CN1106038A - Pure-colored iron oxide direct red pigments, a process for their procuction and their use - Google Patents
Pure-colored iron oxide direct red pigments, a process for their procuction and their use Download PDFInfo
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- CN1106038A CN1106038A CN94101313.8A CN94101313A CN1106038A CN 1106038 A CN1106038 A CN 1106038A CN 94101313 A CN94101313 A CN 94101313A CN 1106038 A CN1106038 A CN 1106038A
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- 238000000034 method Methods 0.000 title claims abstract description 36
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000001054 red pigment Substances 0.000 title claims abstract description 24
- 239000000049 pigment Substances 0.000 claims abstract description 27
- 239000000725 suspension Substances 0.000 claims description 67
- 239000000463 material Substances 0.000 claims description 25
- 230000003647 oxidation Effects 0.000 claims description 20
- 238000007254 oxidation reaction Methods 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 18
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical class [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 15
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000010276 construction Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 8
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 8
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 8
- RAQDACVRFCEPDA-UHFFFAOYSA-L ferrous carbonate Chemical compound [Fe+2].[O-]C([O-])=O RAQDACVRFCEPDA-UHFFFAOYSA-L 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 6
- 239000012670 alkaline solution Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000009423 ventilation Methods 0.000 claims 2
- 150000002926 oxygen Chemical class 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- 239000004566 building material Substances 0.000 abstract description 6
- 239000000919 ceramic Substances 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 239000001034 iron oxide pigment Substances 0.000 description 5
- 235000013980 iron oxide Nutrition 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 3
- 229910052601 baryte Inorganic materials 0.000 description 3
- 239000010428 baryte Substances 0.000 description 3
- 239000011449 brick Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- RFAFBXGYHBOUMV-UHFFFAOYSA-N calcium chromate Chemical compound [Ca+2].[O-][Cr]([O-])(=O)=O RFAFBXGYHBOUMV-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 208000035126 Facies Diseases 0.000 description 1
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000001052 yellow pigment Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Classifications
-
- 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
- C01G49/06—Ferric oxide [Fe2O3]
-
- 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
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/45—Aggregated particles or particles with an intergrown morphology
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
- C01P2006/60—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
- C01P2006/62—L* (lightness 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
- C01P2006/63—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
- 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
- C01P2006/65—Chroma (C*)
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- Compounds Of Iron (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The present invention relates to a new pure iron oxide direct red pigment, its productive method and its application to building material and ceramic pigment.
Description
The present invention relates to direct red of new pure-colored iron oxide and method for making thereof and in material of construction and pottery as the purposes of pigment.
The production red iron oxide pigment is known have four kinds of methods (T.C.Patton, Pigment Handbood, vol.1, New York 1988, p.288).First red iron oxide directly precipitates, and is indicated in US 2716595.In this method, iron (II) salts solution and alkaline solution mix with equivalent basically, air are fed the ironic hydroxide (II) or iron carbonate (II) suspension that are become.Formed oxidation-ironic hydroxide (III) seed (seed is hereinafter to be referred as kind of a material) suspension, in the presence of iron (II) salt by adding metallic iron, heating and making red pigment with the oxygen-containing gas oxidation.
By DE-B-1084405 as can be known, red pigment is only with by the manufacturing of redness kind pulp suspension, and yellow ultramarine is by the manufacturing of yellow kind pulp suspension.Therefore the color of final product depends on used kind material significantly.
Mixture yellow, red iron oxide pigment can only become brown, and its tone is out of favour.US-A 3946103 discloses a kind of method, and it uses kind of a material properties-correcting agent, can make the pure Red Indian race pulp suspension by δ-FeOOH granulometric composition.
Yet the purity of color deficiency that waits the made pigment of kind of pulp suspension to show thus is not so reach the brick red tone attractive in appearance of the needed pure color in building materials market.
Therefore, the problem to be solved in the present invention provides the direct red pigment of improved ferric oxide, and it can obtain the material of construction of the brick red tone attractive in appearance of pure color.
Unexpected find that the direct red pigment of new ferric oxide can satisfy these requirements, these pigment are not to make with ordinary method with the red pulp suspension of planting, but by the manufacturing of yellow kind pulp suspension, and when material of construction is tested gained fullness of shade (C
*) greater than 45 CIELAB units.
Therefore, the present invention relates to the direct red pigment of ferric oxide, it is characterized in that, the fullness of shade of its material of construction test is preferably greater than 45.8 greater than 45 CIELAB units.
In a special preferred version, be characterised in that by pigment of the present invention in experiment of building material, its red composition (a) is greater than 28, yellow composition (b) is greater than 29, CIELAB unit.
By producing of the direct red pigment of ferric oxide of the present invention be: prepare yellow pyrrhosiderite kind pulp suspension (alpha-feooh), add iron (II) salts solution and metallic iron, perhaps add iron (II) salts solution and alkaline solution, heating and use the oxygen-containing gas oxidation.
The accident that need point out finds, the pure-colored iron oxide red pigment that can obtain by this method is because in prior art, by yellow kind pulp suspension only to make yellow iron oxide pigment.
Therefore, the invention still further relates to the method for making the direct red pigment of the saturated ferric oxide of pure color, comprise and use alkali solution precipitate iron (II) salt and use the oxygen-containing gas oxidation, in kind of pulp suspension, add iron (II) salts solution and metallic iron or iron (II) salts solution and alkaline solution, and use the oxygen-containing gas oxidation, till obtaining desired tone, wherein will be in fact by having specific surface area greater than 100m
2The yellow pyrrhosiderite kind pulp suspension that/g and median size are formed less than the starlike ramose particle of 0.2 μ m is used as described kind of pulp suspension, is used for synthetic this pigment.
Wherein the BET surface-area is to be measured by nitrogen-one-point method (DIN 66131), and particle diameter is to be measured by electron photomicrograph.
In the methods of the invention, can in suspension, directly prepare kind of a pulp suspension, perhaps use the kind material of preparation respectively by setting up felicity condition.
The particle shape that is used for the kind pulp suspension of the inventive method is diverse with the routine kind material that is used to make the yellow pigment of ferric oxide.
Fig. 1 illustrates the typical starlike branch that is used for pyrrhosiderite kind material of the present invention.For comparing, shown in Fig. 2 is the conventional yellow material of planting, and it is made up of ramose needle-like individual particle not, and obtains yellow iron oxide pigment by its synthetic dyestuff.
The preparation of described yellow pyrrhosiderite kind pulp suspension (alpha-feooh) is by alkali solution precipitate iron (II) salt, uses the oxygen-containing gas oxidation subsequently.
In the present invention's one preferred version, described kind of pulp suspension is prepared as follows:
(a) produce ferric sulfate (II) aqueous solution, the about 10-80g/ liter of its concentration is preferably the 20-40g/ liter;
(b) add about 0.8-1.0, the preferred normal alkali of 0.85-0.95 as precipitation agent in this ferric sulfate (II) aqueous solution, precipitation becomes ironic hydroxide (II) or iron carbonate (II) suspension;
(c) in described suspension, ventilate strongly with described ironic hydroxide of oxidation (II) or iron carbonate (II) by means of oxygen-containing gas, form oxidation-ironic hydroxide (III) suspension of tool alpha-feooh modification.
Can use from steel acidleach to wash operation and/or produce iron (II) salt of titanium dioxide factory, useful especially is preparation ferric sulfate (II) solution.
The optimal temperature of planting material formation is preferably 15-40 ℃, more preferably 20-35 ℃.
Precipitate and become hydroxide-or iron carbonate (II) suspension by means of adding 0.8-1.0, the preferred normal alkali of 0.85-0.95, preferably use NaOH, Na
2CO
3, NH
3, MgO and/or MgCO
3
After the precipitation is oxidation, preferably uses air as oxygenant.For this reason, every liter of suspension per hour uses the 20-300 litres of air.
Advantageous manner is in 70-100 ℃ of ripe 1-4 hour with gained kind pulp suspension.
What obtain is the yellow pulp suspension of planting, and is learnt by the roentgenogramX facies analysis, is formed (alpha-feooh) (ASTM No.29.0713) by pyrrhosiderite separately.
When forming pigment, preferred kind of the material 4-30g/ liter that uses is pressed Fe
2O
3Calculate, more preferably the 7-20g/ liter.
The advantageous manner that forms pigment has two kinds of methods.First method is that metallic iron and iron (II) salts solution are joined in kind of the pulp suspension, is heated to 70-100 ℃, preferred 75-90 ℃ then, and with every liter of suspension per hour 0.2-50 rise bubbling air and carry out oxidation, till obtaining desired tone.At this moment situation is that the increase multiple of seed is 3-15, preferred 4-10.
Second method, to plant pulp suspension and be heated to 70-100 ℃, preferred 75-90 ℃, add iron (II) salts solution and alkaline solution then, and rise bubbling air with the per hour about 1-400 of every liter of suspension then and carry out oxidation, till obtaining desired tone, its pH value is 4-5.Strengthening multiple at seed is 3-15, after the preferred 4-10, also obtains desired tone.
Removing salts solution can adopt filtration and washing or adopt settling process.The red mashed prod that is become can be processed into slurry, or dry back grinding becoming powdered pigment.
Resulting is soft pure-colored iron oxide pigment.Being detected by X-ray material phase analysis (ASTM No.33.0664) is α-Fe
2O
3
For being used for the pigment color test of material of construction aspect, make rolled-up stock by barite.For this reason, 0.5g pigment and 10g barite are added in the glass jolting bottle of about 250ml.After adding 200 5mm diameter steel balls,, mixture is suppressed into cylindrical with desk-top automatic vibrator jolting 3 minutes.
The mensuration of CIELAB data (DIN 6174) is to use the color measurenent instrument have the Ulbricht ball (lighting condition d/8 °, standard light Type C/2 °); Comprise surface reflection.
Table 1 illustrates the colorimetric data of some pigment of the present invention, and supplies the relatively corresponding data of some commercially available products of usefulness.
Fullness of shade (C
*) be measuring to pigment colour purity.
In experiment of building material, pigment of the present invention has that (Bayferrox 510 than hitherto known direct red pigment
R, press US-A-3946103 and make; Or Pfizer Croma Red RO 3097
R) higher fullness of shade, (for example press DE-A-463773 and make, Bayferrox 110 also to be better than the red pigment of black pigment roasting gained
R).
Obtain desired brick red tone attractive in appearance in experiment of building material, this is by tangible yellow colors (b
*) together with high red composition (a
*) and get.
The invention still further relates to purposes, be used to material of construction and pottery to add pigment coloring, can use powdered pigment and pasty state or slurries pigment by the red pigment of the made ferric oxide of the inventive method.
Fig. 1 is by the made ferric oxide kind of the inventive method material (pyrrhosiderite), and it can make in the pigment building-up process that what make is the red pigment of pure color.For comparison purpose, shown in Figure 2 is conventional Zh a kind material (pyrrhosiderite), and it makes that in the pigment building-up process what make is yellow ultramarine.Shown in Figure 3 is that the CIELAB data of the red pigment of some ferric oxide in the material of construction test are (with a
*-b
*Face is drawn).
By following Examples set but non-limiting the present invention, describe and yellowly plant that pulp suspension forms and synthetic by red pigment of the present invention.
Example 1
22.3 liters of ferrum sulfuricum oxydatum solutums from the titanium dioxide production operation (concentration 25g/ liter, FeSO pack into earlier
4).Temperature is 31 ℃.The NaOH solution that adds 1.325 liters of 4.75N, use then 52 litres of air/hour/rise this suspension of flow oxidation 28 minutes of suspension.The yellow pulp suspension of planting of gained is heated to 80 ℃ of stirrings 2 hours.
Example 2
44m packs into earlier
3Ferrum sulfuricum oxydatum solutum (concentration 24.6g/ liter, FeSO from the titanium dioxide production operation
4).Temperature is 29 ℃.Add 2.85m
34.5N NaOH solution, use then 215 litres of air/hour/rise this suspension of flow oxidation 30 minutes of suspension.The yellow pulp suspension of planting of gained is heated to 80 ℃ of stirrings 2 hours.
Example 3
(200g/ rises FeSO with 126ml ferric sulfate (II) solution
4), 1603ml water and 450g metallic iron join in the made kind pulp suspension of 3271ml example 1.After being heated to 85 ℃, with 20 litres of air/hour/rise this suspension of flow oxidation of suspension.After 40 hours, this yellow kind pulp suspension changes into pure red pigment.Its multiplication constant is 9.6.With suspension filtered, the washing to salt-free, in 85 ℃ of dryings, with the gained pigment grind.
Example 4
With 336ml ferric sulfate (II) solution (200g/ liter, FeSO
4), 6664ml water and 1600g metallic iron join 14, in the made kind pulp suspension of 000ml example 2.After heating 85 ℃, with 0.5 litres of air/hour/rise this suspension of flow oxidation of suspension.
After 18 hours, this yellow kind pulp suspension transforms into the red pigment of pure color.Its multiplication constant is 3.7.With suspension filtered, washing is to salt-free, in 85 ℃ of dryings, with the gained pigment grind.
Example 5
Press the same steps as of example 4, oxidation is after 22 hours, and the multiplication constant of its kind material is 4.6.With suspension filtered, washing is to salt-free, in 85 ℃ of dryings, with the gained pigment filtering.
The colorimetric data of the red pigment of table 1 ferric oxide
Test (building materials purposes) in barite
Pigment L
*a
*b
*C
*Annotate
Pfizer?Croma
Red RO 3097
1)51.0 28.8 22.8 36.7 is directly red
Bayferrox 510
2)52.9 31.2 32.2 44.8 press US-A-3946103
Directly red
Bayferrox 110
2)52.5 30.6 26.9 40.7 roasting black iron oxides
Example 3 54.6 32.1 34.8 47.3
Example 4 57.9 30.0 35.9 46.8
Example 5 54.5 33.1 31.6 45.8
1) Pfizer product
2) Bayer AG product
Claims (20)
1, the direct red pigment of a kind of ferric oxide, its fullness of shade with material of construction test is greater than 45CIELAB unit.
2, the direct red pigment of the ferric oxide of claim 1, the wherein red composition (a in the material of construction test
*) be greater than 28 CIELAB units, yellow composition (b
*) greater than 29 CIBLAB units.
3, a kind of method of making the pure-colored iron oxide red pigment of claim 1 comprises:
Iron (II) salts solution and metallic iron or iron (II) salts solution and alkaline solution are joined in a kind of seed suspension;
Carry out oxidation with oxygen-containing gas, until obtaining desired tone;
The seed suspension that wherein is used for synthetic this pigment be in fact by specific surface area greater than 100m
2The yellow pyrrhosiderite seed suspension that/g, median size are formed less than the starlike ramose particle of 0.2 μ m.
4, the method for claim 3, seed suspension preparation step wherein is:
(a) produce ferric sulfate (II) aqueous solution, the about 10-80g/ liter of its concentration;
(b) add the normal alkali of about 0.8-1.0 as precipitation agent in this ferric sulfate (II) aqueous solution, precipitation becomes ironic hydroxide (II) or iron carbonate (II) suspension;
(c) ventilate with described ironic hydroxide of oxidation (II) or iron carbonate (II) strongly in described suspension by means of oxygen-containing gas, form described seed suspension.
5, the method for claim 4, precipitation wherein and oxidation step carry out in about 15-40 ℃ temperature range.
6, the method for claim 4, precipitation agent wherein comprise and are selected from NaOH, Na
2CO
3, NH
3, MgO, MgCO
3At least a material.
7, the method for claim 4, seed suspension wherein was in ripe 1-4 hour of about 70-100 ℃ of temperature.
8, the method for claim 3, wherein the seed concentration in this seed suspension is about 4-30g/ liter.
9, the method for claim 3, wherein in this seed suspension, add metallic iron and iron (II) salts solution, this suspension is heated to about 70-100 ℃ then, then in about 0.2-50 litres of air/hour/rising suspension ventilation carries out oxidation, till obtaining desired tone.
10, the method for claim 3, wherein this seed suspension is to be heated to about 70-100 ℃, add iron (II) salts solution and alkaline solution then, then with about 1-400 litres of air/hour/rise this suspension of suspension ventilation oxidation, till obtaining desired tone.
11, the direct red pigment of the ferric oxide of claim 1, its fullness of shade with material of construction test is greater than 45.8 CIELAB units.
12, the method for claim 4, wherein the concentration of this ferric sulfate (II) aqueous solution is about 20-40g/ liter.
13, the method for claim 4, wherein the alkali precipitation agent that adds in step (b) is about 0.85-0.95 equivalent.
14, the method for claim 5, wherein this precipitation and oxidation step carry out in about 20-35 ℃ temperature.
15, the method for claim 8, wherein the concentration of seed is about 7-20g/ liter in this seed suspension.
16, the method for claim 9, wherein this suspension is to be heated to about 75-90 ℃.
17, the method for claim 10, wherein this suspension is to be heated to about 75-90 ℃.
18, the method for claim 4, wherein this oxygen-containing gas is an air.
19, the method for claim 18, wherein said air are to be passed in the suspension of described ironic hydroxide (II) or iron carbonate (II), and the feeding amount is about 20-300 litres of air/hour/liter described suspension.
20, contain claim 1, the red directly material of construction of pigment of 2 or 11 ferric oxide.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4235944A DE4235944A1 (en) | 1992-10-23 | 1992-10-23 | Color-pure iron oxide direct red pigments, process for their preparation and their use |
| ITMI932169A IT1270901B (en) | 1992-10-23 | 1993-10-13 | DIRECT RED PIGMENTS OF PURE COLOR IRON OXIDE, PROCESS FOR THEIR PREPARATION AND THEIR USE |
| JP28067893A JP3659983B2 (en) | 1992-10-23 | 1993-10-15 | Pure color iron oxide direct red pigment, its production method and its use |
| GB9321805A GB2271769B (en) | 1992-10-23 | 1993-10-22 | Pure-colored iron oxide direct red pigments, a process for their production and their use |
| CN94101312.XA CN1106037A (en) | 1992-10-23 | 1994-01-26 | Pure-colored iron oxide direct red pigments, a process for their procuction and their use |
| CN94101313.8A CN1106038A (en) | 1992-10-23 | 1994-01-26 | Pure-colored iron oxide direct red pigments, a process for their procuction and their use |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4235944A DE4235944A1 (en) | 1992-10-23 | 1992-10-23 | Color-pure iron oxide direct red pigments, process for their preparation and their use |
| CN94101312.XA CN1106037A (en) | 1992-10-23 | 1994-01-26 | Pure-colored iron oxide direct red pigments, a process for their procuction and their use |
| CN94101313.8A CN1106038A (en) | 1992-10-23 | 1994-01-26 | Pure-colored iron oxide direct red pigments, a process for their procuction and their use |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1106038A true CN1106038A (en) | 1995-08-02 |
Family
ID=36940465
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94101313.8A Pending CN1106038A (en) | 1992-10-23 | 1994-01-26 | Pure-colored iron oxide direct red pigments, a process for their procuction and their use |
| CN94101312.XA Pending CN1106037A (en) | 1992-10-23 | 1994-01-26 | Pure-colored iron oxide direct red pigments, a process for their procuction and their use |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94101312.XA Pending CN1106037A (en) | 1992-10-23 | 1994-01-26 | Pure-colored iron oxide direct red pigments, a process for their procuction and their use |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP3659983B2 (en) |
| CN (2) | CN1106038A (en) |
| DE (1) | DE4235944A1 (en) |
| GB (1) | GB2271769B (en) |
| IT (1) | IT1270901B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7553767B2 (en) | 2005-09-29 | 2009-06-30 | Hynix Semiconductor Inc. | Method for fabricating semiconductor device having taper type trench |
| CN1466548B (en) * | 2000-09-26 | 2013-01-02 | 朗盛德国有限责任公司 | Contacting and adsorbent granules |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0645437B1 (en) * | 1993-09-23 | 1997-03-19 | Bayer Ag | Pure-colored iron oxide direct red pigments, process for their manufacture and their use |
| ES2152470T3 (en) * | 1995-10-26 | 2001-02-01 | Bayer Ag | RED IRON OXIDE PIGMENTS OF CHROMATIC PURITY AND WITH YELLOW FACE, PROCEDURE FOR MANUFACTURE AND USE. |
| JP6440830B2 (en) * | 2014-09-11 | 2018-12-19 | ランクセス・ドイチュランド・ゲーエムベーハー | Red iron oxide pigments with improved color values |
| EP3216764A1 (en) * | 2016-03-09 | 2017-09-13 | LANXESS Deutschland GmbH | Production of iron oxide red pigments |
| EP3683190B1 (en) * | 2019-01-17 | 2022-03-09 | LANXESS Deutschland GmbH | Method for manufacturing hematite pigments |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2556406A1 (en) * | 1975-12-15 | 1977-06-16 | Bayer Ag | PROCESS FOR THE CONTINUOUS PRODUCTION OF IRON OXIDE HYDROXIDE |
| DE3440911C2 (en) * | 1984-11-09 | 1997-08-21 | Bayer Ag | Process for the production of platelet-shaped iron oxide pigments |
| DE3500470A1 (en) * | 1985-01-09 | 1986-07-10 | Bayer Ag, 5090 Leverkusen | METHOD FOR PRODUCING LIGHT COLORED PURE IRON OXIDE RED PIGMENTS |
-
1992
- 1992-10-23 DE DE4235944A patent/DE4235944A1/en not_active Withdrawn
-
1993
- 1993-10-13 IT ITMI932169A patent/IT1270901B/en active IP Right Grant
- 1993-10-15 JP JP28067893A patent/JP3659983B2/en not_active Expired - Fee Related
- 1993-10-22 GB GB9321805A patent/GB2271769B/en not_active Expired - Fee Related
-
1994
- 1994-01-26 CN CN94101313.8A patent/CN1106038A/en active Pending
- 1994-01-26 CN CN94101312.XA patent/CN1106037A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1466548B (en) * | 2000-09-26 | 2013-01-02 | 朗盛德国有限责任公司 | Contacting and adsorbent granules |
| US7553767B2 (en) | 2005-09-29 | 2009-06-30 | Hynix Semiconductor Inc. | Method for fabricating semiconductor device having taper type trench |
Also Published As
| Publication number | Publication date |
|---|---|
| IT1270901B (en) | 1997-05-13 |
| CN1106037A (en) | 1995-08-02 |
| GB9321805D0 (en) | 1993-12-15 |
| JPH06256022A (en) | 1994-09-13 |
| GB2271769B (en) | 1995-09-13 |
| ITMI932169A1 (en) | 1995-04-13 |
| GB2271769A (en) | 1994-04-27 |
| ITMI932169A0 (en) | 1993-10-13 |
| JP3659983B2 (en) | 2005-06-15 |
| DE4235944A1 (en) | 1994-04-28 |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |