Method for preparation of iron oxide pigment from specularite

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

 

The invention relates to the production of inorganic pigments, namely iron oxide, and can be used in the paint industry, production of construction materials, plastics, rubber products and so on

A known method of producing pigments with metallic luster (see patent RU No. 2049798, class SS 1/00, published 10.12.1995 year), according to which conduct the oxidation of CARBONYLS of metals, such as octacarbonyl cobalt, hexacarbonyl chromium, hexacarbonyl molybdenum oxygen-containing gases in a moving fluidized bed of particles of scaly form, such as mica, aluminum, graphite at 40-100°C, in particular, in the presence of inert gas. A method of obtaining micaceous iron pigments of different colors on the particles of mica flake shape (see patent RU No. 2049799, class SS 1/24 published 10.12.1995 year), according to which produce oxidation of PENTACARBONYL iron oxygen-containing gas in a moving fluidized bed of particles of mica flake form at 20-100°C, the oxidation process is conducted in the presence of a chemically inert gas, and further treated in air at a temperature of 250-800°C.

The disadvantage of these methods is the complexity of the technological process, the dependence of the color from the film thickness, the number of precipitated iron oxide, in this regard, strict dependent shall be from temperature regimes. In addition, these methods provide no pigment and film on the particles of mica, which, under the action of mechanical forces can be used up and worsen the appearance of products.

A method of obtaining brown micaceous iron pigment (see patent RU No. 2118972, class SS 1/00, 1/24, published 20.09.1998 g) of rainfall electrochemical treatment of wastewater of electroplating with the addition of reductant 10-0,5 wt.% - fine metal: aluminum or iron, or of easily oxidizable organic substances - waste oil, waste paper, bottoms production of higher alcohols.

The disadvantage of this method is the dependence of the production of a pigment from electroplating, accurate selection of the quantitative proportions of the starting components for the production of a pigment.

The closest in technical essence and essential features to the present invention is a method of obtaining a pigment (see application DE 3624920, class WW 9/00, published 28.01.1988 g), from specularite with the initial content of α-Fe2About380%-95% and a particle size of from 0-15 cm by grinding and beneficiation by flotation. This method allows you to obtain chemically pure pigment from natural specularite with the content of α-Fe2About3and 99.8 wt.% and a particle size of from 63-90 μm. The disadvantage of this is the first way is to obtain a pigment only one color.

The known material is iron oxide. This gray powder with metallic angular Shine with scaly structure due to plates of α-Fe2About3the thickness to 5 μm and a length of 60 μm, which is formed in the film hermetic barrier, reinforced film, reflect rays and delay the penetration of water and gases. According to the international standard ISO 10601: 2007 (E) iron oxide used as anticorrosive pigment has the following parameters: mass fraction of iron compounds in terms of Fe2O3not less than 85 wt.%, sieve residue after wet screening with openings 63 µm depending on the class can be:

class 1 - no more than 5 wt.%,

class 2 - more than 5 wt.%, but less than or equal to 15 wt.%,

class 3 - more than 15 wt.%, but less than or equal to 35 wt.%.

The content of fine scaly plates gradation of the following: - more than 65 wt.%, In 50 wt.% to 65 wt.%.

Used iron oxide in the paint industry as a protective pigment to provide anti-corrosion properties of the coating. It is added to the primer and/or enamel.

The aim of the invention is to obtain iron oxide pigment of different colors (pronounced metallic sheen, not a pronounced metallic sheen (satin sheen), brown, red) from one natural material - specularite.

The aim of the invention is to expand the scope of an anticorrosive pigment derived from specularity.

Final products:

- pigment with a pronounced angular metallic luster is the content of α-Fe2About3more than 60 wt.% and a particle size of 100 μm - 1000 μm, designed for decorative and protective and decorative coatings.

- pigment unexpressed angular metallic sheen (satin sheen) has a content of α-Fe2About3more than 60 wt.% and a particle size of 20 μm is less than 100 microns, designed for decorative and protective and decorative coatings.

- brown pigment has a content of Fe2O3more than 70 wt.% and a particle size of 0.3 μm is less than 20 microns, is designed for protective and decorative coatings.

- the red pigment has a content of α-Fe2About3more 94,0 wt.% and a particle size of less than 0.3 μm, is suitable for the pigmentation of various materials, such as paint, construction.

- pigment matte luster, consisting of iron sludge with the content of Fe2O3more than 85 wt.%, which includes a thin scaly plates more than 50 wt.% and characterized by residue after wet sieving sieve with openings 63 μm is not more than 35 wt.%, designed for decorative and protective and decorative coatings.

This is e the invention concerns a method of obtaining iron oxide pigment from specularite, including the grinding and enrichment in this first grinding lead to a particle size greater than 1 mm - 5 mm, followed by enrichment method of magnetic separation to the content of α-Fe2About3more than 60.0 wt.%, then the enriched specularite again crushed.

The present invention also relates to the aforementioned method of producing iron oxide pigment from specularite, where as specularite use specularity Altai Deposit Ore Log.

The present invention also relates to the aforementioned method of producing iron oxide pigment from specularite, where the enrichment is carried out before the content of α-Fe2About3more than 60.0 wt.%, and grinding after enrichment up to a particle size of 100 μm - 1000 μm.

The present invention also relates to the aforementioned method of producing iron oxide pigment from specularite, where the enrichment is carried out before the content of α-Fe2About3more than 60.0 wt.%, and grinding after enrichment to the particle size of 20 μm is less than 100 microns.

The present invention also relates to the aforementioned method of producing iron oxide pigment from specularite, where the enrichment is carried out before the content of α-Fe2About3more 70,0 wt.%, and grinding after enrichment to the size of particles 0.3 microns - less than 20 microns.

The present invention also relates to wiseup the mentioned method of producing iron oxide pigment from specularite, where the enrichment is carried out before the content of α-Fe2About3more 94,0 wt.%, and grinding after enrichment to particle size less than 0.3 microns.

The present invention also relates to pigment with a matte sheen for decorative and protective and decorative coatings obtained from enriched specularite and consisting of iron sludge with the content of Fe2O3more than 85 wt.%, which includes a thin scaly plates more than 50 wt.% and characterized by residue after wet sieving sieve with openings 63 μm is not more than 35 wt.%.

The present invention also relates to the above-mentioned pigment with a matte sheen, where as specularity can be used specularite Altai Deposit Ore Log.

The range of particle size of the material and its relationship with the color obtained by experiment.

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.

Spent an analysis of the prior art, including searching by the patent and scientific and technical information sources and identify sources that contain information about the equivalents of the claimed invention, has allowed to establish that the petitioners have not found the source, which is characterized by the signs of the, identical essential features of the claimed invention. The definition from the list of identified unique prototype, as the most similar set of features analogue, has allowed to establish the essential towards perceived by the applicants to the technical solution of the distinctive features in the proposed method, set forth in the claims. Not detected the use of a known material for a new purpose set forth in the independent claim.

Therefore, the claimed invention meets the condition of "novelty."

The invention is illustrated by the following examples:

Example 1. The way to obtain iron oxide pigment from specularite with angular metallic luster was carried out as follows. Took a natural material - specularite of career Altai Deposit Ore Log particle size of less than 600 mm and held his ground in a mill, semi-autogenous grinding cantilever type. From autogenous mills specularite was sent to the classifier, the classifier used the hydrocyclone, which was a division of specularite by size. The whole specularite larger than 1 mm - 5 mm was returned for regrinding in the mill, semi-autogenous grinding, specularite with a particle size greater than 1 mm - 5 mm from the classifier was sent to Agnico separation for carrying out the process of enriching the content of α-Fe 2About3more than 60.0 wt.%. After that specularite sent for grinding after enrichment in a planetary mill to obtain specularite particle size of 100 μm - 1000 μm.

It is found experimentally that the best degree of enrichment is achieved by grinding specularite until the particle size is 2 mm.

Table 1 shows the chemical composition of monomineral fractions of specularite Deposit Ore Log.

Example 2. The way to obtain iron oxide pigment from specularite with slightly pronounced angular metallic sheen (satin sheen) was carried out as follows. All operations of example 1, but grinding after enrichment in the planetary mill was performed to obtain specularite particle size of 20 μm is less than 100 microns.

Example 3. The way to obtain iron oxide pigment from specularite brown was carried out as follows. All operations of example 1, but the enrichment process was performed in a magnetic separator to the content of α-Fe2About3more 70,0 wt.%, and grinding after enrichment in the planetary mill was carried out to obtain specularite particle size of 0.3 μm is less than 20 microns.

Example 4. The way to obtain iron oxide pigment from specularite red was carried out as follows. All operations of example 1, but the enrichment process was performed in a magnetic with whom paratore to the content of α-Fe 2About3more 94,0 wt.%, and grinding after enrichment in the planetary mill was carried out to obtain specularite particle size less than 0.3 microns.

Example 5. Pigment with a matte sheen was obtained by use of anticorrosive pigment composed of iron sludge Altai Deposit Ore Log" with the content of Fe2O3more than 85.0 wt.%, the content of fine scaly plates more than 50 wt.% and the sieve residue after wet screening with openings 63 μm is not more than 35 wt.%. Protective and decorative properties of this pigment is manifested in that the coating through the use of this pigment becomes not only decorative (matte Shine, roughness), but also high resistance to abrasion and scratching.

Studies have shown that specularite, in particular from specularite Altai Deposit Ore Log", you can get the pigment decorative, protective and decorative with a pronounced angular metallic luster; ornamental and decorative with a matte sheen; protective, decorative brown and red colors; use anticorrosive pigment is an iron oxide with a content of Fe2O3more than 85.0 wt.%, the content of fine scaly plates more than 50 wt.% and the sieve residue after wet screening with openings 63 μm is not b is than 35 wt.% as a decorative pigment with a matte sheen and/or protective and decorative pigment.

Experimentally it is found that the optimum content of α-Fe2About3the pigment should be 85,0-95,0 wt.%.

The pigment obtained from specularite, has advantages in the following:

- Environmentally friendly. The content of harmful and hazardous substances (Hg, As, U, Cd and others) in ore "Ore Log" not found.

- It is not water-soluble impurities, causing salt efflorescence on the surface of products.

- Permanent.

Pigment with a pronounced angular metallic paint with a matte sheen used for the production of building materials, new building materials to give them a decorative and protective and decorative properties, is used to produce decorative and protective and decorative coatings in the paint industry. Pigment with a matte sheen and with a pronounced angular metallic Shine well dispersed, for example, in the varnish. The resulting suspension is homogeneous, stable and not prone to separation. Paint obtained by adding a pigment with a pronounced angular metallic luster and matte sheen, were used to create decorative coating on a cast iron grate.

Pigment with a pronounced angular metallic luster and matte sheen used to create paints and coatings for the of Ernesta of different materials, in order to give them a certain degree of decoration and different degrees of roughness.

Table 2 summarizes the qualitative characteristics of the brown pigment. This pigment can be used as a brown pigment in the production of building materials for dyeing: roofing tiles, floor tiles, wall plasters, cement-based, concrete products, as a protective antirust iron oxide pigment in the paint industry.

The red pigment used for the pigmentation of paints and varnishes. Red pigment obtained by the present invention was tested for compliance with THE 2322-166-05011907-98 "Pigment iron oxide red. The tests showed that the red pigment from specularite Altai Deposit Ore Log" complies with THE 2322-166-05011907-98.

Used the pigment from specularite Altai Deposit Ore Log" with a matte sheen and size 60-65 microns in GF-021 for protective purposes. The tests showed that the coating GF-021 using pigment from specularite showed some advantage in comparison with coatings GF-021 standard recipe in the hardness and strength of the coating to abrasion. The hardness of the coating film GF-021 with specularite defined by pendulum device M-3, was 0.400 Uslon is x units, whereas the coating GF-021 standard recipe - 0.347 conventional units. The strength of the film to abrasion quartz sand (kg/μm) coating GF-021 with specularite - 0,769, and cover with a standard recipe - 0,608.

The resistance of film to the static action of 3%-aqueous solution of sodium chloride compliance with the requirements of GOST 25129-82. Excess test for this position showed that the coating GF-021 with pigment from specularite resistant to the effects of NaCl up to 48 hours, whereas the coating GF-021 standard recipe immediately observed pomalowania coverage.

Used anticorrosive pigment is an iron oxide obtained from specularite Altai Deposit Ore Log" with the content of Fe2O3more than 85 wt.%, the content of fine scaly plates more than 50 wt.% and the sieve residue after wet screening with openings 63 μm is not more than 35 wt.% as a decorative pigment with a matte sheen. Was created decorative paint by using this pigment-based varnish. This paint was covered with a grille made of cast iron. The floor had a small degree of roughness, dull luster.

All of these pigments are introduced as the only pigments and allow the production of the color corresponding to the particle size of the pigment. Count the number of pigment, enter, for example, the composition of the decorative paint can be from 10 to 20 wt.%.

The choice of pigment largest particle sizes and thus the color depends on the purpose of the pigment and the area of its use.

The main component accompanying specularite is SiO2. Experimentally it was found that the presence of SiO2in the amount of 30-40 wt.% in the pigment with a pronounced angular metallic Shine and pigment with a matte sheen, used for decorative coatings in the paint industry, as a pigment in the manufacture of building materials, does not degrade the quality of the pigment and the quality of coatings with their use, and Vice versa, creates additional light reflecting effect.

In addition, it should be noted that in the process of obtaining pigment remains SiO2good quality, which can be successfully used in various industries and construction.

The production of iron oxide pigment from specularite meets the following environmental requirements: food safety deletecell, no waste, because in the process of crushing any fraction in the range of less than 0.3 μm - 1000 μm can be used as a pigment in a particular area of industry and construction as well as the main ingredient that accompanies specul the RIT - SiO2.

From specularite Altai Deposit Ore Log" you can obtain micronized pigment, which is successfully applied in different industries and construction.

Thus, the claimed technical solution allows you to:

1) to provide natural iron oxide pigments of different colors of the same material - specularite and, in particular, from specularite Altai Deposit Ore Log": red, brown, with a matte sheen and with a pronounced angular metallic Shine,

2) to expand the scope of application of low-cost corrosion-resistant iron oxide pigments derived from specularity, in particular from specularite Altai Deposit Ore Log", through the use of known anti-corrosive pigment - iron sludge with the content of Fe2O3more than 85 wt.%, the content of fine scaly plates more than 50 wt.% and the sieve residue after wet screening with openings 63 μm is not more than 35 wt.% as a decorative and protective decorative pigment.

The pigment according to this invention suitable for use in the paint industry, construction and other industries.

Table 1
The chemical composition manomin the liberal factions of specularite Ore deposits Log (wt.%)
CompositionSpecularite
Fe2About395.0-99.2
SiO22.62-0.41
Al2O30.12-0.03
FeO1.52-acting
Tio20.08-0.01
CaO0.07-0.01
MnOthe concentration is
MgOthe concentration is
Na2Othe concentration is
K2Othe concentration is
P2O5the concentration is
BaOthe concentration is
SrOthe concentration is
S(Val)the concentration is
Fthe concentration is
Clthe concentration is
H2Othe concentration is
PPP0.36-0.19
Amount99.77-99.85

Table 2
Qualitative indicators of the brown pigment
№ p/pName of indicatorActually defined
1ColorBrown
2Mass fraction of iron compounds in terms of Fe2O372,0 and more, depending on the degree of enrichment
3Mass fraction of water soluble substances, %0,1
4Mass fraction of volatile substances, %0,6
5pH of the aqueous suspension7,5
6Weight loss on ignition, %0,6
7The oil absorption, g/100 g pigment 18
8Rate, g/m215
9Dispersibility, mcm25

1. The way to obtain iron oxide pigment from specularite, including the grinding and milling, wherein the first grinding lead to a particle size greater than 1 to 5 mm, and then spend the enrichment method of magnetic separation to the content of α-Fe2About3more than 60.0 wt.%, then the enriched specularite again crushed.

2. The method according to claim 1, characterized in that as specularite use specularity Altai Deposit Ore Log.

3. The method according to claim 1, characterized in that the enrichment is carried out before the content of α-Fe2About3more than 60.0 wt.%, and grinding after enrichment to particle size of 100 to 1000 microns.

4. The method according to claim 1, characterized in that the enrichment is carried out before the content of α-Fe2About3more than 60.0 wt.%, and grinding after enrichment to particle size of 20 μm is less than 100 microns.

5. The method according to claim 1, characterized in that the enrichment is carried out before the content of α-Fe2About3more 70,0 wt.%, and grinding after enrichment to particle size of 0.3 microns - less than 20 microns.

6. The method according to claim 1, characterized in that the enrichment is carried out before the soda is Jania α-Fe 2About3more 94,0 wt.%, and grinding after enrichment to particle size less than 0.3 microns.

7. Pigment with a matte sheen for decorative and protective and decorative coatings obtained from enriched specularite and consisting of iron sludge with the content of Fe2About3more than 85 wt.%, which includes a thin scaly plates more than 50 wt%, and characterized by residue after wet sieving sieve with openings 63 μm is not more than 35 wt%.

8. The pigment according to claim 7, characterized in that it is obtained from specularite Altai Deposit Ore Log".



 

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The invention relates to technology of inorganic substances and can be used to obtain iron coagulants-flocculants for water treatment, deposition of mineral solids from aqueous suspensions and concentration of dissolved metals in them

The invention relates to metallurgy, in particular to methods of producing iron oxide (III) for ferrites with low content of impurities from spent hydrochloric acid pickling solutions rolling production

FIELD: metallurgy; building industry; varnish and paint industry.

SUBSTANCE: the invention is pertaining to the field of metallurgy, building industry, varnish and paint industry, in particular, to the method of production of a red ferrioxide pigment. A ball mill is charged with industrial water, loaded with iron oxide with concentration of 500-900 g/dm3, poured with a neutralizing agent in the amount ensuring pH 6 ÷ 10. The iron oxide is formed at a thermal decomposition of the hydrochloride solutions used at etching treatment of carbon steels. As a neutralizing agent it is possible to use caustic soda, a slaked lime, microcalcite. The suspension is pulped for 3-5 hours, put in a reactor with a stirrer, where it is washed out with formation of a suspension, filtered off and dried. The target product has the following parameters: pH 5 ÷ 8; the share of water-soluble salts - 0.02-0.03 %; dispersing ability - 27-30 microns; hiding power - 6 ÷7 g/m2. The invention allows to simplify process and to upgrade parameters of the pigment.

EFFECT: the invention allows to simplify process and to upgrade parameters of the pigment.

2 cl, 1 tbl, 1 ex

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