Method of obtaining black iron oxide pigment

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

 

The invention relates to the production of inorganic pigments, namely iron oxide black pigments, and can be used in the paint industry, construction and other pigmented materials.

A method of obtaining iron oxide pigments with the structure γ-Fe2O3containing 0.1 to 12.0% SiO2and 0.02 to 5.0% of Al2O3by firing a mixture of Fe3O4, SiO2, Al2O3when 200-700°when the supply of air and oxygen. The method is designed to produce brown pigments. The disadvantage of this method is the instability of the chemical composition that does not exclude the emergence of various shades.

There is also known a method of obtaining a red iron oxide pigment from red mud, waste in the production of alumina by calcination of the mixture with rostomerom.

The closest to the technical nature of the claimed invention is a Method of obtaining iron oxide pigments". [Patent No. 2047631. Declared 17.08.1992. Published 10.11.1995. Authors : A.I. Kalinichenko, Sokolov V.I., Nikonenko E.A., Kolesnikov M.P., Purtov A.I.]. In this way pre-made separation by class size with the selection of the fraction of particles not larger than 0.02 mm, and the calcination of this fraction when 290-850°C. the Pigments obtained pure red is the first color due to α -Fe2O3.

The disadvantage of this method is the inability to obtain a black pigment due to the small number in the selected fraction of sulfide sulfur, which is necessary for recovery of Fe(III) to Fe(II).

The task of the invention to provide pigment black due to the additional sampling fraction from 0.02 to 0.045 mm, containing a higher amount of sulfide sulfur while maintaining the uniformity of the particle size distribution and coverage of 8-10 g/m2. [A.I. Kalinichenko, Kolesnikov M.P., Nikonenko E.A., Sokolov V.I., Purtov A.I. Granulometric composition of red mud. Depon. VINITI, 27.09.96, No. 2892 - B96, Moscow, 1996. - 5 S.].

This task is solved in that red mud before annealing share by class size with sampling fractions up to 0.02 mm, and optionally, from 0.02 to 0.045 mm, and the annealing of these fractions is carried out in a controlled atmosphere (reducing atmosphere, inert gases, vacuum) at a temperature of 500-1000°C.

The increase in the content of sulfide sulfur due to the additional sampling fraction from 0.02 to 0.045 mm and lowering the oxygen content in the gas phase leads to the formation of the pigment mixed oxides of iron, which causes the black color of the obtained pigment, and having a particle size of not more than 0,045 mm provides sufficient uniformity in composition and opacity for the scientists pigment.

The lower limit of the temperature range of annealing due to the fact that at 500°begins With the recovery of Fe2O3FeO and Fe3O4. The upper limit is 1000°because at a higher temperature begins agglomeration of pigment.

The claimed method was carried out obtaining black iron oxide pigment from red mud, taken from the dumps Bogoslovsky aluminum plant, the following chemical composition in terms of oxides, wt.%: Fe2O3- 35,4; Al2O3- 14,6; Cao - 11,5; S - 1,36; TiO2- 3,9; SiO2- 7,5; Na2O - 3,4; CO2- 3,5 (without pod).

A sample of red mud weight 35 kg with a moisture content of 39% was divided by class size. Selected fraction not larger than 0,045 mm, which had the following chemical composition in terms of oxides, wt.%: Fe2O3- 43,0; Al2O3- 13,5; CaO - 7,0; S - 1,2; TiO2- 3,8; SiO2- 6,5 (without pod). The output fraction of 89.9%.

After separation by class size selected fraction was filtered, washed until the pH of wash water, 8.5, and dried, after which the sample was divided into parts and progulivali through the different modes. The table lists the process parameters and the characteristics of the target product, obtained by the claimed method. The chemical composition of the product is determined by the composition of the fraction - 0,045 mm difference from the prototype I have is the color of the pigment, a higher percentage of the useful fraction, temperature interval, the use of sulfide sulfur as the reductant.

The determination of the color and opacity of the resulting pigment was based on standard techniques. [Dobrovolsky, I., A. Bolshakov and other Methods of technical analysis of pigment production. Chelyabinsk, South Ural publishing house, 1973. S-213].

Using the proposed method provides the following technical results:

- obtaining of iron oxide pigment in pure black color with opacity 8-10 g/m2;

- use waste production of alumina red mud (up to 90%) without additional raw materials and additives;

- complete absence of harmful emissions into the environment;

- use for recovery of Fe(III) Fe(II) sulfide sulfur present in the original sludge.

0,05
Table 1
Characteristics of the obtained pigmentsClass size, mm sample Weight (kg)The temperature of calcination, °WednesdayColorThe residue after wet sieving sieve 0063, %Rate, g/m2Dispersibility, mcm
By the present method Smaller 0,045 mm Weight 31 kg290Reducing atmosphereBrown0,05928
ArgonBrown0,05928
Vacuum P˜1,10-3ATMBrown0,05928
500Reducing atmosphereGray-black0,04927
ArgonGray-black0,04827
Vacuum P˜1,10-3ATMGray-black0,04827
850Reducing atmospherePure black0,031030
ArgonPure black0,031030
Vacuum P˜1,10-3ATMPure black0,031030
1000Reducing atmospherePure black0,051030
ArgonPure black1030
Vacuum P˜1,10-3ATMPure black0,051030
In the method prototypeSmaller than 0,02 mm Weight 24 kg290The airDark red0,05932
500The airPure red0,03727
850The airPure red0,051130

A method of obtaining a black iron oxide pigment from red mud waste from alumina production, including the annealing, characterized in that red mud before annealing share by class size with sampling fractions up to 0.02 mm, and optionally, from 0.02 to 0.045 mm, and the annealing of these fractions is carried out in a controlled atmosphere with a lack of oxygen at a temperature of 500-1000°C.



 

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