CN1106036A - A process for the production of pure-colored iron oxide direct red pigments and their use - Google Patents
A process for the production of pure-colored iron oxide direct red pigments and their use Download PDFInfo
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- CN1106036A CN1106036A CN 94101311 CN94101311A CN1106036A CN 1106036 A CN1106036 A CN 1106036A CN 94101311 CN94101311 CN 94101311 CN 94101311 A CN94101311 A CN 94101311A CN 1106036 A CN1106036 A CN 1106036A
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- suspension
- iron
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- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000001054 red pigment Substances 0.000 title claims abstract description 19
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000000725 suspension Substances 0.000 claims abstract description 63
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 230000003647 oxidation Effects 0.000 claims description 23
- 238000007254 oxidation reaction Methods 0.000 claims description 23
- 239000000049 pigment Substances 0.000 claims description 22
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical class [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 11
- 239000012670 alkaline solution Substances 0.000 claims description 9
- 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
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- RAQDACVRFCEPDA-UHFFFAOYSA-L ferrous carbonate Chemical compound [Fe+2].[O-]C([O-])=O RAQDACVRFCEPDA-UHFFFAOYSA-L 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 7
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 7
- 239000007864 aqueous solution 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
- 150000002505 iron Chemical class 0.000 abstract 3
- 230000001590 oxidative effect Effects 0.000 abstract 2
- 239000012266 salt solution Substances 0.000 abstract 2
- 238000000151 deposition Methods 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 229910052601 baryte Inorganic materials 0.000 description 2
- 239000010428 baryte Substances 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000001034 iron oxide pigment Substances 0.000 description 2
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000001052 yellow pigment Substances 0.000 description 2
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- Compounds Of Iron (AREA)
Abstract
The process for directly preparing direct red pigment of pure iron oxide includes such technological steps as depositing iron salt with alkali solution, oxidizing formed suspension with oxygen-containing gas, addition of iron salt solution and metal iron or iron salt solution and alkali solution to the seed, and oxidizing by oxygen-containing gas until the hue meets requirement.
Description
The present invention relates to the method for making and the purposes of the new direct red of pure-colored iron oxide.Its method for making comprises: make iron (II) salt precipitation with alkaline solution; With the formed suspension of oxygen-containing gas oxidation, in by the crystalline substance material (Seed is hereinafter to be referred as kind of a material) of above-mentioned gained, add iron (II) salts solution and metallic iron or iron (II) salts solution and alkaline solution; Use the oxygen-containing gas oxidation then, till obtaining desired tone.
The production red iron oxide pigment is known have four kinds of methods (T.C.Patton, Pigment Handbook, vol.1, New York 1988, p.288).First red iron oxide directly precipitates, and is indicated in US2716595.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.Pulp suspension is planted in formed oxidation, ironic hydroxide (III), makes red pigment by adding metallic iron, heating with the oxygen-containing gas oxidation in the presence of iron (II) salt.
By DE-B-1084405 as can be known, red pigment is only with by the manufacturing of redness kind pulp suspension.Press US-A-3946103, use kind of material properties-correcting agent and make pure red ferric oxide kind pulp suspension.
Because the soft property of the made pigment tool of this method so have improved character, comprises that dispersibility, gloss as flocculation character, when being especially in use in the jaqan system, thereby are better than by yellow and the made pigment of black iron oxide roasting.Yet when being applied to jaqan, do not reach with the purity of color yellow and red pigment that the black iron oxide roasting is made by the purity of color of the red pigment of the made ferric oxide of the direct precipitation method of above-mentioned United States Patent (USP).
Therefore, the problem to be solved in the present invention provides the preparation method of the direct red pigment of improved ferric oxide, but does not have above-mentioned shortcoming.
Accident has been found its corresponding manufacturing method, wherein prepares black magnet mineral pulp suspension (Fe earlier
3O
4), through maturing step and add iron (II) salts solution and metallic iron or iron (II) salts solution and alkaline solution after, heating and transform into the oxygen-containing gas oxidation and to have the red pigment that high purity of color is a feature.
Described kind of pulp suspension is made up of trickle magnetite ore particles.Its specific surface area is greater than 60m
2/ g(BET nitrogen adsorption method, one-point method, DIN 66131), median size is less than 0.05 μ m(electron photomicrograph method).
Therefore, the present invention relates to make the method for 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, form kind of a pulp suspension, 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 this kind pulp suspension is to have specific surface area greater than 60m
2/ g and median size are less than the black magnetite seed suspension of 0.05 μ m.
Method and to make the pure-colored iron oxide red pigment be unexpected a discovery thus, because learn in US-A-5076848, when producing iron oxide yellow or red pigment, the existence of magnetite causes losing significantly purity of color.
By the inventive method, can be by setting up felicity condition or using the kind material of preparation respectively among this suspension itself, to make this kind pulp suspension.
This kind pulp suspension is with iron (II) salt alkali solution precipitate, makes with the oxygen-containing gas oxidation then.
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 0.8-1.5, the preferred normal alkali of 0.9-1.1 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.
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 30-80 ℃, more preferably 30-50 ℃.
Precipitate and become hydroxide-or iron carbonate (II) suspension by means of adding 0.8-1.5, the preferred normal alkali of 0.9-1.1, 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.Obtain the kind pulp suspension of black, wherein use X-ray material phase analysis (Siemens D-500) (ASTM No.19.0629) only to detect magnetite (Fe
3O
4).
Advantageous manner is in 70-100 ℃ of ripe 1-4 hour with gained kind pulp suspension.
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 2.5-10, preferred 3-6.
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.
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 the pigment color test that is used for the jaqan aspect be carry out at Alkydal L 64 (Bayer AG product, a kind of Synolac that contains 63% oleum lini and 23% Tetra hydro Phthalic anhydride wherein is added with 5%Luvotix HT(Lehmann﹠amp; The Voss product) to improve viscosity).The volumetric concentration of this pigment is 10%.For being used for the pigment color test (DIN53237) of building materials aspect, make rolled-up stock by barite.For this reason, 0.5g pigment and 10g barite are joined in about 250ml glass jolting bottle.After adding 200 5mm steel balls, use automatic table shake jolting 3 minutes, be pressed into this mixture cylindric.
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 jaqan test and experiment of building material, the pigment made by the inventive method all shows high fullness of shade, is better than that (Bayferrox 510 by the made direct red pigment of the ordinary method of US-A-3946103
R, Bayer AG product), for example also be better than red pigment (the Bayferrox 105M by black pigment roasting gained by DE-A-2826941 and DE-A-463773
R, Bayferrox 110
R, Bayer AG product).
In the jaqan test, obtain extra high red composition (a
*), thereby become pure color enamelled coating attractive in appearance.
The pigment of made crystal seed multiplication constant 1.0-1.5 is suitable for use as transparent brown.When the crystal seed multiplication constant is 1.5-4, can be used as transparent or semitransparent red pigment.
The invention still further relates to purposes, be used to jaqan, plastics, material of construction, 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 the electron photomicrograph figure by the made fine particle magnet mineral material of the inventive method.
Illustrate but non-limiting the present invention by following embodiment.
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 33 ℃.The NaOH solution that adds 1.35 liters of 4.75N, use then 52 litres of air/hour/rise this suspension of flow oxidation 25 minutes of suspension.Obtain black kind pulp suspension.
Example 2
22.3 liters of ferrum sulfuricum oxydatum solutums from the titanium dioxide production operation (concentration 25g/ liter, FeSO pack into earlier
4).Temperature is 35 ℃.The NaOH solution that adds 1.35 liters of 4.75N, use then 52 litres of air/hour/rise this suspension of flow oxidation 21 minutes of suspension.Obtain black kind pulp suspension and be heated to 80 ℃, continue to ventilate and stirred 2 hours.
Example 3
(200g/ rises FeSO with 23ml ferric sulfate (II) solution
4), 2563ml water and 450g metallic iron join in the made kind pulp suspension of 4414ml example 1.After being heated to 85 ℃, with 10 litres of air/hour/rise this suspension of flow oxidation of suspension.After 32 hours, this black kind pulp suspension changes into pure red pigment.Its multiplication constant is 3.3.With suspension filtered, the washing to salt-free, in 85 ℃ of dryings, with the gained pigment grind.
Example 4
Press the step of example 3, after 52 hours, multiplication constant is 4.6, with suspension filtered, the washing to salt-free, in 85 ℃ of dryings, with the gained pigment grind.
Example 5
With 105ml ferric sulfate (II) solution (200g/ liter, FeSO
4), 3067ml water and 450g metallic iron join in the made kind pulp suspension of 3828ml example 2.After heating 85 ℃, with 7 litres of air/hour/rise this suspension of flow oxidation of suspension.
After 19 hours, this black-brown kind of pulp suspension transforms into the red pigment of pure color.Its multiplication constant is 3.5.With suspension filtered, washing is to salt-free, in 85 ℃ of dryings, with the gained pigment grind.
Claims (15)
1, a kind of method of making the direct red pigment of pure-colored iron oxide comprises:
Make iron (II) salt precipitation and use the oxygen-containing gas oxidation with alkaline solution;
Iron (II) salts solution and metallic iron or iron (II) salts solution and alkaline solution are joined in a kind of seed suspension; Then
Carry out oxidation with oxygen-containing gas, until obtaining desired tone;
The seed suspension that wherein is used for synthetic this pigment is that specific surface area is greater than 60m
2/ g, median size are less than the black magnetite seed suspension of 0.05 μ m.
2, the seed suspension preparation step that the process of claim 1 wherein is:
(a) produce ferric sulfate (II) aqueous solution, the about 10-80g/ liter of its concentration;
(b) add about 0.8-1.5, the preferred normal alkali of 0.9-1.1 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.
3, the method for claim 2, precipitation wherein and oxidation step carry out in about 30-80 ℃ temperature range.
4, the method for claim 2, precipitation agent wherein comprise and are selected from NaOH, Na
2CO
3, NH
3, MgO, MgCO
3At least a material.
5, the method for claim 2, seed suspension wherein was in ripe 1-4 hour of about 70-100 ℃ of temperature.
6, the method for claim 3, wherein the seed concentration in this seed suspension is about 4-30g/ liter.
7, the method for claim 1, wherein in this seed suspension, add metallic iron and iron (II) salts solution, will be heated to about 70-100 ℃ in this suspension then, then, with about 0.2-50 litres of air/hour/rising suspension ventilation carries out oxidation, till obtaining desired color.
8, the method for claim 1, 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 color.
9, the method for claim 2, wherein the concentration of ferric sulfate (II) aqueous solution in the step (a) is about 20-40g/ liter.
10, the method for claim 2, wherein this oxygen-containing gas is an air.
11, the method for claim 10, 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.
12, the method for claim 3, wherein this precipitation and oxidation step carry out in about 30-50 ℃ temperature.
13, the method for claim 6, wherein the concentration of seed is about 7-20g/ liter in this seed suspension.
14, the method for claim 7, wherein this suspension is to be heated to about 75-90 ℃.
15, the method for claim 8, wherein this suspension is to be heated to about 75-90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94101311 CN1106036A (en) | 1994-01-26 | 1994-01-26 | A process for the production of pure-colored iron oxide direct red pigments and their use |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94101311 CN1106036A (en) | 1994-01-26 | 1994-01-26 | A process for the production of pure-colored iron oxide direct red pigments and their use |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1106036A true CN1106036A (en) | 1995-08-02 |
Family
ID=5030109
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94101311 Pending CN1106036A (en) | 1994-01-26 | 1994-01-26 | A process for the production of pure-colored iron oxide direct red pigments and their use |
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|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110506081A (en) * | 2017-03-31 | 2019-11-26 | 朗盛德国有限责任公司 | Iron oxide pigment containing Al |
-
1994
- 1994-01-26 CN CN 94101311 patent/CN1106036A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110506081A (en) * | 2017-03-31 | 2019-11-26 | 朗盛德国有限责任公司 | Iron oxide pigment containing Al |
| CN110506081B (en) * | 2017-03-31 | 2021-12-10 | 朗盛德国有限责任公司 | Iron oxide pigments containing Al |
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