is added to it. The slow rotations of the Lenart mixer are used to avoid heating up the paste.
  • a black toning paste is prepared by mixing 300 g of dioctyl phthalate, 300 g of polyvinyl chloride and 15 g of coal black by means of a Lenart mixer using slow rotation. The paste must not heat up during the mixing. After an aging time of at least 24 h, the paste is passed twice through a triple-roller machine (Drais-Vollhydraulische Dreiwalzenmaschine, type DH, Grosse 3, Draiswerke GmbH, Mannheim-Waldorf).
  • a black PVC paste is prepared by mixing 3600 g of PVC paste and 205 g of a black toning paste by means of a Lenart mixer. The paste must not heat up during the mixing.
  • the dispersibility of titanium dioxide pigment in PVC paste is tested by weighing 152 g of black PVC paste, prepared as above, into a 500-ml steel decanter and by adding to it slowly 5.0 g of the titanium dioxide pigment to be tested, and by mixing it by means of a Lenart mixer (400 r/min). After the adding stage, the mixing is continued at the same rotation speed for two minutes, whereafter the speed is increased (960 r/min) and mixing is continued for one more minute. Thereafter, the paste is passed through a triple-roller machine.
  • Plastic sheets are drawn from the pastes obtained by Lenart mixing and from the triple-rolled pastes, using as an aid a polished-edged glass pane and 0.25-mm-thick steel strips on tin-coated metal sheets attached to a magnetic table.
  • the sheets are gelled at 175° C. for 3 min in an aging oven provided with a blower.
  • the degree of whiteness and the tone of the plastic sheet surfaces are measured using a HUNTERLAB COLORIMETER (type D25D-3A), manufacturer HUNTERLAB, 9529 Lee High Way, Fairfax, Va. 22030) with color measuring filters X, Y and Z.
  • the numerical value obtained with colorimeter filter Y expresses the whiteness of the sheet measured.
  • a high Y value indicates high dispersibity.
  • Expression YI calculated from the values measured using filters X, Y and Z, was used as a color index which describes the color tone of the pigment.
  • FIG. 1 depicts the weight loss of a titanium dioxide pigment coated with aluminum sulfate, in percent, as a function of the temperature
  • FIG. 2 depicts the weight loss of a titanium dioxide pigment coated with a mixture of titanyl sulfate and magnesium suflate, in percent, as a function of the temperature;
  • FIG. 3 depicts the weight loss of a titanium dioxide pigment coated with a mixture of zirconium sulfate and magnesium sulfate, in percent, as a function of the temperature;
  • FIG. 4 depicts the weight loss of a titanium dioxide pigment coated with zinc sulfate, in percent, as a function of the temperature
  • FIG. 5 depicts the weight loss of a titanium dioxide pigment coated with magnesium sulfate, in percent, as a function of the temperature.
  • the weight loss of a titanium dioxide pigment after-treated in accordance with the invention is compared with the weight loss of a titanium dioxide pigment which has not been after-treated with a metal compound.
  • a calcinated rutile titanium dioxide pigment was dry ground and dispersed in water, and the aqueous dispersion was ground in a sand grinder.
  • the concentration of TiO 2 in the sand-ground pigment slurry was 200 g/l.
  • the pigment slurry was heated to 50° C. Acidic aluminum sulfate solution was added to the slurry in an amount corresponding to 0.1% Al 2 O 3 , calculated from the amount of TiO 2 in the slurry. During this addition, the pH of the slurry dropped to 2.5. The slurry was neutralized by means of a sodium carbonate solution to a pH value of 7.5. After the neutralization, the treated titanium dioxide pigment was recovered by filtration. The filter cake was washed with water from which salts had been removed by means of an ion exchanger, 0.35% dimethyl polysiloxane, calculated from the TiO 2 , was added to the washed filter cake. The pigment was dried in an aging oven at 105° C. for 16 h and ground in a steam jet mill. An analysis of 0.10% Al 2 O 3 , calculated from the weight, was obtained from the dried and jet-ground pigment.
  • Pigments were prepared as in Example 1a, but aluminum sulfate solution was added in amounts corresponding to 0.3, 0.5 and 1.0% Al 2 O 3 , calculated from the amounts of TiO 2 in the slurry. 0.35% dimethyl polysiloxane, calculated from the TiO 2 , was added to all the pigments of the example, as in Example 1a. Analyses of 0.29, 0.49 and 0.96% Al 2 O 3 , respectively, calculated from the weight of the pigment, were obtained from the dried and jet-ground pigments.
  • Example 1d in which 1.0% Al 2 O 3 was deposited in the coating of the pigment, is a reference example.
  • FIG. 1 shows graphically the heat loss of the pigments prepared in Examples 1a-1d, as a function of the temperature. It can be seen from the figure that the heat loss of the inorganically after-treated pigments prepared in Examples 1a-1d, at different temperatures, is less than that of the reference pigment not coated with an inorganic pigment, when the Al 2 O 3 coating is 0.5% or less, calculated from the weight of the pigment.
  • Pigments were prepared as in Example 1a, but aluminum sulfate solution was added in amounts corresponding to 0.25, 0.5 and 1.0% Al 2 O 3 , calculated from the TiO 2 amount in the slurry. 0.35% dimethyl polysiloxane, calculated from the TiO 2 , was added to all the pigments of the example, as in Examples 1a-1d. Analyses of 0.23, 0.49 and 0.90% Al 2 O 3 , calculated from the weight of the pigment, were obtained from the dried and jet-ground pigments.
  • the pigments prepared in Examples 2a-2b are in accordance with the invention, whereas the pigment prepared in Example 2c, in which 1.0% Al 2 O 3 was deposited in the coating, is a reference example.
  • the dispersibility of the pigments prepared in Examples 2a-2c in PVC plastic was tested using the above-mentioned dispersibility test.
  • the reference pigment used was the same titanium dioxide pigment, not after-treated with an inorganic substance, as above. It can be observed from the results of Table 1 that the dispersibility properties of the inorganically coated pigments are considerably better than those of the reference pigment not coated with an inorganic substance.
  • Master batches containing pigment 50% by weight and polyethylene 50% by weight were made from pigments prepared according to Examples 2a-2c and polyethene.
  • the reference pigment used was the above-mentioned titanium dioxide pigment not after-treated with an inorganic substance. It was observed in connection with the preparation of the master batches that the inorganically coated pigments dispersed better in plastic than did the reference pigment, and so the production capacity could be increased when using pigments prepared according to Examples 2a-2c.
  • Dry mixtures with a TiO 2 concentration of 12.5% by weight were prepared from the master batches described above and unpigmented polyethylene. Using the dry mixtures, a trial run was carried out with an extrusion coating machine; in the trial run, paper was coated with pigmented polyethylene. In the coating trial runs, the speed the paper was 100 and 200 m/min and the amount of polyethylene coating was 10 and 20 g/m 2 .
  • the pigments according to the invention, prepared as in Examples 2a-2b are suitable for extrusion coating, but the pigment prepared according to Example 2c, in which the Al 2 O 3 concentration in the coating is 0.90% calculated from the weight of the pigment, is not suitable for extrusion coating because of lacing.
  • Pigments were prepared as in Example 1a, but, instead of aluminum sulfate solution, titanyl sulfate was added in amounts corresponding to 0.1 and 0.45% TiO 2 , calculated from the amount of TiO 2 in the slurry.
  • magnesium sulfate solution was added to both pigments of the example in an amount corresponding to 0.08% MgO, calculated from the amount of TiO 2 in the slurry. Part of the magnesium sulfate dissolves when the filter cake is washed, and so an analysis of 0.03% MgO, calculated from the weight of the pigment, was obtained from the dried and jet-ground pigment.
  • 0.35% dimethyl polysiloxane was added to each pigment of the example, as in Examples 1a-1d.
  • Pigments were prepared as in Examples 3a-3b, but, instead of titanyl sulfate solution, zirconium sulfate solution was added in amounts corresponding to 0.1 to 0.45% ZrO 2 , calculated from the amount of TiO 2 in the slurry.
  • zirconium sulfate solution was added to each pigment of the example in an amount corresponding to 0.08% MgO, calculated from the amount of TiO 2 in the slurry, as in Examples 3a-3b.
  • Dimethyl polysiloxane was also added to each pigment of the example in an amount of 0.35%, calculated from the amount of TiO 2 .
  • Analyses of 0.03% MgO and 0.10 and 0.45% ZrO 2 calculated from the weight of the pigment, were obtained from the dried and jet-ground pigments.
  • Pigments were prepared as in Example 1a, but, instead of aluminum sulfate solution, zinc sulfate solution was added in amounts corresponding to 0.1, 0.4 and 0.5% ZnO, calculated from the amount of TiO 2 in the slurry.
  • Dimethyl polysiloxane was added to all pigments of the example in an amount of 0.35%, calculated from the amount of TiO 2 .
  • Analyses of 0.10, 0.40 and 0.50 ZnO, respectively, calculated from the weight of the pigment, were obtained from the dried and jet-ground pigments.
  • Pigment was prepared as in Example 1a, but, instead of aluminum sulfate solution, magnesium sulfate solution was added in an amount corresponding to 0.2% MgO, calculated from the amount of TiO 2 in the slurry. Dimethyl polysiloxane was also added, in an amount of 0.35% as in Example 1a.
  • the pigments prepared in Examples 3-6 are all in accordance with the invention.
US06/501,502 1980-07-18 1983-06-06 Coated titanium dioxide pigment and a process for the production of the same Expired - Fee Related USRE31602E (en)

Applications Claiming Priority (2)

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FI802279 1980-07-18
FI802279A FI62130C (fi) 1980-07-18 1980-07-18 Ytbelagt titandioxidpigment och foerfarande foer framstaellning daerav

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US06/283,818 Reissue US4375989A (en) 1981-07-16 1981-07-16 Coated titanium dioxide pigment and a process for the production of the same

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EP (1) EP0044515B1 (fr)
DE (1) DE3163980D1 (fr)
FI (1) FI62130C (fr)

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US4894092A (en) 1986-06-20 1990-01-16 Mitsubishi Kinzoku Kabushiki Kaisha Process for preparing coated heat-resistant pigment
US5171631A (en) * 1990-07-19 1992-12-15 Aluminum Company Of America Spacer/extender for titanium dioxide in pigment systems for coatings
US5443811A (en) * 1990-03-01 1995-08-22 Kemira Oy Method of preparing titanium dioxide
US6544328B2 (en) * 2001-01-26 2003-04-08 Kerr-Mcgee Chemical Llc Process for preparing pigment dispersible in paints and plastics concentrates
CN114958034A (zh) * 2022-05-31 2022-08-30 龙佰禄丰钛业有限公司 一种塑料用钛白粉有机复合包覆的制备方法

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DE10002163A1 (de) 2000-01-20 2001-07-26 Mitsubishi Polyester Film Gmbh Weiße, schwerentflammbare, UV-stabile Folie aus einem kristallisierbaren Thermoplasten, Verfahren zu ihrer Herstellung und ihre Verwendung
DE10011652A1 (de) 2000-03-10 2001-09-13 Mitsubishi Polyester Film Gmbh Biaxial orientierte Polyesterfolie mit hohem Weißgrad, Verfahren zu ihrer Herstellung und ihre Verwendung
DE10251675A1 (de) 2002-11-07 2004-05-19 Mitsubishi Polyester Film Gmbh Verfahren zur Herstellung einer Thermoplastfolie unter Verwendung von Kunststoffflaschen-Recyclat
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JP5782650B2 (ja) 2009-11-18 2015-09-24 ディーエスエム アイピー アセッツ ビー．ブイ． 局所用組成物
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EP3436530A1 (fr) 2016-03-29 2019-02-06 Venator P&A Finland Oy Procédé de traitement de particules de dioxyde de titane, particule de dioxyde de titane et ses utilisations
CN110072931A (zh) * 2016-12-13 2019-07-30 科慕埃弗西有限公司 刚性单层容器
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US4540652A (en) 1983-05-24 1985-09-10 Chuiko Alexei A Material for the electrostatic data recording containing silicon and titanium oxides
US4894092A (en) 1986-06-20 1990-01-16 Mitsubishi Kinzoku Kabushiki Kaisha Process for preparing coated heat-resistant pigment
US5443811A (en) * 1990-03-01 1995-08-22 Kemira Oy Method of preparing titanium dioxide
US5171631A (en) * 1990-07-19 1992-12-15 Aluminum Company Of America Spacer/extender for titanium dioxide in pigment systems for coatings
US6544328B2 (en) * 2001-01-26 2003-04-08 Kerr-Mcgee Chemical Llc Process for preparing pigment dispersible in paints and plastics concentrates
CN114958034A (zh) * 2022-05-31 2022-08-30 龙佰禄丰钛业有限公司 一种塑料用钛白粉有机复合包覆的制备方法

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EP0044515B1 (fr) 1984-06-06
FI802279A (fi) 1982-01-19
EP0044515A1 (fr) 1982-01-27
DE3163980D1 (en) 1984-07-12
FI62130C (fi) 1982-11-10
FI62130B (fi) 1982-07-30

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