US20070261604A1 - Yellow iron oxide pigments - Google Patents

Yellow iron oxide pigments Download PDF

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Publication number
US20070261604A1
US20070261604A1 US11/800,404 US80040407A US2007261604A1 US 20070261604 A1 US20070261604 A1 US 20070261604A1 US 80040407 A US80040407 A US 80040407A US 2007261604 A1 US2007261604 A1 US 2007261604A1
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Prior art keywords
iron oxide
yellow iron
oxide pigment
din
value
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Abandoned
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US11/800,404
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English (en)
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Carsten Rosenhahn
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Lanxess Deutschland GmbH
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Lanxess Deutschland GmbH
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Assigned to LANXESS DEUTSCHLAND GMBH reassignment LANXESS DEUTSCHLAND GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ROSENHAHN, CARSTEN
Publication of US20070261604A1 publication Critical patent/US20070261604A1/en
Priority to US12/194,580 priority Critical patent/US7799125B2/en
Abandoned legal-status Critical Current

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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
    • C09C1/22—Compounds of iron
    • C09C1/24—Oxides of iron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/30—Oxides other than silica
    • C04B14/308—Iron oxide
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • 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
    • 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
    • C01P2006/63—Optical properties, e.g. expressed in CIELAB-values a* (red-green axis)
    • 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
    • C01P2006/64—Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)
    • 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
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals

Definitions

  • the present invention relates to improved yellow iron oxide pigments and to their use.
  • the precipitation process and also the Penniman-Zoph process of producing yellow iron oxide pigments have been known for a long time.
  • the typical course of these processes is described by way of example in Ullmann's Encyclopaedia of Industrial Chemistry, 5th Ed., Vol. A20, p. 297 ff., or in U.S. Pat. No. 1,327,061 A1 and U.S. Pat. No. 1,368,748 A1 and DE 3907910 A1.
  • the raw material and electrolyte catalyst used is commonly iron(II) sulphate, which is obtained in the pickling of steel sheets or in the production of titanium dioxide by the sulphate process.
  • a further possibility is the use of iron(II) sulphate from the production of low-alloy steel residues in the form of sheets, wire rolls, Fe powder with sulphuric acid.
  • ⁇ -FeOOH yellow iron oxide
  • ⁇ -FeOOH yellow iron oxide
  • the precipitation process DE 2 455 158 A1
  • the Penniman process U.S. Pat. No. 1,368,748 A1, U.S. Pat. No. 1,327,061 A1
  • a nucleus is produced first of all, onto which then, in a further step, relatively slowly, additional ⁇ -FeOOH is caused to grow.
  • the yellow iron oxide pigments produced by these processes are notable for a bright, yellow colour, but have an oil absorption value the end user finds unfavourable.
  • the oil absorption value is determined in accordance with DIN 53199, which dates from 1973. With the aid of the oil absorption value the practitioner is able to estimate the binder demand of a pigment. The higher the oil absorption value, the higher, too, the binder demand. The oil absorption value also, moreover, permits conclusions concerning the level of the pigment-volume concentration to be expected.
  • a pigment with a lower oil absorption value can be processed in a more eco-friendly manner, thereby simplifying the process and lowering the energy consumption for the end user.
  • Low oil absorption in oxides allows the user, especially in the paint industry, to use a composition having a greater amount of oxide and a lower level of additives in order to achieve the desired quality for the product.
  • the higher pigment-volume concentration permits a greater colour density in paste production, which in turn is beneficial to the specific transport costs of the pigment pastes.
  • a high colour strength additionally boosts the desired effects for the end user.
  • the yellow iron oxide pigment has, for example, a dispersibility to EN 21524/DIN ISO 1524 (2002) in the extended “3-box method” form of better than 30-50-70.
  • the yellow iron oxide pigment has, for example, a water absorption value ⁇ 50.
  • the yellow iron oxide pigment has, for example, a BET >14.
  • the yellow iron oxide pigment has, for example, a bulk density >0.4.
  • the yellow iron oxide pigment has, for example, a tamped density >0.7.
  • the high bulk density and tamped density not only makes it easier to produce the formula but also has consequences for the transport costs and storage costs.
  • the yellow iron oxide pigment has, for example, a viscosity in MAP ⁇ 25 against Bayferrox® 3910.
  • the process of producing the yellow iron oxide pigments is divided into two parts: nucleus preparation and pigment preparation.
  • the iron oxide nucleus is prepared from an iron sulphate solution by addition of aqueous sodium hydroxide solution with air oxidation. This gives FeOOH in the form of microcrystals (nucleus).
  • the nucleus prepared in the first process step is built up to a crystal by addition of iron scrap, with oxidation by atmospheric oxygen.
  • the product is washed salt-free, so that the conductivity of the washing water which runs off is no more than 2 mS/cm.
  • the conductivity of the washing water which runs off is no more than 2 mS/cm.
  • an iron oxide paste having a moisture content of 50%. After that the product is dried and ground.
  • the invention also embraces the use of the yellow iron oxide pigment for colouring organic or inorganic dispersions, products of the ink, paint, coating, building-material, plastics and paper industry, in foods, and in products of the pharmaceutical industry such as tablets.
  • the pigment was prepared using the Muller in a non-drying test binder.
  • the test binder (paste) is composed of two components for the white reduction; for the full shade only component 1 is used:
  • SACOLYD® L640 (Krems Chemie AG, AU, alkyd resin binder based on linseed oil and phthalic anhydride) (formerly ALKYDAL® L64 (Bayer AG, DE)). It corresponds to the specifications given in standards DIN EN ISO 787-24 (October 1995), ISO 787-25: 1993 and DIN 55983 (December 1983) as requirements of a test binder for colour pigments.
  • LUVOTHIX® HT Lehmann & Voss & Co., DE, pulverulent, modified, hydrogenated castor oil
  • LUVOTHIX® HT Lehmann & Voss & Co., DE, pulverulent, modified, hydrogenated castor oil
  • Component 2 was dissolved in component 1 at 75-95° C.
  • the cooled, compact material was passed once through a triple-roll mill. With this step the L64 paste was complete.
  • a plate type paint dispersing machine (muller) was used, of the kind described in DIN EN ISO 8780-5 (April 1995).
  • the apparatus employed was an Engelsmann Jel 25/53 muller with an effective plate diameter of 24 cm.
  • the speed of the bottom plate was approximately 75 min ⁇ 1 .
  • the force between the plates was set at about 0.5 kN by insertion of a 2.5 kg loading weight suspended from the loading bracket.
  • the reductant used was a commercially customary titanium dioxide pigment, TRONOX® R-KB-2, Kerr-McGee Corp., US) (formerly BAYERTITAN® R-KB-2 (Bayer AG, DE)).
  • R-KB-2 corresponds in its composition to type R 2 in ISO 591-1977.
  • 0.4 g of test pigment, 2.0 g of TRONOX® R-KB-2 and 3.0 g of paste were dispersed in five stages of 25 revolutions each by the method described in DIN EN ISO 8780-5 (April 1995) section 8.1.
  • 1 g of test pigment is dispersed in 3 g of component 1 in five stages each of 25 revolutions in accordance with the method described in DIN EN ISO 8780-5 (April 1995) section 8.1.
  • the pigment paste mixture was subsequently spread into a paste plate corresponding in its function to the paste plate in DIN 55983 (December 1983).
  • the doctor blade associated with the paste plate is drawn over the indentation in the plate that is filled with the pigment paste mixture, to produce a smooth surface.
  • the doctor blade is moved in one direction with a speed of about 3-7 cm/s.
  • the smooth surface is measured within a few minutes.
  • a spectrophotometer (“calorimeter”) having the d/8 measuring geometry without a gloss trap was used. This measuring geometry is described in ISO 7724/2-1984 (E), section 4.1.1, in DIN 5033 part 7 (July 1983), section 3.2.4 and in DIN 53236 (January 1983), section 7.1.1.
  • a DATAFLASH® 2000 measuring instrument (Datacolor International Corp., USA) was employed.
  • the calorimeter was calibrated against a white ceramic working standard, as described in ISO 7724/2-1984 (E) section 8.3.
  • the reflection data of the working standard against an ideally matt-white body are deposited in the colorimeter so that, after calibration with the white working standard, all coloured measurements are related to the ideally matt-white body.
  • the black-point calibration was carried out using a hollow black body from the colorimeter manufacturer.
  • the result of the colorimetry is a reflection spectrum.
  • the illuminant used to take the measurement is unimportant (except in the case of fluorescent samples).
  • From the reflection spectrum it is possible to calculate any desired calorimetric parameter.
  • the calorimetric parameters used in this case are calculated in accordance with DIN 6174 (CIELAB values).
  • the temperature of colorimeter and test specimen was approximately 25° C. ⁇ 5° C.
  • the colour coordinates are stated in accordance with the measurement described above to DIN 6174 (CIELAB values).
  • the measurement in the white reduction also results in the colour strength of the colour pigment measured (see Table 1).
  • the so-called “reduction ratio” was calculated.
  • the reduction ratio was determined in accordance with DIN standard 53235 part 1 and part 2 from 1974 for the standard depth of shade B 1/9.
  • the reduction ratio indicates the ratio of a colour-imparting substance to a mixing component (in the present case: TiO 2 ) with which a defined depth of shade (depth of colouring) in accordance with DIN standard 53235 part 1 and part 2 from 1974 is achieved.
  • a high reduction ratio means that the same depth of colouring can be achieved with less pigment. Such a pigment is therefore more strongly coloured in practical application.
  • the “3-box” method employed for testing the pigments is an extended form of reading off, in which three values are reported as the result.
  • the main region in the form of a close coherent array of bits; above it a region with a moderately high concentration of bits; and finally, over that, a region with a very low concentration of bits (individual bits, virtually, but appearing reproducibly) ( FIG. 2 ). Therefore of a trio of values is recorded that characterizes the upper limits of the three regions indicated.
  • a grindometer spread according to FIG. 2 is assessed, accordingly, as follows: ⁇ 10/25/35 ⁇ m.
  • the water absorption value was determined in accordance with DIN 55608 (June 2000).
  • the bulk density was determined for the finished material without further treatment of the product, from the ratio of mass to volume.
  • the tamped density was determined in accordance with ISO 787 part 11 (1995).
  • the stirring shaft and inner wall of the beaker are cleaned to remove particles of pigment that have not been wetted.
  • the stirrer is switched off briefly and lifted from the sample beaker.
  • the walls of the beaker are cleaned with a spatula. Then the stirrer is lowered again and restarted.
  • the distance of the toothed disc from the base is approximately 10 mm.
  • the speed is increased to 3000 ⁇ 100 min ⁇ 1 .
  • the time of dispersing at this speed is 15 minutes.
  • the paste is adjusted to a pH of 8.5 ⁇ 0.5 by addition of 10% strength sodium hydroxide solution (quantity approximately 3-6 ml); the pH must in no case fall below 7.5. It is necessary to check the pH a number of times within the dispersing time, since the pH value is subject to creeping variation.
  • the poly beaker is sealed with a lid and cooled in a water bath at 20° C. for 30 minutes.
  • the viscosity standard must in each case be prepared in parallel.
  • the paste should be stirred briefly with a spatula prior to measurement.
  • the paddle stirrer of a commercially available standard Krebs-Stormer viscosimeter should be introduced to the point where the marking on the shaft can still just be seen. The result reported is the value which no longer shows any change over about 1 minute. The paddle stirrer is cleaned after each measurement.
  • Equipment open stirring kettle with a capacity of 65 m 3 , nozzle introduction of air, circulation pump and a mechanical stirrer.
  • the reactor is charged with 27.0 m 3 of plant water and 0.47 t (11.7 m 3 ) of iron sulphate heptahydrate (FeSO 4 .7H 2 O). After the circulation pump and stirrer have been switched on, 667 kg (9.532 l) of dissolved sodium hydroxide (NaOH+H 2 O) are added. Thereafter the air feed is commenced. The air feed takes place, for example, with a throughput of 250 ⁇ 200 m 3 /h or, for example at 170 ⁇ 85 m 3 /h. The volume is made up with industrial water.
  • the monitored parameters are as follows:
  • the nucleus was pumped into the reactor and the volume was made up to 110 m 3 with water.
  • the iron sulphate heptahydrate (FeSO 4 .7H 2 O) concentration was adjusted to a concentration of 45 g/l.
  • the reaction was at an end when the desired colour coordinates had been reached. Steam and air were shut off after the reaction and the product passes through operations of removal of coarse solids and of washing, before being filtered.
  • the product washed salt-free so that the conductivity of the wash water running off was approximately not more than 2 mS/cm.
  • the drier used was a “continuous drier with a dual drying stage”, known to the skilled worker as a rotary tube drier.
  • the product was dried to a final residual moisture content of ⁇ 10%. After that it was conveyed to the grinding stage.
  • a mill known to the skilled worker a horizontal classifier mill or a vertical mill (turbine type) without classifier.
  • the grinding parameters set were as follows:
  • FIGS. 1 to 6 show the results of the “3-box” method employed for testing the pigments. A trio of values is thereby recorded, which characterizes the upper limits of the three regions indicated.
  • FIG. 1 shows a 3-box method spread of ⁇ 25/--/-- ⁇ m.
  • FIG. 2 shows a 3-box method spread of ⁇ 10/25/35 ⁇ m.
  • FIG. 3 shows a 3-box method spread of 15/-/- ⁇ m.
  • FIG. 4 shows a 3-box method spread of 10/25/- ⁇ m.
  • FIG. 5 shows a 3-box method spread ⁇ 10/-/30 ⁇ m.
  • FIG. 6 shows a 3-box method spread of ⁇ 10/ 25 /35 ⁇ m.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Paints Or Removers (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Compounds Of Iron (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
US11/800,404 2006-05-13 2007-05-04 Yellow iron oxide pigments Abandoned US20070261604A1 (en)

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Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006022449A DE102006022449A1 (de) 2006-05-13 2006-05-13 Verbesserte Eisenoxidgelbpigmente
DE102006022449.3 2006-05-13

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US12/194,580 Active US7799125B2 (en) 2006-05-13 2008-08-20 Yellow iron oxide pigments

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US (2) US20070261604A1 (enrdf_load_stackoverflow)
EP (1) EP1854849A3 (enrdf_load_stackoverflow)
JP (4) JP2007302894A (enrdf_load_stackoverflow)
CN (1) CN101074327B (enrdf_load_stackoverflow)
AU (1) AU2007201990A1 (enrdf_load_stackoverflow)
BR (1) BRPI0702535B8 (enrdf_load_stackoverflow)
CA (1) CA2588982C (enrdf_load_stackoverflow)
DE (1) DE102006022449A1 (enrdf_load_stackoverflow)
MX (1) MX2007005746A (enrdf_load_stackoverflow)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102604436A (zh) * 2012-02-21 2012-07-25 升华集团德清华源颜料有限公司 一种低吸油量氧化铁黄的制备方法
CN102604438A (zh) * 2012-02-21 2012-07-25 升华集团德清华源颜料有限公司 低吸油量氧化铁黄颜料
CN103305032A (zh) * 2013-07-04 2013-09-18 南通宝聚颜料有限公司 一种降低氧化铁黄粘度的方法
US20130244869A1 (en) * 2010-10-22 2013-09-19 Sachtleben Pigment Gmbh Supported Catalyst of Digestion Residues of Titanyl Sulphate-Containing Black Solution
CN117361637A (zh) * 2023-10-08 2024-01-09 江苏宇星科技有限公司 一种高着色力低吸油量重质氧化铁黄颜料的制备方法

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US1327061A (en) * 1917-06-20 1920-01-06 West Coast Kalsomine Company Process of manufacturing iron compounds
US1368748A (en) * 1920-01-05 1921-02-15 Nat Ferrite Company Process of manufacturing iron compounds and product
US4374677A (en) * 1979-05-20 1983-02-22 Titan Kogyo K.K. Japan Preparation of improved heat stable yellow iron oxide pigments
US4376656A (en) * 1979-05-30 1983-03-15 Titan Kogyo K.K. Heat resistant yellow iron oxide pigment
US4256508A (en) * 1979-06-29 1981-03-17 Basf Wyandotte Corporation Iron oxide pigments with improved color strength
US4291010A (en) * 1979-09-05 1981-09-22 Titan Kogyo Kabushiki Kaisha Heat stable yellow iron oxides
US4459276A (en) * 1981-09-17 1984-07-10 Agency Of Industrial Science & Technology Yellow iron oxide pigment and method for manufacture thereof
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US20130244869A1 (en) * 2010-10-22 2013-09-19 Sachtleben Pigment Gmbh Supported Catalyst of Digestion Residues of Titanyl Sulphate-Containing Black Solution
US9211526B2 (en) * 2010-10-22 2015-12-15 Sachtleben Pigment Gmbh Supported catalyst of digestion residues of titanyl sulphate-containing black solution
CN102604436A (zh) * 2012-02-21 2012-07-25 升华集团德清华源颜料有限公司 一种低吸油量氧化铁黄的制备方法
CN102604438A (zh) * 2012-02-21 2012-07-25 升华集团德清华源颜料有限公司 低吸油量氧化铁黄颜料
CN102604438B (zh) * 2012-02-21 2014-09-24 升华集团德清华源颜料有限公司 低吸油量氧化铁黄颜料
CN103305032A (zh) * 2013-07-04 2013-09-18 南通宝聚颜料有限公司 一种降低氧化铁黄粘度的方法
CN117361637A (zh) * 2023-10-08 2024-01-09 江苏宇星科技有限公司 一种高着色力低吸油量重质氧化铁黄颜料的制备方法

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CA2588982C (en) 2015-03-24
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US20090199737A1 (en) 2009-08-13
EP1854849A2 (de) 2007-11-14
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JP2007302894A (ja) 2007-11-22
CN101074327A (zh) 2007-11-21
EP1854849A3 (de) 2009-09-02
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