Method of preparing iron oxide pigments

FIELD: varnish-and-paint industry.

SUBSTANCE: invention is intended for use in chemical industry and construction for preparing varnishes, paints, and rubber products. Gas treatment slime from converter industry is fractioned, fraction up to 10 mm is dehydrated by drying at 70-110°C to at most 5% moisture content and reduced to particles not exceeding 300 μm in size. Color spectrum of product is extended from red to black by calcining disintegrated product at 300 to 900°C. Content of iron oxides in pigment is much higher than in pigments prepared using known processes.

EFFECT: widened resource of raw materials, utilized converter industry waste, and reduced price of product.

2 cl, 1 tbl, 6 ex

 

The invention relates to the production of inorganic pigments, namely micaceous iron, and can be used in the paint industry, building materials industry, production of rubber products.

A method of obtaining micaceous iron pigments from spent etching carbon steels hydrochloric acid solutions by thermal decomposition at a temperature 480-750°With the combustion of combustible gas in air flow with subsequent washing steam condensate (ed. St. No. 749873, M CL 3 09 With 1/24, publ. bull. No. 27, 23.07.80).

The disadvantage of this method is the formation of waste combustible gas and the need to wash, produces 3 tons of waste (much zakislenna water) per 1 ton of product. How expensive and difficult, because it requires special equipment.

A method of obtaining micaceous iron pigments of different colors on the particles of mica flake form by oxidation of PENTACARBONYL iron, which is movable in a fluidized bed, oxygen-containing gas at a temperature of 20-100° (RF patent No. 2049799 M CL 6 09 With 1/24, published. 10.12.95 year). The invention is not obtaining the pigment as such, and its receipt on the particles of mica.

A method of obtaining brown iron-containing pigment through the use of fine dust (sludge) is artemovskogo and electric steel production from hydrothermal treatment at 60-80° C for 1.0 to 1.5 h in a mixture with one-deputizing the calcium phosphate, followed by washing and heat treatment at 150-350° (RF patent No. 2057154, MCL 6 09 With 1/24, published. 27.03.96). This method requires sophisticated technology, has four of the original substance, you want cold and hot water. Waste water exceeds 20-30 times the amount of the final product.

A method of obtaining micaceous iron pigments by treating a solution of iron salts in the presence of inert carrier alkaline reagent and oxygen at elevated temperatures. As the inert carrier used conveyor clay slurries potash production (patent RF №2209820, IPC 7 09 With 1/24, published. 10.08.03). This method is difficult to use and requires special equipment. Forms waste, require water for flushing.

A method of obtaining micaceous iron pigment based on iron oxide with the use of oxides of aluminum, magnesium and calcium in the following ratio, wt.%:

Aluminum oxide 31,10-36,90

Magnesium oxide 0,26-0,30

Calcium oxide 0,09-0,11

The iron oxides else.

To obtain a pigment used pyrite cinder, which before chopping mixed with molmol - a waste product of acetone, the mixture is treated with sulfuric acid and calcined (ed. St. No. 1154300, CL 09 With 1/24, published. 07.05.85,, bull. No. 17).

Famous Nai is more close to the proposed method of producing micaceous iron pigments from waste in the production of alumina by dividing by class size in the hydrocyclone with a sampling fraction of particles not larger than 0.02 mm and annealing them when 290-850°With (Prototype, patent RF №2047631, IPC 6 09 With 1/24, published. 10.11.95 year). This method requires a large consumption of water. The ratio of liquid - solid when hydrocycloning equal to 5.0, in addition, require a certain flow of water for washing. This increases the cost of production and causes substantial damage to the environment.

The final product contains only 53% Fe2O3. the pH of the final product is equal to 8.5, i.e. it is too alkaline environment.

In the production of pigment takes place except water 31,3% of solid waste.

The method is complicated and requires special equipment (it was tested on laboratory cyclone).

The task of the invention to provide micaceous iron pigments (black, red and brown colors) more effective at expanding the resource base, excluding consumption of water and no waste. The final product is a black pigment - containing FeO to 63%, and the red pigment has a content of Fe2About3up to 90%, the pH is equal to 7.5 for both pigments.

This task is achieved in that in the method of obtaining micaceous iron pigments from raw materials based on iron oxides as raw materials use waste Converter production - gas cleaning sludge, separating the fraction up to 10 mm, subjecting it to dehydration to a moisture content of not more than 5% method of drying at a temperature of 70-110°and change ICALT to the size of the particles not exceeding 300 microns with receipt of the finished product - pigment black. To obtain pigments of brown and red colors after grinding, the slurry is subjected to calcination at a temperature of 300-900°C.

Check the patentability showed that the proposed solution meets inventive step, since it is not necessary for professionals in the obvious way from the prior art.

Used as raw material waste Converter production - gas purification sludges are unusable waste. Annually only at the Cherepovets steel mill is formed of 180 thousand tons of such waste per year.

Studies have shown that the use of gas cleaning sludge with a moisture content of more than 5% causes difficulty in his grinding, increases the cost of grinding. The use of drying before grinding reduces the grinding process.

Dehydration at temperatures below 70°lengthens the drying process, and the use of dehydration at a temperature of more than 110°causes the transition of FeO to Fe2About3and undesirable color change pigment.

The value of particle sizes of grinding depends on the destination - use area (paint industry, tint the concrete mass, bricks, rubber products etc).

For grinding can be used known equipment, such as fibroma the instructor VM-200, ball mill, float stone.

For conducting experiments used the Converter gas cleaning sludge from the chemical composition, %:

Fe Society. 62,57

Fe met. 3,02

FeO 58,47

Fe2O328,83

MgO 4,21

CaO 11,33

SiO24,48

other (Al2About3, P, Mn, Ni, Cu, S) 1,33

Example 1. Took BOF sludge, separated fraction to 10 mm, was subjected to drying at a temperature of 100°up to 0.5% moisture, crushed it up to a particle size of not more than 300 μm on a grater WITH Burr 124 (productive, easy and common mill). Got the black pigment. Fractional composition of a heterogeneous: from particles less than 50 microns to 300 microns. Waste of any kind are absent. Without improvements this pigment can be used for painting of concrete, sand-lime bricks and other things, which do not require finer grinding.

Example 2. All operations are fully in example 1. Optionally, the pigment after grinding was subjected to calcination in air at a temperature of 600°C for one hour. The pigment has acquired a red color. No waste is formed. Apply analogously to example 1.

Example 3. Took BOF sludge, separated fraction to 10 mm was subjected to drying at a temperature of 100°to a moisture content of 0.5%, crush it to a size less than 30 microns in a ball mill. Got the black pigment. Waste of any kind are absent. PR is change any.

Example 4. All operations are fully in example 3. Optionally, the pigment was subjected to calcination in air at a temperature of 600°C for one hour. The pigment has acquired a red color. No waste is formed. Apply analogously to example 3.

Example 5. All operations are fully in example 3. Optionally, the pigment was subjected to calcination in air at a temperature of 400°for fifty minutes. The pigment has acquired a brown color. No waste is formed. Apply analogously to example 3.

Example 6. All operations are fully in example 3. Optionally, the pigment was subjected to calcination in air at a temperature of 400°within half an hour, the pigment has acquired a dark brown color. No waste is formed. Apply analogously to example 3.

The table below shows comparative data of the effectiveness of the proposed method.

Table
The way to obtainWater consumptionPHThe content of Fe2About3in the finished productYield in % of the raw materials
The known method (prototype)5 tons per 1 ton of the product when hydrocycloning + consumption for washing to a pH of 8.58,55368,7 (OST the aspects of 31.3 - waste)
The proposed method (red pigment)no7,5Up to 92105 (waste not)

Studies have shown that sludge gas purification Converter production contains Fetotalto 62-64% and allows you to get in the final product - the black pigment - FeO to 63%, and the final product - the red pigment contents in D2About3up to 92%.

The output of the red color is 105-106% (depending on the content of FeO), i.e. exceeds the number of recovered raw materials due to the accession of atmospheric oxygen during the process of calcination and conversion of FeO to Fe2O3.

the pH of the initial slurry is always in the optimal value of 7.5.

The temperature and duration of calcination depends on the quality of the processed sludge and equipment used.

The proposed method has advantages in comparison with prototype: allows you to expand the raw material base, dispose of waste, simplify production, reduce the cost of production.

So well-known domestic micaceous iron pigments have cost more than 10 thousand rubles/t, foreign - 40 RR/ton, and offer about 6 RR/so

1. The method of obtaining micaceous iron pigments from raw materials based on iron oxides PU is eating his grinding, characterized in that is used as raw material waste - gas cleaning sludge Converter production, separate the fraction up to 10 mm, subjecting it to dehydration to a moisture content of not more than 5% method of drying at a temperature of 70-110°and crushed to particle size of not more than 300 μm.

2. The method according to claim 1, characterized in that after grinding, the slurry is subjected to calcination at a temperature of 300-900°C.



 

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FIELD: chemical industry and agriculture; production of hydrosol of ferric iron hydroxide.

SUBSTANCE: the invention is intended for a chemical industry, an agriculture and pedology and may be used at production of solutions for soils reclamation. 0.5 l of a ferric chloride solution with concentration of 0.5 l/mole gram-molecule is poured into a pan. Carbon electrodes are put into the solution. Pass a current of 1А. Each 5-60 seconds polarity of the electrodes is changed. In a result of replacement of anions of the salt for ions of the hydroxyl obtain a stable hydrosol of the ferric iron hydroxide. The invention allows to produce such sols using a simple and a production-friendly method commercially.

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6 ex

The invention relates to the production of magnetic recording media and can be used to obtain magnetic powder cobalt containing magnetic iron oxide

The invention relates to the field of recycling industrial waste to produce valuable components and can be used, in particular, for technical iron oxide of the abrasive slurry waste generated in the bearing and other industrial applications

FIELD: chemical industry and agriculture; production of hydrosol of ferric iron hydroxide.

SUBSTANCE: the invention is intended for a chemical industry, an agriculture and pedology and may be used at production of solutions for soils reclamation. 0.5 l of a ferric chloride solution with concentration of 0.5 l/mole gram-molecule is poured into a pan. Carbon electrodes are put into the solution. Pass a current of 1А. Each 5-60 seconds polarity of the electrodes is changed. In a result of replacement of anions of the salt for ions of the hydroxyl obtain a stable hydrosol of the ferric iron hydroxide. The invention allows to produce such sols using a simple and a production-friendly method commercially.

EFFECT: the invention allows to produce such sols using a simple and a production-friendly method commercially.

6 ex

FIELD: varnish-and-paint industry.

SUBSTANCE: invention is intended for use in chemical industry and construction for preparing varnishes, paints, and rubber products. Gas treatment slime from converter industry is fractioned, fraction up to 10 mm is dehydrated by drying at 70-110°C to at most 5% moisture content and reduced to particles not exceeding 300 μm in size. Color spectrum of product is extended from red to black by calcining disintegrated product at 300 to 900°C. Content of iron oxides in pigment is much higher than in pigments prepared using known processes.

EFFECT: widened resource of raw materials, utilized converter industry waste, and reduced price of product.

2 cl, 1 tbl, 6 ex

FIELD: chemical industry; mechanical engineering; etching and galvanic production branches; methods of production of the magnetic liquids.

SUBSTANCE: the invention is pertaining to the field of production of the magnetic liquids from the wastes of the etching and galvanic productions. The invention problem is production of the magnetic liquids on the basis of the water using the waste etching solution of the engineering plants as the source of the bivalent iron and the sediment-waste after purification of the waste waters of the galvanic manufacture by electrocoagulation - as the source for production of the trivalent iron. The problem is settled due to the fact, that the method provides for co-sedimentation of the salts of the bivalent and trivalent iron by the surplus of the ammonia concentrated solution, coating of the surface of the particles with the adsorbed layer of the stabilizing substance - sodium oleate, heating of the suspension and bringing it up to boiling at the constant hashing, centrifuging of the mixture after its cooling for separation of the large- dispersed particles be notable for the fact, that as salts of the bivalent and trivalent iron using the mixture of the waste etching solution of the engineering plants containing FeSO4 and the muriatic sediment-waste containing Fe(OH)3 in the ratio of 2:3 after purification of the sewage of the galvanic production by electrocoagulation.

EFFECT: the invention ensures production of the magnetic liquids on the basis of the water using the waste etching solution of the engineering plants as the source of the bivalent iron and the sediment-waste after purification of the waste waters of the galvanic manufacture by electrocoagulation - as the source for production of the trivalent iron.

1 tbl, 3 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: metallurgy.

SUBSTANCE: method of sulphide minerals oxidation includes feeding of pulp with sulphide minerals and oxidising agent into reactor with following its blending and outlet of oxidised composition from reactor. During blending of pulp and oxidising agent in internal chamber of reactor in turbulent conditions it is implemented mechanical activation of surface of solid phase of pulp and disperse of oxidising agent. Outlet of oxidised compositions from internal chamber into external chamber of reactor is implemented under action of pressure created by inlet flow of pulp through openings overlapped in top part of internal chamber by regulator of pulp outlet. Additionally liquid phase of pulp is continuously circulates from external chamber into internal chamber of reactor. Oxidation rate of sulphide minerals is regulated by means of changing of oxidising agent concentration in pulp ensured b changing of its amount form 3000 up to 15000 mg·l/h at activation of pulp in reactor.

EFFECT: invention provides reduction of sulphur content in treatment products of mineral raw material directed to following enrichment or metallurgical redistribution, increasing of reactor productivity.

1 dwg, 3 tbl, 3 ex

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