Method of preparing iron-containing pigment

FIELD: chemistry.

SUBSTANCE: to obtain an iron-containing pigment, aqueous solutions of sodium or ammonium carbonate and magnesium chloride or sulphate are first mixed in equimolar ratio. A magnesium carbonate pulp is obtained and settled. After that the clear portion is decanted and washed 2-3 times with water in volume ratio pulp : water=1:(2-3), each time decanting the clear portion. Iron (III) sulphate solution is then added to the magnesium carbonate pulp. The obtained residue of iron hydroxides or hydroxocarbonates is filtered off, washed with water, dried and annealed.

EFFECT: invention increases output when preparing a pigment owing to 2-3 times faster filtration of the iron-containing residue.

2 tbl, 2 ex

 

The invention relates to the field of technology of inorganic pigments, and more specifically to the technology of iron oxide pigments.

A method of obtaining brown iron-containing pigment, the essence of which is that fine dust (sludge) open hearth and electric steel plants subjected to hydrothermal treatment at 60-80°C for 1.0 to 1.5 h in a mixture with one-deputizing calcium phosphate, taken in the ratio 1:(0,05-0,08), followed by washing the resulting product from water-soluble substances and heat it at 150-350°C.

EN 2057154, IPC SS 1/24, 1994

A method of processing an acidic iron-containing waste water, the essence of which is that iron-containing aqueous solution is treated with a solution of potassium hydroxide for allocation of iron in the form of hydroxide, followed by the separation of the precipitate by filtration

EN 2019524, IPC C02F 1/64, 1991

A disadvantage of known methods is the formation of clay, amorphous precipitate of hydroxides, are prone to the formation of a colloidal gel with a very low filtration rate.

The closest technical solution and the achieved result is a method of producing gypsum and micaceous iron pigment from acidic wastes from production of titanium dioxide by the sulphate method.

US 6440377, IPC C01F 100; C01G 49/00, 2002 is.

The disadvantages of this method is the length and a multi-stage process with the need for more introduction of metallic iron or substance containing metallic iron, dual neutralizing solution to achieve a pH of 3-5, use of oxygen as an oxidizing agent upon receipt of the brown pigment.

The challenge aimed proposed solution - improving the performance of the allocation process of iron-containing precipitate by increasing the rate of filtration.

According to the proposed method of obtaining zhelezosoderzhashchie pigment this objective is achieved in that the solution obtained by the method of bioleaching copper containing iron in the ferric form, treated with an aqueous slurry obtained by mixing aqueous solutions of sodium carbonate (potassium) or ammonium chloride or magnesium sulfate in equimolar ratio. It is important to obtain crystalline magnesium carbonate and to withstand the recommended order of addition of the solutions. From a practical point of view, the pulp is advisable to obtain mixing of solutions containing 100-150 g/l potassium carbonate or sodium, or ammonium, and 100-150 g/l sulfate or magnesium chloride. In the process of mixing the carbonate is produced (and partly carbonate) magnesium. The resulting slurry of magnesium carbonate from Tivat, merge decanting the clarified part, 2-3 times washed with water at a ratio (vol.) pulp:water=1:(2-3), each time decanter clarified part. The solution of salt of iron (III) is added slowly to a slurry of magnesium carbonate avoid foaming due to the release of carbon dioxide. Magnesium carbonate interacts with cations of trivalent iron with the formation of hydroxides and hydroxycarbonate iron precipitated. The amount of magnesium to iron support in a ratio (mol): iron:magnesium=(1,02-1,05):1. The precipitate of hydroxides or hydroxycarbonate iron is separated by filtration, washed with water, dried and calcined to obtain a transparent pigment.

A positive effect is to increase the filtration rate of the slurry at the stage of separation of iron-containing precipitate and at the stage of washing this precipitate.

Example 1

Iron-containing pigment was obtained by precipitation of iron from solution obtained by leaching project metallurgical wastes. The content of sulphate of iron (calculated as Fe3+) of 40.3 g/l, pH of 1.6. To aqueous solution of sodium carbonate with a concentration of 100 g/l solution was added magnesium sulfate with a concentration of 154 g/l in equimolar ratio. The precipitation of magnesium carbonate was separated by decantation. To the resulting slurry was added water in sootnoshenie the volume of pulp:the volume of water=1:2 and mixed to the slurry. Subsequent assertion of the clarified part amounted to 2/3 of the total. The clarified portion was decanted and the operation was repeated two more times. The resulting slurry of magnesium carbonate containing a small amount of water-soluble sulfate sodium (less than 5 g/l). Removal of soluble salts of sodium sulfate is necessary because from solutions containing high concentrations of soluble salts, iron carbonate precipitation forms, with the worst filterability. In the resulting slurry was introduced, the calculated amount of iron-containing solution slowly with stirring (option 1, table 1). In the second variant, on the contrary, in the ferric sulfate solution was injected the same amount of slurry of magnesium carbonate. The number of iron taken a few more (in moles) in comparison with magnesium carbonate (0.04 mol). This is done to ensure that all the magnesium carbonate reacted, and in the pulp remained excess of solid magnesium carbonate (which after filtering will remain with sediment iron). Practically it is more convenient to follow the pH value, as even with a small excess of ferric sulfate pH is shifted to values of 3.0-3.5. In table 1 also shows the results of filtering the pulp (option 3), obtained in accordance with known methods, i.e. by adding a solution of potassium hydroxide to the iron-containing solution.

Financial p the tats showed the use of the proposed method to increase the filtration rate of the slurry in 2-3 times.

Table 1
The results of the iron filter sediment
OptionThe sequence of operationsThe filtration rate of the slurry, m3/m2h
1Adding to the slurry of magnesium carbonate solution of trivalent iron0,40
2Adding to a solution of trivalent iron slurry of magnesium carbonate0,15
3Adding to the solution of ferric solution of potassium hydroxide0,12

Example 2

A solution of ammonium carbonate with a concentration of 80 g/l, and magnesium chloride with a concentration of 65 g/l were mixed in equimolar ratio. The precipitate of magnesium carbonate was separated from the mother liquor by decantation and washed with water 3 times at a ratio of pulp:water=1:2. The clarified portion was removed by decantation. Bicarbonate of iron was obtained in two ways: by adding the of astora iron slurry of magnesium carbonate and adding the slurry to a solution of trivalent iron.

The results (table 2) showed that the use of ammonium carbonate filtration rate is somewhat less than when using sodium carbonate. This is due to the higher degree of hydrolysis of ammonium carbonate, which results in smaller crystals of magnesium carbonate. However, using the proposed method also allows to increase the filtration rate of the slurry in 2-3 times.

Table 2
The results of the iron filter sediment
OptionThe sequence of operationsThe filtration rate of the slurry, m3/m2h
1Adding to the slurry of magnesium carbonate solution of trivalent iron0,34
2Adding to a solution of trivalent iron slurry of magnesium carbonate0,16
3Adding to the solution of ferric solution of potassium hydroxide0,13

The way to obtain iron oxide pigment, comprising mixing the existence of magnesium carbonate with a solution of iron salts, filtration, washing with water, drying and calcination, wherein the first mixed aqueous solutions of sodium carbonate or ammonium chloride or magnesium sulfate in equimolar ratio with obtaining a slurry of magnesium carbonate, defend, decanted clarified part, washed 2-3 times with water at a volume ratio of the pulp: water=1:(2-3), each time decanted clarified part, then a solution of sulphate of iron (III) is added to the resulting slurry of magnesium carbonate, the precipitate of hydroxides or hydroxocobalamin iron is separated by filtration.



 

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1 tbl, 12 ex

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2 cl, 5 tbl, 6 ex

FIELD: chemical industry; metallurgy industry; other industries; methods of production of the high purity ferric oxides.

SUBSTANCE: the invention is pertaining to the method of production of the high purity ferric oxides and may be used in production of the pigments and the catalysts at production of the high purity ferric oxides. The ferric oxides are produced by interaction of the metallic iron made in the form of the microball-shaped particles either the scrap, or the turning chips, which dimensions are such, that the area of their surface per one kg of iron and per one liter of the reaction medium makes more than 0.01 m2 with the being stirred water solution of the carboxylic acid having рКа from 0.5 up to 6 for the first carboxyl and capable to thermolysis in the open air at the temperature of from 200 up to 350°С into carbon dioxide and the water. The ratio between the moles of the carboxylic acid and g-atoms of the iron makes from 0.03 up to 1.5 and the mass ratio of the water/iron - from 1 up to 20, the microball-shaped particles are kept in the suspension by stirring. The produced carboxylate of the ferrum (II) is oxidized up to carboxylate of the ferrum (III) with the oxidant selected from oxygen, the oxygen-containing gaseous mixture and hydrogen dioxide. The earlier produced carboxylate of the ferrum (II) also may be exposed to the oxidizing. Then the carboxylate of the ferrum (III) is heated up in the open air till production of the oxides. The invention allows to increase the purity of the ferric oxides and productivity at their production.

EFFECT: the invention ensures the increased purity of the produced ferric oxides and productivity at their production.

9 cl, 12 ex

FIELD: chemistry.

SUBSTANCE: present invention pertains to production of black iron oxide pigments and can be used in paint and coating industry. The black iron oxide pigment is obtained from burning red mud - aluminous production waste. Before burning, the red mud is sorted according to size, with selection of the 0.02 mm fraction and further selection of the 0.02-0.045 mm fraction. These fractions are burnt in a controlled atmosphere with oxygen deficiency at 500-1000°C temperature.

EFFECT: obtaining iron oxide pigment of a pure black colour with 8-10 g/m2 coverage using aluminous production wastes - red mud, without more raw materials and additives and pollution of the environment.

1 tbl

FIELD: chemistry.

SUBSTANCE: natural mechanically milled iron (III) oxide of lamellar structure at least 50 wt %, preferentially 75 wt %, contains particles sized 10 mcm and less in amount, at least, 50 wt %, preferentially 70 wt %, particularly preferentially 90 wt %. The ratio of thickness to maximum diametre of iron (III) oxide plates is 1:5, preferentially 1:10. To produce such iron (III) oxide, it is mechanically milled in an impactor or a jet-type mill. Iron (III) oxide resulted from mechanical milling, is separated by size grade, e.g. by an air separator. Iron (III) oxide can be used in lacquering for a base corrosion protection, mechanical load protection, UV and IR protection, for decorative coating, and also as an extender for polymeric and ceramic materials.

EFFECT: possibility to prepare highly dispersed lamellar particles of natural iron oxide.

15 cl

FIELD: chemistry.

SUBSTANCE: method for preparation of iron oxide pigment from specularite includes specularite milling up to particle size more than 1 mm - 5 mm, after material concentration with magnetic separation up to content of α-Fe2O3 more than 60.0 wt % specularite is concentrated again. Concentrated specularite can serve as starting material for obtaining of pigment with dull luster consisting of iron mica with Fe2O3 content more than 85 wt % which includes thin scaly plates in amount more than 50 wt % and is featured with residue after wet sieving on a sieve with mesh size 63 mcm not more than 35 wt %.

EFFECT: invention allows to obtain pigments from specularite for protective-decorative and decorative coatings.

8 cl, 2 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: invention relates to protection of metals from corrosion using lacquer coatings. The engineering problem is solved using a method of preparing an anticorrosion pigment based on aspiration dust wastes from foundry electric furnaces. The aspiration dust is mixed with calcium hydroxide in water with content of calcium hydroxide in the mixture with aspiration dust equal to 8-11 wt %, and aspiration dust with calcium hydroxide in water is taken in ratio of 1:1 respectively. The obtained mixture is dried, calcined at 820-900°C for 3.5-5.5 hours and then ground up to the required degree of dispersion.

EFFECT: possibility of simplifying preparation of a highly efficient anticorrosion pigment and without presence of toxic components in it, as well as reduction of cost of the pigment and environmental conservation.

1 cl, 2 tbl, 15 ex

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