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INVENTION
Russian Federation Patent RU2236426

METHOD FOR PRODUCING weather resistant pigments from sphene CONCENTRATE

METHOD FOR PRODUCING weather resistant pigments from sphene CONCENTRATE

Name of the inventor: Galinurova LA (RU); Alekseev AI (RU); Brylyakov YE (RU); Bulls ME (RU); Vasilyeva N. (RU); Plahin VF (RU); Sakovsky YN
The name of the patentee: Open Joint Stock Company "Apatit"
Address for correspondence: 184250, Murmansk, Kirovsk, Str.. Leningrad, 1, OAO "Apatit", Technical Department
Starting date of the patent: 2002.03.11

The invention is designed for the chemical and paint industries. Sphene concentrate with Fe 2 O 3 is not more than 1.5 wt.% Was heat treated at 400 ° C for 40 minutes. Modifier added - a mixture of particles containing 5-30 wt% silica gel calcined at 800-900ºS coated with 5.1 wt% cobalt phosphate, with particles containing the dried mixture at 100-120ºS triphosphate 35-45% by weight... alumina and 20-30 wt.% of the silica gel coated with 10-20 wt.% of chromium phosphate. The modifier can enter the 1-3% by weight of powdered fluorescent fluorescent organic pigment -. Belofora to convert the absorbed portion of light in the visible radiation. Was dry milled to ultrafine particle size less than 10 microns. 87-96 RLU white pigment, oil absorption - 20-24 g / 100 g pigment yellowness - RLU 10-18, for 4 hours lightfastness - 0.25-0.3 RLU, paint stability delamination - 6 months. Paint made from the resulting pigment is tested in the apparatus of artificial weather. After 500 hours, the film does not differ from the original in color and smoothness

DESCRIPTION OF THE INVENTION

The invention relates to preparation of inorganic materials, in particular pigments used in the paint industry.

A large number of chemical processing methods sphene concentrate to give the titanium dioxide pigment or containing compositions. All of these methods are characterized by varying degrees of difficulty associated with the use of aggressive inorganic acids, acid-resistant special equipment used in numerous operations to produce a significant amount of weakly acid waste, polluting the environment. All this increases the cost of technological conversion and thus increases the price of the finished product. Produced by one of the technologies titanokaltsievy pigment has limited use (for indoor painting), i.e. coatings based on it neatmosferostoykie [Motov DL, GK Maximov Sphen and chemical processing on titanium pigments. M .: Nauka, 1983, 88 pp.].

On the other technologies are weatherproof rutile, but because of the low content of TiO 2 in sphene concentrate and extract the degree of TiO 2 ~ 70% of the finished product yield is 200 kg of 1 ton of sphene concentrate [AS N 1331828, BI 31, 1987. A method of processing sphene concentrate AS N 1621909, BI 45, 1990. A method of processing sphene concentrate].

The closest to the claimed technical solution is a method for producing weather-resistant pigment of sphene concentrate - US Pat. RU №2177016. The process involves dry milling sphene concentrate and heat treatment, after which a suspension concentrate modifier consisting of aluminum phosphate and silica gel in an amount of 15-30% by weight of the concentrate, the resulting paste is dispersed for 2-5 hours and then subjected to heat treatment at 50-500ºS. The pigments obtained by this method acquire high light fastness, low photochemical activity, anti-corrosive properties and may be used as weatherable pigments. The properties of the pigment are shown in Table 1 below.

The disadvantages of the described method include the following:

- Crushed sphene concentrate processed modifier and subjected to heat treatment at 50-350ºS retains a grayish hue due to the fact that it has a dominant streak of light absorption = 450-600 and additional = 700 to give a mixture of three primary colors: yellow, red, blue and green with an impurity, which leads to the formation of a gray color and the inability to obtain razbele paints (coatings) with sufficient color purity;

- Crushed sphene concentrate processed modifier and subjected to heat treatment at 350-500ºS by introducing into the crystal lattice of impurity oxides, causing the deformation of the crystal lattice, it becomes yellow, which also reduces the purity of the colors in the paint razbele.

- Sphene milled concentrate modifier treated and subjected to heat treatment, and sintered poorly to disaggregate, leading to a reduction of the finished pigment dispersibility.

The present invention is directed at reducing the yellowness, whiteness and improvement of color purity, light fastness, dispersion, pigment sedimentation stability in paint, resistance to photochemical processes, enlargement range based coatings of this pigment with the increase of their quality.

Reduced yellowness is achieved by subtracting the unwanted portion of the spectrum modifier - an optical brightener: bluish-green phosphate chromium dried in the presence of aluminum triphosphate and silicic acid subtracted reddish color pigment composition and a light purple phosphate cobalt calcined in the presence of silicon oxide, is subtracted yellow shade.

Improved whiteness and purity of the pigment is achieved by increasing the degree of reflection of all wavelengths of light in the visible part of the spectrum as a result of heat treatment for 40 minutes at 400 ° C, increase the scattering power of the shortwave light by reducing the average radius of pigment particles in an ultrathin grinding, create enough microregions with unequal refractive indices, reducing light absorption in the short-wave part of the visible spectrum and in the ultra-violet region, due to the composition of the modifier and subtracting the unnecessary part of the spectrum with an optical whitening light purple phosphate, cobalt calcined in the presence of silica and blue-green phosphor chromated , in the presence of dried aluminum triphosphate and silicic acid.

2. The method of claim 1, a brightness increase achieved by introducing a fluorescent powder of the fluorescent organic pigment belofora-converting part of the absorbed radiation into visible light.

Increased dispersibility, reduced lyophobic and as a result, eliminating delamination, sedimentation and aggregation of pigment particles in paint formulations is achieved by the presence of modifier calcined silica dried silica and hydrated triphosphate aluminum which plakiruya pigment particles prevent adhesion of the latter, increasing the degree peretiraemosti and in paint formulations act as a stabilizer dispersions, increasing sedimentation stability of pigments, improving the thixotropic properties, favorably affecting the ability of coatings applied with a brush and prevent the swelling it with a vertical surface.

Improved lightfastness and photochemical reduction process is achieved by the presence of the phosphate modifier cobalt, chromium phosphate, aluminum triphosphate and silicon dioxide processes which prevent browning and color changes, as a corrosion inhibitor or inhibitors photochemical processes.

This object is achieved in that the first heat treatment is carried out at a temperature sphene concentrate at 400C for 40 minutes and then grinding in presence of a modifier - an optical otbelivagelya which is administered in an amount of 10-20% by weight of the concentrate, until a produce grinding fineness below 10 m. Modifier - optical brightener mixture comprises 5-30% by weight of particles of silica gel calcined at 800-900ºS coated with 5.1 wt% cobalt phosphate, with particles containing the dried mixture at 100-120ºS triphosphate 35-45% by weight... alumina and 20-30 wt.% of the silica gel coated with 10-20 wt.% of chromium phosphate.

Thermal treatment above 400 ° C leads to a strong deformation sphene crystal lattice and, consequently, a more intense staining in the yellowish-brown color. The temperature treatment below 400 ° C does not provide sufficient clarification.

Cobalt phosphate content of less than 1 (wt.%), Leads to the need to increase the percentage of the modifier in the pigment, and more than 5% (wt.%) Results in a change of color change n wavelengths which it will be subtracted from the light spectrum.

Chromium phosphate content less than 10% (wt.%), Leads to the need to increase the percentage of the modifier in the pigment, and more than 20% leads to a change of color and change in the wavelengths which it will be subtracted from the light spectrum.

The content of silicon dioxide and aluminum triphosphate has no significant role.

Addition of a modifier - an optical brightener in an amount of <10% (.% By weight) increases the grinding time, does not provide sufficient pigment white, not fully reduced yellowness insufficiently improves lightfastness and sedimentation stability of the finished coatings, and> 20% leads to a characteristic greenish -golubovatogo shade and enhance oil absorption.

The method is as follows. Source sphene concentrate was heat treated at 400C for 40 minutes was added to the concentrate ostyvshemu modifier - an optical brightener, which is prepared from a mixture of particles of 5-30% by weight of silica gel calcined at 800-900ºS coated with 1.5 wt% of phosphate.. cobalt particles containing mixture 100-120ºS dried at 35-45 wt.% of aluminum triphosphate and 20-30 wt.% of the silica gel coated with 10-20 wt.% of chromium phosphate.

The mixture was charged into an apparatus for dry grinding, and the grinding is conducted until the particle size less than 10 microns.

Properties of the obtained pigment are shown in Table 2.

The essence of the proposed method is illustrated by the following examples.

Example 1. Take 1 kg of concentrate sphene, Fe 2 O 3 content of no more than 0.6%, it was subjected to heat treatment at 400C for 40 minutes. Ostyvshemu To the concentrate was added 100 g (10 wt.%) A modifier - an optical brightener, which consists of a mixture of particles containing 5% by weight of silica gel calcined at 800-900ºS coated with 1 wt% cobalt phosphate particles containing.. 100-120ºS dried mixture with 45 wt.% of aluminum triphosphate and 30 wt.% of the silica gel coated with 20 wt.% of chromium phosphate.

The resulting mixture was dry milled to yield ultra-thin material with a dispersity less than 10 microns. The refractive index of sphene concentrate - 2.1. the refractive index of the pigment is reduced slightly to 2.0. Spreading rate of 100 g / m 2, white 88 standard units, yellowness 18 standard units, an oil absorption of 20 g / 100 g pigment.

On the basis of the pigment prepared in oil paint using a synthetic varnish on the serial formulation. iron oxide pigment green 7% was added to the total weight of the fast light yellow pigment and 3% by weight of the total pigment. The paint had ukryvnstost 70 Change Condition units. With the same technical specifications and color of oil paint was prepared for reference on the basis of traditional pigments: imported rutile, chalk, imported green iron oxide pigment and yellow fast light. Clean test sample color was 95% of the standard. It is noted that to achieve the desired opacity and color saturation chromatic iron oxide pigment used in the standard formulation in 2 times more. Paint has been tested in the apparatus of artificial weather. After 500 hours, the film does not differ from the original in color and smoothness.

Example 2. Take 1 kg of concentrate sphene, Fe 2 O 3 content of no more than 0.6%, it was subjected to heat treatment at 400C for 40 minutes. Ostyvshemu To the concentrate was added 150 g (15 wt.%) A modifier - an optical brightener which is obtained from a mixture of particles containing 30% by weight of silica gel calcined at 800-900ºS coated with 5 wt% cobalt phosphate particles containing.. 100-120ºS dried mixture with 35 wt.% of aluminum triphosphate and 20 wt.% of the silica gel coated with 10 wt.% of chromium phosphate.

The resulting mixture was dry milled to yield ultra-thin material with a dispersion of 0.5-5 microns. The refractive index of sphene concentrate 2.1. the refractive index of the pigment is reduced slightly to 2.0-2.05. Spreading rate of 90 g / m 2, white 90 standard units, yellowness 14 standard units, an oil absorption of 22 g / 100 g pigment.

On the basis of the pigment prepared in oil paint using a synthetic varnish on the serial formulation. red iron oxide pigment has been added. Paint coverage was 70 conv. u With the same technical specifications and color of oil paint was prepared for reference on the basis of traditional pigments: imported rutile, chalk, imported red iron oxide pigment. Clean test sample color was 95% of the standard. It is noted that to achieve the desired opacity and color saturation chromatic iron oxide pigment used in the standard formulation in 2 times more. Paint has been tested in the apparatus of artificial weather. After 500 hours, the film does not differ from the original in color and smoothness.

Example 3. Take 1 kg of concentrate sphene, Fe 2 O 3 content of no more than 1%, it is subjected to heat treatment at 400C for 40 minutes. Ostyvshemu To the concentrate was added 200 g (20 wt.%) -optical Bleach modifier which is prepared from a mixture of particles containing 5 wt.% Silica gel calcined at 800-900ºS coated with 1 wt.% Cobalt phosphate particles containing 100-120ºS dried mixture with 45 wt.% of aluminum triphosphate and 30 wt.% of the silica gel coated with 20 wt.% of chromium phosphate. Add 100 g of titanium dioxide (10 wt.%).

The resulting mixture was dry milled to yield ultra-thin material with a dispersion of 0.5-5 microns. The refractive index of sphene concentrate 2.1. The refractive index of the pigment is not reduced. Spreading rate of 70 g / m 2, 96 conventional units whiteness, yellowness 10 standard units, an oil absorption of 24 g / 100 g pigment. On the basis of this pigment is prepared using oil paint as a binder of synthetic varnishes, and a water-dispersion paint (binder - latex SKS-65GPB). On the basis of the same reference binder paint samples were prepared, which is used as a pigment imported rutile, and chalk as filler. Spreading rate of 70 g / m 2. Both the test sample differed from the reference slight bluish-green tint. Paints tested in the apparatus of artificial weather. After 500 hours, the film does not differ from the original in color and smoothness.

Example 4. Take 1 kg of concentrate sphene, Fe 2 O 3 content of no more than 1.5%, it was subjected to heat treatment at 400C for 40 minutes. Ostyvshemu To the concentrate was added 200 g (20 wt.%) A modifier - an optical brightener which is obtained from a mixture of particles containing 5% by weight of silica gel calcined at 800-900ºS coated with 1 wt% cobalt phosphate particles containing.. 100-120ºS dried mixture with 45 wt.% of aluminum triphosphate and 30 wt.% of the silica gel coated with 20 wt.% of chromium phosphate.

The resulting mixture was dry milled to yield ultra-thin material with a dispersion of 0.5-5 microns. The refractive index of the pigment 2.0. Spreading rate of 90 g / m 2, white 93 standard units, yellowness 12 standard units, an oil absorption of 22 g / 100 g pigment. On the basis of this pigment is prepared using oil paint as a binder of synthetic varnishes, and a water-dispersion paint (binder - latex SKS-65GPB). In addition, 10% of iron oxide green pigment paint was spreading rate of 70 standard units was introduced With the same technical specifications and color, based on the same binder was prepared paint for reference on the basis of traditional pigments: imported rutile, chalk, imported green iron oxide pigment. Both color purity of the test specimens was 95% of the standard is noted that to achieve the desired color and saturation ukryvnstosti chromatic iron oxide pigment in formulations used as standards two times. Paints tested in the apparatus of artificial weather. After 500 hours, the film does not differ from the original in color and smoothness.

Example 5. Take 1 kg of concentrate sphene, Fe 2 O 3 content of no more than 0.6%, it was subjected to heat treatment at 400C for 40 minutes. By ostyvshemu concentrate was added 100 g (10 wt.%) A modifier - an optical brightener which is obtained from a mixture of particles containing 5 wt.% Of the gel of silica calcined at 800-900 º C, coated with 1 wt.% Of phosphate, cobalt particles, comprising 100-120ºS dried mixture with 45 wt.% of aluminum triphosphate and 30 wt.% of the silica gel coated with 20 wt.% of chromium phosphate. Add 3% organic fluorescent pigment powder belofora.

The resulting mixture was dry milled to yield ultra-thin material with a dispersity less than 10 microns. The refractive index of sphene concentrate 2.1. the refractive index of the pigment is reduced slightly to 2.0. Spreading rate of 100 g / m 2, white 87 standard units, yellowness 18 standard units, an oil absorption of 20 g / 100 g pigment. Visual pigment looks much whiter than in the example №1.

EXAMPLE 6 Take 1 kg of concentrate sphene, Fe 2 O 3 content of no more than 1.5%, it was subjected to heat treatment at 400C for 40 minutes. Ostyvshemu To the concentrate was added 200 g (20 wt.%) A modifier - an optical brightener which is obtained from a mixture of particles containing 5% by weight of silica gel calcined at 800-900ºS coated with 1 wt% cobalt phosphate particles containing.. 100-120ºS dried mixture with 45 wt.% of aluminum triphosphate and 30 wt.% of the silica gel coated with 20 wt.% of chromium phosphate. Add 1% of fluorescent organic powder pigment belofora

The resulting mixture was dry milled to give material with dispersibility ultragonkogo 0.5-5 microns. The refractive index of the pigment 2.0. Spreading rate of 90 g / m 2, white 93 standard units, yellowness 12 standard units, an oil absorption of 2 g / 100 g pigment visual pigment is perceived much whiter than the pigment shown in Example 4.

These examples show that the proposed method as well as the method gives the prototype coating system sedimentation stability, but compared with the prior art can improve whiteness, lower yellowness. Increasing oil absorption due to the higher dispersion. Light resistance is within the permissible limits for atmospheric colors. These benefits are achieved by way of the selected parameters.

CLAIM

1. A method of producing a weatherable sphene pigment concentrate, comprising adding to sphene modifier concentrate containing phosphate and silica, ultra-fine grinding in the dry mode and heat treatment, characterized in that the first sphene concentrate was heat treated at 400 ° C for 40 minutes, whereupon modifier, which is used as a mixture of particles containing 5-30 wt.% of the silica gel calcined at 800-900ºS coated with 5.1 wt.% cobalt phosphate, with particles containing the dried mixture at 35-45 wt 100-120ºS .% aluminum triphosphate, and 20-30 wt.% of the silica gel coated with 10-20 wt.% of chromium phosphate.

2. The method of claim 1, wherein the modifier is introduced in 3.1 wt% organic fluorescent powder fluorescent pigment -. Belofora which converts part of the absorbed radiation into visible light.

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Publication date 18.01.2007gg