The method of producing titanium dioxide

 

(57) Abstract:

The invention relates to methods for producing titanium dioxide. When a vapor-phase oxidation of titanium tetrachloride oxygen-containing gas in the presence of chlorides of aluminum and silicon with subsequent microasperities received product in a steam jet mill in the presence of 20-30% water solution of ammonia in titanium dioxide before microasperities enter tetraethoxysilane, or tetrabutoxide titanium or polyaluminosilicate or their mixture in an amount of 0.3 to 6.0% by weight of pigment, when the mass ratio of ammonia of 1: (0.01 to 1,6), in terms of 100% substance, and an aqueous solution of ammonia is used in a quantity of 0.3-2.0% by weight of pigment. 1 C.p. f-crystals, 1 table.

The invention relates to a process for the production of titanium dioxide pigment used in paint, paper and other industries.

Known methods for producing pigmentary titanium dioxide by vapor-phase oxidation of titanium tetrachloride oxygen-containing gas in the presence of additives of inorganic compounds (with or without supplements) with subsequent microasperities in a steam jet mill in the presence of an aqueous solution of ammonia (A. C. 604863, Ál. C 09 C 1/Anta. Closest to the claimed is a method for pigmentary titanium dioxide by vapor-phase oxidation of titanium tetrachloride oxygen-containing gas in the presence of chlorides of aluminum and silicon with subsequent microasperities product in a steam jet mill in the presence of 20-30%, aqueous solution of ammonia with the introduction in the process of micromilieu of polyethylsiloxane in the amount of 0.3-0.6 wt.% to the pigment mass in the mass ratio polyethylsiloxane: ammonia= 1:(0.3 to 0.4) per 100% green matter (A. C. 1700027, Ál. C 09 C 1/36, 1991).

The disadvantage of this method is low bleaching ability, the weather resistance of pigment and a high residue on sieve 0045.

The objective of the invention is to improve bleaching ability, reduced residue on the sieve and improving the weather resistance of pigment titanium dioxide.

The problem is solved by the method of obtaining of titanium dioxide pigment, comprising vapor-phase oxidation of titanium tetrachloride oxygen-containing gas in the presence of chlorides of aluminum and silicon with subsequent microasperities pigment in a steam jet mill in the presence of 20-30% aqueous ammonia solution, and when the mass ratio of the ORGANOMETALLIC compound:ammonia=1:(from 0.01 to 1.6) in terms of 100% substance, a water solution of ammonia is used in the amount of 0.3 to 2.0 by weight of pigment. As the ORGANOMETALLIC compound used tetraethoxysilane, or tetrabutoxide titanium or polyaluminosilicate or their mixture.

The difference of the proposed method is the introduction of tetraethoxysilane, or tetrabutoxide titanium or polyaluminosilicate or mixtures thereof in the amount of 0.3 to 6.0 wt.% when the ratio of ORGANOMETALLIC compound:ammonia= 1:(from 0.01 to 1.6) in terms of 100% substance.

Thus, the invention conforms to the criterion "novelty". Comparison of the proposed method with the prototype and other well-known technical solutions in this field of technology is not allowed to reveal the features distinguishing the claimed invention from the prototype, which allows to conclude that the criterion of "inventive step".

Examples of the method.

Example 1. Vaporous titanium tetrachloride oxidize oxygen-containing gas at 1150oC in the presence of 2.0 wt.% aluminium chloride and 0.3 wt.% chloride of silicon. The obtained titanium dioxide is applied by spraying liquid tetraethoxysilane (TES) in the amount of 0.3% by weight of pigment. Then just before microsmall ammonia in amount of 0.2% by weight of pigment and produce micromelia under the following steam parameters: pressure of 12 ATM. (1.2 MPa) and a temperature of 340oC.

Example 2. The method is carried out according to example 1,except that titanium dioxide is applied TPP in the amount of 6.0 wt.%, and aqueous ammonia serves in the amount of 2.0 wt.%.

Example 3. The method is carried out according to example 1, except that the obtained titanium dioxide is applied liquid tetrabutoxide titanium (TBT) in the amount of 0.3% by weight of pigment and 25% aqueous ammonia solution serves in the amount of 1.2% by weight of pigment.

Example 4. The method is carried out according to example 1, except that the obtained titanium dioxide is applied TBT in the amount of 6.0% by weight of pigment and 25% aqueous ammonia solution serves in the amount of 2.0 wt.%.

Example 5. The method is carried out according to example 1, except that the obtained titanium dioxide is applied liquid polyaluminosilicate (ALOX) in the amount of 0.3% by weight of pigment, 25% aqueous ammonia solution in the amount of 2.0% by weight of pigment.

Example 6. The method is carried out according to example 5, only ALOX add in the amount of 6.0% by weight of a pigment, a solution of ammonia in amount of 0.2 wt.%.

Example 7. The method is carried out according to example 1, except that the obtained titanium dioxide is applied pre-cooked mixture ALEX, TPS and SPS in the amount of 6.0% (2.0% cadetblue in example 7, only the mixture in the amount of 0.3% (0.1% of each component) to the pigment mass and aqueous ammonia in the amount of 1.2% by weight of pigment.

Example 9. The method is carried out according to example 7, the mixture is applied in the amount of 3.0% (1.0% in each component), and ammonia solution in the amount of 1.0% by weight of pigment.

Example 10. The method is carried out according to example 1, except that the obtained titanium dioxide put the mixture ALEX and TBT in the amount of 0.3%, (0.1 and 0.2%) and ammonia solution in the amount of 0.3% by weight of pigment.

Example 11. The method is carried out according to example 10, only titanium dioxide is applied mixture consisting of 4,0% ALEX% and 2.0%, TBT, and aqueous ammonia in an amount of 0.4% by weight of pigment.

Example 12. The method is carried out according to example 1, except that titanium dioxide is applied a mixture of TPP and ALEX in the amount of 6.0% (3.0% for each), and ammonia serves in the amount of 0.2% by weight of pigment.

Example 13. The method is carried out according to example 12, only a mixture of TPP and ALEX put in the amount of 0.3% (0.1 and 0.2%).

Example 14. The method is carried out according to example 1, except that the obtained titanium dioxide is applied a mixture of 0.1% TBT and 0.2% TPP, and aqueous ammonia in the amount of 2.0% by weight of p% (3.0% respectively), a solution of ammonia serves in the amount of 0.3% by weight of pigment.

The properties of the pigments obtained in examples 1-15, and prototype. C. N 1700027 presented in the table. The resulting products have a bleaching ability 1850-1900 srvc.ed., the residue on the sieve 0,045 - 0,002-0,001% or absence and the number of cycles VIAM before melenija 8-9. Bleaching ability and the residue on the sieve 0,045 of titanium dioxide pigment was determined according to GOST 9608-84 with ISM. N 2 "titanium Dioxide pigment, and resistance to cycles VIAM on RTM - 35-6-1 "Coating of paint. The main methods of accelerated environmental tests". The publishing house of standards, M, 1 - 966.

From the data the table shows that in comparison with the known, the proposed method of producing pigmentary titanium dioxide provides improved bleaching ability 100-150 srvc.ed., the reduction of the residue on sieve 0045 on 0,003-0,005% and improving the weather resistance of the coating 2-5 cycle VIAM. The effectiveness of the proposed method of producing pigmentary titanium dioxide was confirmed in the experimental shop of the Chelyabinsk branch of JSC APF "Pigment".

1. The method of obtaining of titanium dioxide pigment, comprising vapor-phase oxidation of tetrachlorid received product in a steam jet mill in the presence of 20-30% aqueous ammonia solution, characterized in that the titanium dioxide before microasperities enter ORGANOMETALLIC compound and/or tetracyclin in the amount of 0.3 to 6.0% by weight of pigment in a mass ratio of the ORGANOMETALLIC compound and/or tetracyclin : ammonia = 1 : (from 0.01 to 1.6) in terms of 100% substance, and an aqueous solution of ammonia is used in a quantity of 0.3 - 2.0% by weight of pigment.

2. The method according to p. 1, characterized in that as the ORGANOMETALLIC compound used tetrabutoxide titanium or polyaluminosilicate or their mixture.

 

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FIELD: production and cooling of titanium dioxide.

SUBSTANCE: gaseous titanium tetrachloride and oxygen are brought into react at high temperature. Titanium dioxide and gaseous reaction products are cooled by passing through tube-type heat exchanger together with cleaning agent to remove depositions from inner walls. Inner walls of heat exchanger contain spiral blades arranged over at least part of heat exchange surface.

EFFECT: deposition removing with, as well as titanium dioxide and gaseous product cooling with increased effectiveness.

13 cl, 2 dwg

FIELD: industrial inorganic synthesis.

SUBSTANCE: invention is directed to production of dispersed titanium dioxide via vapor-phase hydrolysis of titanium tetrachloride. Process comprises combusting natural gas in air atmosphere, supplying titanium tetrachloride and water to reaction zone, performing thermal hydrolysis operation, separating titanium dioxide from gaseous products, and subsequent treatment of gaseous reaction products in several steps. Gaseous products are first treated with calcium chloride solution to produce titanium dioxide slurry, which is then filtered. Resulting precipitate is rinsed, dried, and ground to form commercial titanium dioxide. Gaseous products are further treated with calcium hydroxide suspension to form commercial calcium chloride.

EFFECT: reduced loss of titanium dioxide with gaseous products and additionally enabled production of calcium chloride so that environmental pollution is also reduced.

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FIELD: chemical industry; methods and installations for the synthesis of the titanium dioxide.

SUBSTANCE: the invention may be used for production of the powdery titanium dioxide using the chloride process engineering. The installations for the synthesis of the titanium dioxide contains: the plasmatron (1), to which the source (2) of oxygen or the oxygen-containing gas is connected; the plasma-chemical reactor (3) connected to the consumption tank (4); the device (5) used for feeding of the titanium tetrachloride; the hardening chamber (6); the single-pipe heat exchanger (8) of the "the pipe inside the pipe" type; the synthesis products separation block (10). The synthesis products separations block consists of the cyclone (11) and the screen (13). The hardening chamber has the cylindrical body, the cone bottom of which is connected to the hopper (21) with the coarse fractions of titanium dioxide and to the radially arranged outlet fitting pipe (9). The hardening chamber is additionally supplied with the pneumoimpulsive generator (7). The trunk (14) of the pneumoimpulsive generator is mounted in the lower part of the cylindrical body coaxially and diametrically opposite to the radial outlet fitting pipe (9). The cyclone of the synthesis products separation block, which inlet is connected to the heat exchanger (8,) is made with the axially symmetric leveling chamber (15), which is coaxially arranged between the body and the discharge pipe (17) at the following ratio of the geometrical parameters: d/D = (0.l÷0.7), where "d" is the maximum diameter of the leveling chamber; "D" is the diameter of the cylindrical body. The method of the synthesis of the titanium dioxide provides that refrigerating of the reaction products after the hardening chamber is exercised at the flow of the dust-gas stream in the single-pipe heat exchanger of the " a pipe inside the pipe" type with the mass speed - the mass stream density from 5 up to 80 kg/ms. The invention allows to boost efficiency and reliability of the installation operation for the synthesis of the titanium dioxide.

EFFECT: the invention allows to increase efficiency and reliability of the installation operation for the synthesis of the titanium dioxide.

3 cl, 1 dwg, 2 tbl

FIELD: varnish-and-paint industry.

SUBSTANCE: process of producing titanium dioxide pigment according to chloride technology comprises oxidation of titanium tetrachloride with oxygen or oxygen-containing gas in plasmachemical reactor followed by cooling of reaction products in tempering chamber and subsequent multistep fine grinding of intermediate product, titanium dioxide, by way of affection with supersonic gas flow at 100-500°C and ratio of gas mass intake to titanium dioxide mass intake = 0.2. In the first step of titanium dioxide fine grinding, treatment of titanium dioxide is performed with a dry gas supplemented by vapor of organic or organosilicon modifier having in its molecule at least one of the following functional groups: -OH, -NH2, NH, SH at mass intake of modifier representing 0.1-2.0% of the mass intake of titanium dioxide.

EFFECT: improved quality of titanium dioxide pigment and simplified process of production thereof.

1 dwg, 1 tbl

FIELD: industrial inorganic synthesis.

SUBSTANCE: method of preparing high-quality titanium nanoxide with particle size 10 to 100 nm comprises generation of gas plasma, introducing gas plasma flow, oxygen, and titanium tetrachloride vapors, oxidation of titanium tetrachloride with oxygen in synthesis zone to form titanium dioxide and chlorine, and quenching synthesis products in supersonic nozzle by way of transforming subsonic synthesis products flow escaping synthesis zone into supersonic flow, which is then expanded and cold quenching gas is injected thereto. Prior to enter synthesis zone, titanium tetrachloride is mixed with oxygen at molar ratio between 0.05 and 0.25, respectively. Cold quenching gas is injected when supersonic flow is expanded inside expanding portion of supersonic nozzle having opening angle 10-15°.

EFFECT: improved quality of titanium nanoxide.

1 dwg, 2 tbl

FIELD: industrial inorganic synthesis.

SUBSTANCE: invention is meant to be used in varnish-and-paint industry, in production of catalysts, dielectrics, and other industries. Titanium dioxide production process is based on conversion of titanium tetrachloride in oxygen plasma into disperse titanium dioxide and chlorine gas. Oxygen plasma stream is generated by several electroarc plasmatrons uniformly distributed across horizontal cross-section of reactor and disposed below feed and rutilization additive entry zone. Feed and rutilization additive (aluminum chloride) are added to plasma stream from above in the form of disintegrated solution of aluminum chloride in titanium tetrachloride. A disintegration additive, namely silicon tetrachloride. is simultaneously added together with oxygen. Feed and indicated additives are stirred with oxygen plasma. Two-phase conversion product stream at the mixing zone outlet is squeezed with tangential stream of return chlorine gas, rutile titanium dioxide and chlorine gas are separated consecutively in cyclone, on metallized cloth and metal-ceramic filters, pigmented disperse titanium dioxide is continuously withdrawn from apparatus and chlorine gas is continuously purified from residual disperse phase and then recycled.

EFFECT: increased yield of rutile modification of titanium dioxide and reactor operation efficiency, reduced titanium dioxide loss and power consumption.

9 cl, 2 dwg, 1 tbl

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