A method of processing sphene

 

(57) Abstract:

The invention is intended for the chemical industry and can be used to obtain pigments for paper, plastics, paints and varnishes. In the solution of H2SO4with a concentration of 350-550 g/l add sphene. After 5-10 h, heated to boiling, the suspension is injected phosphate solution with a content of 25-50% P2O5. The amount of phosphate solution enables linking 20-35% of Tio2in sphene. As phosphate solution, you can use the filtrate after sulfuric opening of Apatite. With stirring, add the germs of Tio2and a solution of Ti2ABOUT3. Stand when heated for 10 h, diluted with hot water. The precipitate was separated, washed with water T:W=1:(5-6), calcined at 650-750C. Extraction of Tio2~95%. The filtration rate of the suspension 500-600 l/m2including the oil absorption of the pigment from 25.8 27.4 g/100 g, opacity 49,7 of 51.0 g/m2the content of water-soluble salts of 0.55-0,98%. 1 C.p. f-crystals, 2 tab.

The present invention relates to chemical technology of inorganic materials, in particular of such pigment compositions used in the manufacture of paper, plastic, and lacquer is Klimova, K. Sphene and chemical processing of titanium pigments. - L.: Nauka, 1983. - 88 C. ) to obtain the titanium containing pigment composition (titanium-calcium composition. At the specified method stanovy concentrate reveal sulfuric acid in two stages: the first is 70%, t - 170oC; the second is 55%, t - 130oC. the Reaction mass is then cooled and separating the precipitate. Last subjected to leaching in three stages. Combine the resulting titanium containing solution, and after addition the mixture of lime milk suspension is subjected to thermohydraulic. Resulting precipitate is washed, treated with modifiers and calcined at 850-870oC. Removing TiO2from sphene is 75%. Duration of 45 hours of Pigment composition CaSO4+ TiO2contains soluble salts (HRV) - 6.5-7.0%, white is 95-96 srvc. unit , the oil absorption - 25-28 g/100 g, opacity - 55-70 g/m2.

The main disadvantage of this method is its multi-stage (total duration - 45 hours) that defines a significant loss to the main component is titanium dioxide (through the extraction of TiO2from the source of the concentrate is not more than 75%). In addition, the pigment indices pasiune surfaces only indoors.

Also known is a method of processing sphene (see ed. St. USSR N 42232, C 09 C 1/36, 1935) by processing sphene when heated to 50% sulfuric acid with an allocation of 50% of TiO2of sphene in the liquid phase or salt, followed by diluting the suspension with water and hydrolysis of titanium (IV) in certain circumstances with the formation of titanium hydroxide. At the end of the process, the formed precipitate was separated from the liquid phase, the filtration rate is 100 l/m2hour, washed it with water otmuchivaniem unopened mineral, and then calcined at 800-850oC. the Obtained pigment composition contains 20% of TiO2has a noticeable yellow tint, its oil absorption equals 35-45 g/100 g, the spreading rate is 100-120 g/m2the content of HRV 8-10%. Removing TiO2- 50%.

The disadvantages of the described method include low degree of extraction of TiO2of sphene in the final product, poor filterability of the suspension in the separation of the precipitate from the liquid phase, and the low quality of the final product.

The present invention aims at improving the extraction of TiO2of sphene and improving the quality of such pigment compositions while increasing the speed of the precipitate from the liquid phase is otcu his solution of sulfuric acid when heated with translation of titanium in the liquid phase and the subsequent allocation of him in the sediment, the sludge separation, washing and calcination to obtain such pigment compositions according to the invention the processing of sphene are the sulfuric acid solution with a concentration of 350-550 g/l, and after 5-10 hours from the start of heating of the injected phosphate solution containing 25-50% P2O5in an amount to provide binding 20-35% of TiO2located in sphene.

The problem is solved and the fact that as phosphate solution using the filtrate after sulfuric opening of Apatite.

The method is as follows. In the sulfuric acid solution with a concentration of H2SO4- 350-550 g/l enter sphene before reaching T:W=1:3-4 and the suspension is heated to boiling. After 5-10 hours from the start of heating it is injected phosphate solution with a concentration of 25-50% P2O5based binding 20-35% of TiO2located in sphene. The suspension is maintained at the heat for another 10-15 hours in the presence of germs titanium and solution of trivalent titanium, consumption, which equals respectively 0.5% TiO2and 0.2% of Ti2O3in relation to the TiO2in sphene. The mixture is then cooled and separated the sediment (filtration rate of 500-600 l/m2the e TiO2from sphene - 95%. The obtained titanium containing pigment composition consisting of anhydrite (CaSO4), silica gel, calcium phosphate and titanium dioxide is white 96.3-97.1 the river. units, the content of DIF - 0.55 - 0.98%, oil absorption - 25.8-27.4 g/100 g, opacity - 49.7-51.0 g/m2.

The process under these conditions ensures obtaining fine sediment shell structure. Particles represent inert core consisting of CaSO4and SiO2on the surface of which is formed pigment coating of phosphate and hydroxide of titanium. During annealing, this shell is attached to the core, reducing the solubility of calcium sulfate and compensating activity of silica gel, thereby increasing filtration rate and quality of the final pigment product.

The treatment of sphene sulfuric acid with a concentration of less than 350 g/l H2SO4reduce the rate of filtration and the degree of extraction of him TiO2and when the concentration of H2SO4more than 550 g/l is low, the extraction of titanium (IV) from the liquid phase in the form of a hydroxide of titanium.

Introduction phosphate solution into the heated suspension in less than 5 hours leads to a decrease in the Aqua phosphate solution more than 10 hours leads to an increase in the content of the pigment HRV and thus to reduce its quality.

The consumption of phosphate solution in an amount to provide linking more than 35% of TiO2located in sphene, as well as reducing its concentration in the phosphate solution is less than 25% P2O5leads to dilution of the sulfuric acid to the suspension and thus to reduce the extraction of TiO2from sphene, as well as lower quality of the pigment product. At the rate of phosphate solution in an amount to provide binding of less than 20% of TiO2, and the concentration of more than 50% of the P2O5increases the viscosity of the suspension decreases the speed of filtration, which leads to a decrease in the whiteness index.

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

Example 1. Take 3.5 l of sulfuric acid solution with a concentration of 350 g/l H2SO4add 1 kg of sphene and the suspension is heated to boiling. After 5 h in the heated suspension is injected phosphate solution with a concentration of 50% P2O5in an amount to provide a binding 20% TiO2located in sphene, stirred for 0.5 h and add the germs titanium 0.5% TiO2and the solution of trivalent titanium 0.2% of Ti2O3in relation to the TiO2in sphene. The suspension is allowed to stand for 1 is laidout 40-50oC and filtered (filtration rate 500 l/m2hours, the precipitate is washed with water at T:W=1:5 and calcined at 650oC. the Obtained pigment product (1.32 kg) contains DIF - 0.55%, white - 96.3 srvc. units, opacity - 50 g/m2the oil absorption - 27.4 g/100 g Extract TiO2- 95%.

Example 2. Take 3.5 l of sulfuric acid solution (450 g/l H2SO4), add 1 kg of sphene and the suspension is heated to boiling. After 7.5 h in the heated suspension is injected phosphate solution with a concentration of 35% P2O5in an amount to provide a binding 30% TiO2located in sphene, stirred for 0.5 h, type embryos titanium 0.5% TiO2and the solution of trivalent titanium 0.2% of Ti2O3in relation to the TiO2in sphene. The suspension is incubated 12.5 hours under heating, and then dilute it with hot water (350 ml) and after 4 hours off the heating, the suspension is cooled to 40-50oC and filtered (filtration rate 500 l/m2hours, the precipitate is washed with water at T:W=1:6 and calcined at 700oC. the Obtained pigment product (1.35 kg) contains DIF - 0.61%, white - 97 srvc. units, opacity - 49,7 g/m2the oil absorption - 25.8 g/100 g Extract TiO2- 95%.

Example 3. Take 3.5 l of a solution to sernauto suspension is injected phosphate solution with a concentration of 25% P2O5in an amount to provide a binding 35% TiO2located in sphene, stirred for 0.5 h, type embryos titanium 0.5% TiO2and the solution of trivalent titanium 0.2% of Ti2O3in relation to the TiO2in sphene. The suspension is incubated for 10 hours under heating, and then dilute it with hot water (350 ml) and after 4 hours off the heating, the suspension is cooled to 40-50oC and filtered (filtration rate 600 l/m2hour). The precipitate is washed with water at T:W=1:6 and calcined at 750oC. the Obtained pigment product (1.30 kg) contains DIF - 0.98%, white - 97.1 the river. units, opacity - 51 g/m2the oil absorption of 26.0 g/100 g Extract TiO2- 95%.

Example 4. Take 3.5 l of sulfuric acid solution with a concentration of 450 g/l H2SO4, add 1 kg of sphene and the suspension is heated to boiling. After 7.5 h in the heated suspension is injected phosphate solution (filtrate after sulfuric opening Apatite) with a concentration of 35% P2O5in an amount to provide a binding 30% TiO2located in sphene, stirred for 0.5 h, type embryos titanium 0.5% TiO2and the solution of trivalent titanium 0.2% of Ti2O3in relation to the TiO2in sphene. The suspension is incubated 12T up to 40-50oC and filtered (filtration rate of 500 g/m2hours, the precipitate is washed with water at T:W=1:6 and calcined at 700oC. the Obtained pigment product (1.35 kg) contains DIF - 0.61%, white - 97.0 srvc. units, opacity - 49.7 g/m2the oil absorption - 25.8 g/100 g Extract TiO2- 95%.

Phosphate solution obtained by opening 60 g of Apatite sulfuric acid with a concentration of 350 g/l H2SO4at a temperature of 95-100oC and stirring for 4-5 hours. The consumption of sulfuric acid is 105% of the stoichiometric (calculated for CaO, located in Apatite). The reaction mass is then cooled and filtered liquid phase, which is a phosphate solution containing 35% P2O5.

In table. 1 Examples 1-4 with the declared parameters of the process, Examples 5-12 with transcendent values, and Example 13 of the prototype.

In table. 2 shows the indices of the known and proposed methods.

Thus, from these Examples it follows that the proposed method compared with the prototype to increase the extraction of TiO2from sphene 45%, 5-6 times increases the rate of filtration of the suspension and improve the quality of the pigment composition is for use in various coatings, including weather-resistant paint due to a significant reduction in HRV. Use as a phosphate solution of the filtrate from the opening of the Apatite reduces the cost of the finished product by reducing the cost of materials used for the implementation of the proposed method.

1. A method of processing sphene, including the processing solution of sulfuric acid when heated with translation of titanium in the liquid phase and the subsequent allocation of it in the precipitate, separating the precipitate, washing and calcination to obtain such pigment compositions, characterized in that the processing of sphene are the sulfuric acid solution with a concentration of 350 - 550 g/l, and after 5 to 10 hours from the start of heating of the injected phosphate solution containing 25 - 50% R2ABOUT5in an amount to provide a binding 20 - 35% of TiO2located in sphene.

2. The method according to p. 1, characterized in that as phosphate solution using the filtrate after sulfuric opening of Apatite.

 

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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

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