Method for treating of titanium dioxide

FIELD: production of pigments and catalysts based on titanium dioxide, in particular, process for treatment of titanium dioxide for removal of sulfur, in particular sulfates.

SUBSTANCE: method involves treating calcined titanium dioxide at elevated temperatures using aqueous solution containing one or more ammonium compounds; separating titanium dioxide from aqueous solution and drying titanium dioxide. Ammonium compounds preferably used in treatment process are ammonium acetate or ammonium chloride.

EFFECT: increased efficiency in cleaning of titanium dioxide from sulfur, in particular sulfates.

9 cl, 5 tbl, 5 ex

 

The technical field to which the invention relates.

The present invention relates to a method of purification of titanium dioxide from sulfur in the washing of titanium dioxide using an aqueous solution of one or more ammonium compounds, separation of titanium dioxide and washing liquid and drying the titanium dioxide. To a greater extent, the invention relates to the removal of the titanium dioxide sulfur (mainly present in the form of sulfate compounds).

The level of technology

It is well known the use of pigments in paints, varnishes, inks, building materials, rubber and the like. As the dyes are widely used organic and inorganic compounds. Usually the pigment consists of (very) small particles, which are practically insoluble in damage to the environment, this is their contrast dyes, which are soluble in the applied environment.

Basic white inorganic pigment is titanium dioxide or titanium dioxide). To obtain titanium dioxide in an industrial scale using two methods. See, for example, Ullmann′s Encyclopedia of Industrial Chemistry, Fifth edition, Vol. A20, pages 271-281.

In "chloride method" of such raw materials such as ilmenite, leucoxene, natural and synthetic rutile, titanium slag and anatase, glorious at 700-1200°the. The titanium tetrachloride separated from other chlorides by distillation. The titanium tetrachloride, optionally after further purification, burned using oxygen-containing gas at temperatures in the range from 900 to 1400°obtaining titanium dioxide. The pigment obtained in this way, very clean. Depending on the type of application may be required and some additional processing.

In another way - "sulfate way" - titanium containing raw materials, particularly ilmenite and titanium slag is dissolved in concentrated sulfuric acid at 150-220°C. Remove insoluble particles and deposition of sulphate of iron in the results allow to obtain a concentrated solution of titanyl sulphate. As a result of hydrolysis of the sulfate solution at approximately 100°To precipitate relatively pure dihydrate, titanium dioxide (also referred to as "metatitanate acid"). Other impurities, in particular sulfates of metals, mainly to remove the additional steps of purification, particularly in the wash by using a diluted acid or leachate. The hydrate is filtered (usually using a rotary vacuum filter) until then, until you get the content of titanium dioxide (anhydrous TiO2) 30-40 wt.%, calcined, pulverized and subjected to stage niceley processing depending on the type of application. The calcination (in the appropriate case, at temperatures below 1000°With, in particular in the range from 400 to 700°With, in the range from 0.1 to 3 hours) is usually carried out in rotary kilns. Approximately two-thirds of the time (often 7-20 hours total) required for drying the material. Above 500°removes sulfur trioxide, which is partially decomposed to sulfur dioxide and oxygen at higher temperatures. In another kind of way obtained the hydrate of titanium dioxide suspended in water and subjected to spray drying, optionally followed by calcination.

In addition to the use of titanium dioxide as a pigment, there are also other applications. Therefore another application of titanium dioxide is used as a catalyst carrier. The problem with the use of titanium dioxide as a catalyst carrier, in particular of titanium dioxide obtained in the sulfate method is the high content in the titanium dioxide sulphur, in particular sulfate. The presence of sulfur or adsorbed sulfuric acid or sulfates of metals, or in any other form often adversely affects the performance characteristics of the catalyst obtained with the use of media on the basis dioxide t is Tana. Negative influence can be exerted on the activity, selectivity and/or stability. In some cases regeneration using treatment with hydrogen in the results of hydrogen sulfide, which has a negative impact on the performance of the catalyst.

Presently discovered that the treatment of titanium dioxide at elevated temperatures using an aqueous solution containing one or more ammonium compounds, followed by separation of the titanium dioxide from aqueous solution and drying the titanium dioxide in the results (optional) purified titanium dioxide, in which at least significantly reduced sulfur content. In addition, also can greatly be reduced and the number of unwanted metal (metals other than titanium, in particular iron and sodium).

Disclosure of inventions

The present invention particularly suitable for titanium dioxide, obtained by using the sulfate method. Titanium dioxide, obtained in accordance with this method, and commercially available on the market, generally contains from 0.4 to 2 wt.% sulfur (elemental sulfur). In the method corresponding to the present invention, the titanium dioxide can be treated once or more is eaten once. In the General case, after each treatment (washing and highlighting) the amount of sulfur is reduced by 20-98%. After a certain number of times of performing the treatment under the impression that the remaining amount of sulfur (elemental sulfur) is usually in the range from 0.02 to 0.04 wt.%, no longer decreases. It seems that the remaining amount of sulfur incorporated in the inner space of the primary particles, and cannot be removed using the method of simple washing. The amount of sodium is usually reduced by 50-90 wt.%, the amount of iron is usually reduced by 10-80 wt.%.

As mentioned above, the titanium dioxide can be obtained by deposition, cleaning sludge, filtration and calcination. In a modified method of titanium dioxide was obtained, carrying out spray drying or heat drying cleaned of sludge, in particular their suspension filtered precipitate, optionally followed by calcination.

Titanium dioxide used in the method of the present invention, commercially available. Titanium dioxide typically contains at least 90 wt.% TiO2preferably 95 wt.%, more preferably from 96 to 99 wt.% TiO2. The size of the agglomerates is insignificant, but in an appropriate case, it is in the range from 1 to 200 microns, in a more appropriate case from 3 to 30 microns. Also m is tenderly to use larger or smaller agglomerates, but, taking into account the performance of the stage washing and necessary stage of selection, they are less desirable. In General, titanium dioxide was progulivali before cleaning at temperatures at least equal to 300°S, preferably 500°C. you Can use the anatase, rutile, and all types of compounds or intermediates. The amount of sulfur (elemental sulfur) is in the range from 0.2 to 4 wt.%, preferably from 0.3 to 3 wt.%. In one or more stages of washing removes preferably 90% sulfur, more preferably 95%.

Processing of titanium dioxide through an aqueous solution in a suitable case are the result of mixing two components. Possible periodic methods, and continuous methods. In order to minimize the amount of fluid handling washing is preferably carried out using a countercurrent. Processing washing is usually carried out at a volume ratio liquid/solid phase, at least equal to 0.4, preferably in the range from 0.7 to 20, more preferably from 1 to 5. You can use the reaction apparatus with stirrer. Titanium dioxide and/or wash liquid can be added continuously and/or periodically. The suspension can be removed continuously and/or periodically. In addition to the reaction apparatus with stirrer also the you can use the equipment of the tubular form for washing with a relatively small degree of back-mixing. In addition, you can also use and ways of relating the type of leaching. the pH of the wash liquid is preferably in the range from 8 to 11, more preferably equal to 9.

In a preferred variant of realization of titanium dioxide is washed using pure water, after treatment by washing using an aqueous solution of ammonia. It allows you to put less stress on the stage of calcination, because you will burn fewer undesirable materials, and/or will be received more pure product. If desired, the treatment by washing using a solution of ammonium may be preceded by washing using pure water and/or pre-wetting or filling of the pore volume of titanium dioxide in the impregnation of a suitable liquid, such as pure water or preferably an aqueous solution of ammonia.

Processing by washing in the method of the present invention in a suitable case is carried out at elevated temperature in the range from 40 to 150°C, preferably from 60 to 110°S, more preferably from 80 to 95°C. Stage of processing by washing in a suitable case are in the range from 0.01 to 12 hours, preferably from 0.1 to 2 hours, more preferably from 0.4 to 1.5 hours, most preferably from 0.2 to 1.2 hours.

In prefer enom implementation spend several treatments of washing, to remove sulfate as best as possible. For each treatment by washing may be followed by a stage of annealing, but this is not preferable. Is preferred when the number of washes (with subsequent separation of titanium dioxide and an aqueous solution) comes up to 6, preferably 2 or 3. Processing the washing is preferably carried out at atmospheric pressure. If requested by the temperature, it is possible to use higher pressures. The processing of washing can also be carried out using aqueous leaching solution containing a mixture of water and one or more miscible with water and organic compounds. Miscible with water and organic compounds can be, for example, an alcohol, preferably an alcohol containing from 1 to 10 carbon atoms, more preferably an alcohol containing from 1 to 4 carbon atoms, in particular methanol or ethanol. In General, at least 50 wt.% aqueous leaching solution will be a water, preferably at least 70 wt.%.

Ammonium compounds used in this way, in an appropriate case, are obtained from compounds of trialkylamine, connection dialkylamino, connection alkylamine or compounds unsubstituted ammonium, preferably compounds unsubstituted ammonium. Besides the fact, you can use aromatic and/or alkyl/aromatic ammonium compounds, but preference is given to compounds of alkylamine or most preferably unsubstituted ammonium. More specifically, the above-mentioned alkyl groups in an appropriate case, contain from 1 to 12 carbon atoms, preferably from 1 to 6, more preferably from 1 to 3. The above-mentioned aromatic compounds in a suitable case, are phenyl or benzyl groups (especially substituted mono - or di-alkyl (C1to C6in particular, C1)), preferably phenyl or benzyl. Ammonium compounds in a suitable case optionally derived from organic acids, inorganic acids or their salts. More preferably the organic acid is selected from the group consisting of alkanovykh acids containing from 1 to 12 carbon atoms, preferably from 1 to 6 carbon atoms, more preferably 2 carbon atoms, dibasic carboxylic acids containing from 1 to 12 carbon atoms, preferably from 1 to 6 carbon atoms. These alcamovia and dibasic carboxylic acids optionally substituted by one or more CNS groups containing less than 5 carbon atoms, hydroxyl groups and lagrappe, hydrogen fluoride, hydrogen chloride, bromide water is kind, phosphoric acid, phosphorous acid, nitric acid, nitrous acid, karnavati acid and perchloric acid. In a particularly preferred variant of the invention ammonium compounds derived from formic acid, acetic acid, succinic acid, glutaric acid, phthalic acid, nitric acid or hydrogen chloride. Most preferably the compound of ammonia is ammonium acetate or ammonium chloride. In the case of ammonium chloride can be obtained catalysts for Fischer-Tropsch having essentially the same operating characteristics as the catalyst based on titanium dioxide, obtained in accordance with the chloride method.

In the present method, the concentration of ammonium compounds in a suitable case is in the range from 0.01 to 5.0 M, preferably from 0.1 to 2 M. in Addition, the molar ratio of ammonium compounds and titanium dioxide is in the range from 0.01 to 1, preferably equal to approximately 0.5.

After the above processing, rinsing the washed product in a suitable case from aqueous solution produce. It is done using methods well known in the literature. You can use the plate filters, centrifugal filters, filter presses, vacuum filters, and the like. Part of the liquid can be removed after gravitational usaidinitiated titanium followed by additional processing. You can use continuous methods, and periodic methods. After filtration of titanium dioxide, optionally dried and optionally calcined. Alternatively, the filter cake is optionally washed using water, in particular at a temperature in the range from 30 to 70°that as a result leads to additional improvement of the selectivity in the reaction of synthesis of hydrocarbons using the Fischer-Tropsch process. Preferably the number ranging from 5 to 100 l of water/kg of titanium dioxide. Drying in a suitable case performed using commercially available equipment, a well-known specialist in the relevant field, at temperatures in the range from 30 to 250°C. the Calcination is carried out in standard equipment, a well-known specialist in the relevant field. The final temperature at most equal to 1000°C, preferably is in the range from 400 to 700°C. Appropriate annealing times are in the range of from 0.1 to 3 hours, in particular equal to about 0.5 hours.

In yet another variant of realization of titanium dioxide after removal of the leaching solution suspended with a predetermined amount of water, followed by thermal drying or spray drying and optional calcination. Thermal and Raspletin the Yu drying carried out using standard equipment well-known specialist in the relevant field. Drying in a suitable case is carried out at temperatures at the inlet in the range from 1000 to 350, preferably from 850 to 400°C. a Suitable pressure is in the range from 0.5 to 0.01 bar. The annealing also carried out in standard equipment, a well-known specialist in the relevant field. The final temperature at most equal to 1500°C, preferably is in the range from 400 to 700°C. Appropriate annealing times are in the range of from 0.1 to 3 hours.

Processing lavage of the present invention when carrying out it for titanium dioxide, intended for use as carriers of catalysts, particularly useful when it is carrying out to improve the selectivity, activity and/or stability of catalysts containing at least one metal or one metal connection when selecting a metal from groups Ib, IIb, IIIb, IVb, VIb, VIIb and VIII of the periodic table of elements, more preferably from groups IVb, VIb and VIII, in particular of titanium, chromium, iron, cobalt, Nickel, zirconium, ruthenium, rhodium, palladium rhenium and platinum, in particular iron and/or cobalt. This occurs in particular when the washing is carried out at a pH equal to 7 or more, in particular in the range from 8 to 11, more preferably RA is NR 9. the pH can be increased by adding hydroxy-compounds of the above-mentioned ammonium compounds. In particular, you can use the hydroxides alkyl-, dialkyl - or trialkylamine, with alkyl groups, in particular, are ethyl or methyl. The most preferred compound is ammonium hydroxide. You can also use and hydroxides of alkali metals (NaOH or KOH), particularly if washing will be followed by a rinsing with water. However, in some cases, trace amounts of alkali metals can cause negative consequences.

The specific surface area of titanium dioxide after washing and optional calcination in an appropriate case, is in the range from 20 to 250 m2/g, preferably from 30 to 80 m2/, Appropriate temperature control of the drying and/or calcination may allow to obtain the desired specific surface area. In this respect, it is observed that higher temperature calcination or longer annealing times result in obtaining a smaller specific surface area.

Subjected to washing and drying titanium dioxide, optionally after calcination, can be very suitable for use in obtaining katal is congestion, in particular, catalysts suitable for obtaining hydrocarbons from synthesis gas, in the reaction, which is known in the literature under the name of the reaction of the Fischer-Tropsch process.

The catalysts intended for use in this way often contain as catalytically active component, a metal of group VIII of the periodic table of elements. In particular catalytically active metals include ruthenium, iron, cobalt and Nickel. Cobalt is the preferred catalytically active metal. The preferred hydrocarbon feedstock to produce synthesis gas is natural gas and/or associated gas. Because the data types of the raw material after partial oxidation and/or steam reforming the result is usually enable you to obtain a synthesis gas with a ratio of N2/, Is approximately equal to 2, a very good catalyst for Fischer-Tropsch will be cobalt, because the custom value for this type of catalysts is also approximately equal to 2.

The catalytically active metal is preferably applied to a porous carrier, in particular titanium dioxide, obtained in accordance with the method of the present invention.

The amount of catalytically active metal on the carrier is preferably in the range from 3 to 300 M.Ch. on 100 machine hours of material media, more pre is respectfully from 10 to 80 machine hours, in particular from 15 to 60 m.ch..

If desired, the catalyst may also contain one or more metals or metal oxides as promoters. Suitable promoters on the basis of metal oxides can be selected from groups IIA, IIIB, IVB, VB and VIB of the periodic table of the elements or of actinoids and lanthanoids. In particular, very well suitable promoters include oxides of magnesium, calcium, strontium, barium, scandium, yttrium, lanthanum, cerium, titanium, zirconium, hafnium, thorium, uranium, vanadium, chromium and manganese. Particularly preferred promoters on the basis of oxides of metals for the catalyst used to obtain waxes intended for use in the present invention are the oxides of manganese and zirconium. Suitable promoters based metals can be selected from groups VIIB or VIII of the periodic table. Particularly suitable are rhenium and noble metals from group VIII, in particular the preferred platinum and palladium. The amount of promoter present in the catalyst, in a suitable case is in the range from 0.01 to 100 machine hours, preferably from 0.1 to 40, more preferably from 1 to 20 M.Ch. on 100 machine hours media. The most preferred promoters are selected from vanadium, manganese, rhenium, zirconium, and platinum.

The catalytically active metal and the promoter, if such is the th feature, can be applied to the material carrier using any suitable processing, such as impregnation, kneading and extrusion. After application of the metal and, if appropriate promoter on material media media caused these components are usually subjected to calcination. The effect of treatment with annealing is to remove the water of crystallization, decomposition of volatile products of decomposition and transformation of organic and inorganic compounds to their respective oxides. After calcination of the resulting catalyst can be activated as a result of introduction of the catalyst into contact with hydrogen or a hydrogen-containing gas, usually at temperatures in the range from approximately 200 to 350°C. Other methods of obtaining catalysts of the Fischer-Tropsch include mixing/kneading, often followed by extrusion, drying/calcination and activation or mixing/kneading with the subsequent receipt of a suspension, spray drying and calcination.

Method of catalytic conversion can be implemented in normal conditions of synthesis of the known state of the art. Catalytic conversion can usually be done at a temperature in the range from 150 to 300°C, preferably from 180 to 260°C. Normal values of total pressure on the I way catalytic conversion are in the range from 1 to 200 bar absolute pressure, more preferably from 10 to 70 bar absolute pressure. In a method of catalytic conversion gain in particular more than 75 wt.% C5+-, preferably more than 85 wt.% With5+-hydrocarbons. Depending on the catalyst and conditions of conversion of the number of heavy paraffin (C20+) can reach up to 60 wt.%, sometimes up to 70 wt.%, and sometimes even up to 85 wt.%. Is preferred when using a cobalt catalyst, use a low ratio of N2/WITH (especially 1.7 or even below) and use low temperature (190-230°). In order to avoid any coke formation is preferred to use a ratio of N2/WITH at least 0.3. Particularly preferably carrying out the reaction of the Fischer-Tropsch under such conditions, when SF is the alpha value obtained for products containing at least 20 carbon atoms, at least equal 0,925, preferably at least equal 0,935, more preferably at least equal 0,945, even more preferably at least equal 0,955. Is preferred when the flow of hydrocarbons using the Fischer-Tropsch contains at least 35 wt.% With30+, preferably 40 wt.%, more preferably 50 wt.%.

Preferably using a catalyst Fischer-Tropsch process, which ensures that significant amounts of PA is atinav, more preferably essentially unbranched paraffins. Catalyst, the most suitable for this purpose is a cobalt containing catalyst Fischer-Tropsch process. Such catalysts are described in the literature, see, for example, AU 698392 and WO 99/34917.

The way the Fischer-Tropsch process may be suspended by way of the Fischer-Tropsch or Fischer-Tropsch fixed bed catalyst, in particular with a fixed catalyst bed in novotrubnom the reactor, preferably by way of a three-phase fluidized bed.

The invention is additionally illustrated by the following further examples, which, however, must in no way be used to limit the scope of the invention.

Example 1

Commercially available titanium dioxide was washed for 1 hour at 90°using a solution of ammonium acetate in water with a concentration of 1 M. the Mass ratio of the aqueous solution/titanium dioxide 4. After extraction, drying at 120°and annealing at 600°conducted by measuring the amount of sulfur. The same method was repeated several times using several treatments by washing. The results are summarized in table 1.

td align="center"> 0,240
Sulfur content (wt.%)
Not probivaucheisa titanium dioxide:
1 processing lavage0,040
2 processing lavage0,040
3 processing lavage0,030
10 treatments lavage0,030

In three comparative experiments, in which titanium dioxide was washed using water, sulfuric acid and chloride-hydrogen acid, was observed only minimal reduction of the sulphur content.

Example 2

Experiment 1 was repeated at a temperature of 120°in the autoclave. The results are summarized in table 2.

Sulfur content (wt.%)
Not probivaucheisa titanium dioxide:0,240
1 processing lavage0,035
2 processing lavage0,030

Example 3

Experiment 1 was repeated using a commercially available titanium dioxide from another manufacturer. The results are summarized in table 3.

Sulfur content (wt.%)
Not probivaucheisa titanium dioxide:0,750
3 processing lavageto 0.060

Example 4

Experiment 1 repeat what or using commercially available titanium dioxide from another manufacturer. The results are summarized in table 4.

Sulfur content (wt.%)
Not probivaucheisa titanium dioxide:0,160
3 processing lavage0,050

Example 5

Not probivaucheisa material described in example 1, the material, washed three times in accordance with the description of example 1, and the material washed three times with the use of ammonium chloride in the same manner as described in example 1 was subjected to a process such quantities of cobalt oxide promoted with manganese. After activation with hydrogen in the synthesis of hydrocarbons by the Fischer-Tropsch got the following results:

Temperature, °Output in grams per hour per 1 cubic centimeter of volume of catalystThe selectivity for C5+The selectivity for C1
Not probivaucheisa material219224327
Washing (3 times, acetate NH4)223156886
Washing (3 times, chloride NH4)20979 847
Washing (l times, NH4Cl, pH 9)222157876

The above results indicate that the activity (proxied by the yield in grams per hour per 1 cubic centimeter of volume of the catalyst) and selectivity (selectivity for C5+and methane yield) significantly increased in the treatment lavage.

1. The method of purification of calcined titanium dioxide from sulfur, in particular sulfates in the treatment of titanium dioxide using an aqueous solution containing one or more compounds of ammonia, at elevated temperatures, separation of titanium dioxide from aqueous solution and drying the titanium dioxide.

2. The method according to claim 1, in which titanium dioxide is obtained using the sulfate method.

3. The method according to claim 1, in which the elevated temperature is a temperature in the range from 40 to 150°C, preferably from 60 to 110°S, more preferably from 80 to 95°C.

4. The method according to claims 1 to 3, in which stage of processing is carried out in the course of from 0.01 to 12 h, preferably from 0.1 to 3 hours, more preferably from 0.4 to 1.5 hours

5. The method according to claims 1 to 3, in which ammonium compounds derived from compounds of trialkylamine, compounds selected from the group consisting of dialkylamino is, connection alkylamine or compounds unsubstituted ammonium, preferably, compounds unsubstituted ammonium.

6. The method according to claims 1 to 3, in which ammonium compounds optionally derived from an organic acid or inorganic acid, and, preferably, the organic acid is selected from the group consisting of alkanovykh acids containing from 1 to 12 carbon atoms, preferably from 1 to 6 carbon atoms, more preferably 2 carbon atoms, dibasic carboxylic acids containing from 1 to 12 carbon atoms, preferably from 1 to 6 carbon atoms, these alcamovia and dibasic carboxylic acids optionally substituted by one or more CNS groups containing less than 5 carbon atoms, hydroxyl groups and lagrappe, or hydrogen fluoride, hydrogen chloride, hydrogen bromide, phosphoric acid, phosphorous acid, nitric acid, nitrous acid, karnavati acid and perchloric acid, more preferably, a combination of ammonia is ammonium acetate or ammonium chloride.

7. The method according to claims 1 to 3, in which the concentration of ammonium compounds in a suitable case is in the range from 0.01 to 5.0 M, preferably, from 0.1 to 2 M, and the molar ratio of ammonium compounds and titanium dioxide is in the range from 0.01 to 1, preferably equal is approximately 0.5.

8. The catalyst or the raw material for the catalyst containing the medium for titanium dioxide obtained by the method according to claims 1-7.

9. A method of producing hydrocarbons, which impose synthesis gas under conversion into contact with a suitable catalyst containing as a carrier of titanium dioxide obtained by the method according to claims 1-7.



 

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Reactor // 2275332

FIELD: nonferrous metallurgy; fluoride methods of titanium raw reprocessing.

SUBSTANCE: the invention is pertaining to the field of nonferrous metallurgy, in particular, to the fluoride method of titanium raw reprocessing, for example, reprocessing of the ilmenite concentrates at production of titanium dioxide. The reactor contains: the housing including a shell, the ends of which are overlapped by the butt walls; the tool of stirring of the reactionary components supplied with the drive of rotation arranged outside the cavity of the reactor; the charging and discharging units. The heat-feeding unit is arranged outside the concavity of the reactor. The surface of the cavity of the reactor housing is made out of magnesium or silicon oxide or magnesium. The components of the reactor housing are connected hermetically. The charging unit and the discharging unit are made with a capability of sealing. The invention improves reliability and operability of the reactor in conditions of usage of the highly aggressive fluoride-containing materials.

EFFECT: the invention ensures improved reliability and operability of the reactor in conditions of usage of the highly aggressive fluoride-containing materials.

4 cl, 3 dwg

Reactor // 2263073

FIELD: fluoride methods of processing of titanium-containing raw materials.

SUBSTANCE: the invention is pertaining to the fluoride methods of processing of titanium-containing raw materials, for example, ilmenite concentrates at production of titanium dioxide. The reactor contains a body including a tubular wall with a bottom and a cover. The driving shaft with stirrers is located in a cavity of the reactor. The heat-supply unit is placed outside the cavity of the reactor. The reactor has a loading unit and an unloading unit. The surface of the cavity of the body of the reactor is made out of magnesium; the surfaces of the details located in the cavity of the reactor is made out of a material resistant to action of solutions of fluoride-containing reactants. Components of the body are connected hermetically and the loading unit and unloading unit are made with a capability to be sealed. The cover of the reactor is supplied with a gas outlet line branch pipe supplied with the shutoff valves. In the bottom of the reactor there is an unloading gate. The invention allows to improve reliability and serviceability of the reactor in operations with usage of a highly aggressive reactant, excludes losses of quality of the final product.

EFFECT: the invention ensures improved reliability and serviceability of the reactor in operations with usage of a highly aggressive reactant, excludes losses of quality of the final product.

3 cl, 1 dwg

Reactor // 2263072

FIELD: fluoride methods of processing of titanium-containing raw materials.

SUBSTANCE: the invention is pertaining to the fluoride methods of processing of titanium-containing raw materials, for example, ilmenite concentrates at production of titanium dioxide. The reactor contains a body including a tubular wall with a bottom and a cover. The driving shaft with stirrers is located in a cavity of the reactor. The heat-supply unit is placed outside the cavity of the reactor. The reactor has a loading unit and an unloading unit. The surface of the cavity of the body of the reactor is made out of magnesium; the surfaces of the details located in the cavity of the reactor is made out of a material resistant to action of solutions of fluoride-containing reactants. Components of the body are connected hermetically and the loading unit and unloading unit are made with a capability to be sealed. The cover of the reactor is supplied with a gas outlet line branch pipe connected to a unit of utilization of the gaseous products of the reaction. In the bottom of the reactor there is an unloading gate. The invention allows to improve reliability and serviceability of the reactor in operations with usage of a highly aggressive reactant, excludes losses of quality of the final product.

EFFECT: the invention ensures improved reliability and serviceability of the reactor in operations with usage of a highly aggressive reactant, excludes losses of quality of the final product.

3 ck, 1 dwg

FIELD: fluoride methods of processing of titanium-containing raw materials.

SUBSTANCE: the invention is pertaining to the equipment for materials processing and the fluoride methods of processing of titanium-containing raw materials, for example, ilmenite concentrates. The installation for processing of materials contains a reactor made in the form of a cylindrical body, a means of stirring of reactive components, a heating unit located outside a cavity of the reactor, a loading and an unloading units. At that the means of stirring of the reactive components is made in the form of the rotary drive of the body of the reactor. The installation is supplied with an additional reactor made in the form of a cylindrical body, supplied with a rotary drive, a loading unit and an unloading unit and a heating unit. The internal surface of the main reactor is made out magnesium, and such a surface of the additional reactor - out of silicon oxide. The unloading unit of the main reactor is hermetically coupled with the loading unit of the additional reactor. Both reactors are supplied with the gas outlet line branch pipes and the steam conduits for the superheated steam feeding in. The invention improves reliability and service capability of the installation in operations with usage of a highly aggressive fluoride-containing materials, ensures the high efficiency of the process and allows to reach the purity of titanium dioxide up to 100 %.

EFFECT: the invention ensures improved reliability and service capability of the installation in operations with usage of a highly aggressive fluoride-containing materials, the high efficiency of the process and a possibility to reach the purity of titanium dioxide up to 100 %.

3 cl, 1 dwg

FIELD: equipment and methods of fluorine processing of titanium-containing raw materials.

SUBSTANCE: the invention is pertaining to the field of equipment and methods of fluorine processing of titanium-containing raw materials, for example, ilmenite concentrates at production of titanium dioxide. The reactor installation contains the reactor coupled with the sources of reactants, which through a discharge assembly is connected with apparatuses of the subsequent processing of the reaction products. At that as the sources of the reactants they use a hopper - for a solid titanium-containing material, for example, ilmenite, and the source of ammonium fluoride. The discharge assembly contains a filtrate outlet, a slurry outlet and a gas outlet. At that the gas outlet of the reactor is fused to an ammonia feeder, the reactor filtrate outlet is fused to the first screen, a filtrate outlet of which is coupled to the second screen, the filtrate outlet of which is coupled to the cavity of a hydrolysis reactor, the outlet of which is in turn coupled to the third screen, the slurry outlet of which is coupled to the dryer-dispenser, the slurry outlet of which is coupled to the charging assembly of the reactor of pyrohydrolysis, the outlet of which is coupled to a container for storage of a satin white. At that the gas outlets of the second screen, the dryer-dispenser, the third screen and the reactor of pyrohydrolysis are coupled to the source of ammonium fluoride. Besides the ammonia feeder is coupled to the second screen and to the cavity of the reactor of hydrolysis. At that the source of ammonium fluoride is additionally coupled to the cavity of the reactor of hydrolysis. Besides the slurry outlets of the reactor and the first screen are coupled to the container for storage of the slurry. At that the cavity of the reactor of pyrohydrolysis is coupled to the source of steam through the steam conduits. The invention allows to improve reliability and serviceability of the installation at usage of the highly-corrosive fluorine-containing materials during processing of titanium-containing raw material with production of white pigment, to ensure the high completeness of utilization of the raw materials, the high yield and whiteness of the product, and to simplify of the process of production.

EFFECT: the invention ensures improved reliability and serviceability of the installation at highly-corrosive fluorine-containing materials use in titanium-containing raw material processing, production of white pigment, high yield and whiteness of the product, simplified process.

5 cl, 4 dwg

FIELD: equipment and methods of fluorine processing of titanium-containing raw materials.

SUBSTANCE: the invention is pertaining to the field of equipment and methods of fluorine processing of titanium-containing raw materials, for example, fluorine processing of ilmenite concentrates, at titanium dioxide production. The reactor installation contains the reactor coupled with the sources of reactants, which through a discharge assembly is connected with apparatuses of the subsequent processing of the reaction products. At that the reactor, devices and components of the installation are made out of a material resistant to action of the contacting with them corrosive materials.

At that as sources of the reactants use a hopper - for a solid titanium-containing material, for example, ilmenite, and a source of ammonium fluoride. The discharge assembly contains a filtrate outlet, a slurry outlet and a gas outlet. At that the gas outlet of the reactor is fused to an ammonia feeder, the reactor filtrate outlet is fused to the first screen, a filtrate outlet of which is coupled to the second screen, the filtrate outlet of which is coupled to the cavity of a hydrolysis reactor, the outlet of which is in turn coupled to the third screen, the outlet of which is coupled to the first dryer-dispenser, the slurry outlet of which is coupled to a charging assembly of the first reactor of the pyrohydrolysis, the outlet of which is coupled to a container for storage of a satin white. At that the gas outlets of the second screen, the first dryer-dispenser, the third screen and the first reactor of pyrohydrolysis are coupled to the source of ammonium fluoride. Besides the ammonia feeder is additionally coupled to the second screen and to the cavity of the reactor of hydrolysis. At that the source of ammonium fluoride is additionally coupled to the cavity of the reactor of hydrolysis. Besides the slurry outlets of the reactor and the first screen are coupled to the second dryer-dispenser, the slurry outlet of which is coupled to the cavity of the second reactor of pyrohydrolysis, outlet of which is coupled to a container for storage of a red pigment. At that the gas outlets of the second dryer-dispenser and the second reactor of pyrohydrolysis are coupled to the source of the ammonium fluoride. In addition the cavities of the first and the second reactors of pyrohydrolysis are coupled to the source of steam through the steam conduits. The invention ensures improved reliability and the state of serviceability of the installation in conditions of usage of the highly-corrosive fluorine-containing materials during processing of titanium-containing raw material and high yield of white and red pigments, high completeness of utilization of the raw materials, high yield and whiteness of the product, and also simplification of the process.

EFFECT: the invention ensures simplified process, improved installation reliability and serviceability, raw materials utilization completeness, high yield of white and red pigments, high product whiteness.

5 cl, 4 dwg

FIELD: inorganic chemistry, chemical technology.

SUBSTANCE: invention relates to technology for preparing titanium dioxide. Method for preparing titanium dioxide involves electrochemical oxidation of metallic titanium in sodium hydroxide alkaline solution with the concentration 45-46.5 wt.-% at density of alternating sinusoidal current of industrial frequency 1.5-2.0 A/cm2 and temperature 70-90°C and thermal treatment at 110-900°C. Invention provides enhancing quality of product due to diminishing particle sizes and elevating specific surface square.

EFFECT: improved method for preparing.

1 tbl, 8 ex

The invention relates to a device for carrying out the reaction in a tubular reactor of one or more gaseous reactants with high flow rates

The invention relates to the extraction of titanium from leucoxene concentrate, obtained during the concentration of oil-bearing silicon-titanium ores

FIELD: catalyst carriers.

SUBSTANCE: invention relates to structure and composition of carrier based on grid-structured tissue of glass, silica, or another interaction fiber treated with formulations imparting rigidity to grids and preventing deformation-caused destruction of fibers, which carrier is used mainly to retain photocatalytically active material on its surface, but also suitable to retain catalysts exhibiting activity in the absence of light. Provided is catalyst carrier constituted by one or several arranged in parallel layers of corrugated grid made from inorganic woven fibers and impregnated with binding material or constituted by one or several arranged in parallel layers of non-corrugated grid also made from inorganic woven fibers and impregnated with binding material.

EFFECT: increased catalyst retention ability and increased area of illuminated photocatalyst surface.

3 cl, 3 dwg, 8 ex

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