Method of processing kyanite concentrate. RU patent 2489503.

IPC classes for russian patent Method of processing kyanite concentrate. RU patent 2489503. (RU 2489503):

C22B5/10 - by solid carbonaceous reducing agents

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Method involves mixing a concentrate, a carbonaceous reducing agent and a pore-forming additive in form of ammonium sulphate, pelletising the obtained mixture, firing and holding at maximum temperature with reduction of silicon dioxide to a gaseous monoxide, crushing the obtained sinter, treatment thereof with ammonium bifluoride and calcining the reaction mass to obtain an aluminium-containing product, wherein ammonium sulphate is taken in an amount of 10-20% of the mass of the concentrate; before pelletising, the mixture is milled to obtain particles with size of 50-75 mcm in amount of at least 80%; the mixture is fired at temperature of 1690-1750°C; ammonium bifluoride is taken in amount of 0.4-14% of the mass of the sinter; and the reaction mass is calcined at 700-900°C. Before treatment with ammonium bifluoride, the sinter can be treated with 10-20% hydrochloric acid. The degree of extraction of aluminium oxide from the concentrate is increased by 1.3-9.9%. Content of aluminium oxide in the end product reaches 97.7% with content of silicon oxide impurities of 0.13-1.0%.

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FIELD: chemistry.

SUBSTANCE: method involves mixing a concentrate, a carbonaceous reducing agent and a pore-forming additive in form of ammonium sulphate, pelletising the obtained mixture, firing and holding at maximum temperature with reduction of silicon dioxide to a gaseous monoxide, crushing the obtained sinter, treatment thereof with ammonium bifluoride and calcining the reaction mass to obtain an aluminium-containing product, wherein ammonium sulphate is taken in an amount of 10-20% of the mass of the concentrate; before pelletising, the mixture is milled to obtain particles with size of 50-75 mcm in amount of at least 80%; the mixture is fired at temperature of 1690-1750°C; ammonium bifluoride is taken in amount of 0.4-14% of the mass of the sinter; and the reaction mass is calcined at 700-900°C. Before treatment with ammonium bifluoride, the sinter can be treated with 10-20% hydrochloric acid. The degree of extraction of aluminium oxide from the concentrate is increased by 1.3-9.9%. Content of aluminium oxide in the end product reaches 97.7% with content of silicon oxide impurities of 0.13-1.0%.

EFFECT: high content of aluminium oxide in the end product while reducing content of silicon oxide impurities.

3 cl, 6 ex

The invention relates to the field of processing of aluminium raw material, in particular , and can be used in the production of alumina, corundum refractories, ceramics, silumin and aluminium.

There is a method of processing of aluminium raw material, mainly bauxite (see Pat. 2136378 of the Russian Federation, the IPC 6 03 1/02, 03 1/02, 1999), which includes grinding preliminary calcined at a temperature of about 800 degrees bauxite with the content, wt.%: Al 2 O 3 - 69, SiO 2 - 9, Fe 2 O 3 - 2, blending it with carbonaceous reducing agent, taken in the quantity necessary for the restoration of silicon dioxide SiO2 to silicon monoxide SiO and recovery of iron oxide Fe 2 O 3 to education iron carbide Fe 3 C, briquetting weight by pressing, firing briquettes in a vacuum at 1200-1300 OC for 1 hour with the removal of the SiO and magnetic separation for removal of iron carbide. The share of aluminium oxide compounds in the final product increases in the range of concentrations of carbon 1-5 wt.%. As a result of firing at a 1200C With the content of silicon dioxide is reduced approximately twice, and at 1300 OC is the complete removal. The total content of iron compounds decreased to 0.5 wt.%.

The disadvantage of this method is the inability to use it for processing of aluminum silicates with a high content of silicon dioxide: kyanite, andalusite, sillimanite, as at 665 C and higher education begins good connection mullite that blocks the process. In addition, the firing of briquettes in a vacuum complicates the process, and briquetting prevent a more complete removal of the produced silicon monoxide.

Known also adopted as a prototype method for processing concentrate (see Grishin N.N., Belogurova, O.A. Ivanova, A.G. Enrichment of kyanite by carbothermic reduction // New refractories. 2010. №6. P.11-20), comprising a mixture of concentrate that contains, mass%: Al 2 O 3 - 63,17, SiO 2 - 31,85, TiO 2 - 1,1, Fe 2 O 3 - 2,0, with carbonaceous reducing agent, taken in the amount of 4 to 15 wt.% and additive in the form of ammonium sulphate in the amount of 21.5 wt.%. The resulting mixture okomkovyvayut and subjected regenerative burning with exposure at a temperature of 1700-1800 OC for 2-4 hours with the restoration of silicon dioxide to the gaseous monoxide and deleting it. The resulting spectra are crushed, process ammonium and calcined reaction mass with 1200-1250 degree C for a complete removal of volatile compounds. product obtained after the recovery firing at a temperature of 1800 degrees With delayed for 4 hours and processing ammonium, contains, mass%: Al 2 O 3 - 93,49, SiO 2 - 1.05, The TiO 2 - 2,2, Fe 2 O 3 - 1,78.

The main disadvantage of this method is that when annealing temperature up to 1700°together with gaseous silicon formed and removes gaseous compounds of aluminium, which reduces extraction of aluminium oxide in product and fails to achieve the required contents of Al 2 O 3 . In addition, the content of impurity dioxide silicon is significant, and the energy intensity of the method is relatively high.

The present invention is directed to achievement of the technical result, which consists in enhancing the degree of extraction of aluminium oxide, ensuring its high content in product and reduction of impurity silicon oxide. In addition, the technical result consists in reducing the energy intensity of the way.

The technical result is achieved by the method of processing concentrate, which includes a mixture of concentrate, carbonaceous reducing agents or supplements in the form of ammonium sulfate, pelletizing received the charge, firing with exposure at the maximum temperature with the restoration of silicon dioxide to the gaseous monoxide, grinding received SPECA, processing ammonium and calcination reaction mass with obtaining of aluminum-containing product, according to the invention ammonium sulfate take in the amount of 10-20% in relation to mass concentrate, before blend palletizing charge by grinding to a particle size of 50 to 75 microns not less than 80%of firing the charge carried out at a temperature 1690-1750°, ammonium take in the amount of 0.4 to 14% in relation to mass SPECA and calcination reaction mass is conducted at 700-900°N

The achievement of a technical result contributes to the fact that exposure lead the charge for 4-6 hours.

The achievement of a technical result also contributes to the fact that prior to treatment ammonium spec process 10-20% hydrochloric acid.

The essential features of the claimed invention to determine the scope of legal protection and sufficient for obtaining a technical result of the above, perform the functions and correlate with the results as follows.

The use of ammonium sulfate in the amount of 10-20% in relation to mass concentrate contributes to the increase in porosity of granules and increasing the reaction surface concentrate, that intensifies the removal of gaseous silicon monoxide and lead to fuller restoration of silicon dioxide. Introduction of ammonium sulfate in the quantity is less than 10% will reduce the porosity of the granules and the reaction surface concentrate, and the introduction of more than 20% causes a decrease in durability of granules, they are destroyed, filling the pore space and limiting removal of gaseous silicon monoxide.

Grinding of the charge before it blend palletizing to a particle size of 50 to 75 microns not less than 80% contributes to a more equal distribution of components in the amount of the charge and provides firm contact particles that creates the best conditions for response components with the formation of gaseous products. Grinding charge to a particle size of less than 50 microns dramatically increases grinding process does not lead to a substantial improvement in the diffusion of reducing agent in grain kyanite and backward diffusion of gaseous SiO. Grinding charge to a particle size of more than 75 microns is undesirable due to deterioration of diffusion beans kyanite.

The choice of the firing temperature of the mixture in the interval 1690-1750°With due to the fact that at this temperature, already there is a redistribution of Al 2 O 3 and SiO 2 separate phases with the removal of silicon oxide. The aluminum oxide in a given interval of temperatures remains in Speke, promotes increase of degree of extraction of aluminium oxide and its higher contents in the output product. Furthermore, the reduced energy intensity of the way. The firing of charge at a temperature below 1690°not provides full recovery of silicon dioxide contained in concentrate, as a significant number of silicon dioxide (up to 50%) remains in thermally stable 3Al 2 O 3 2SiO 2 . The firing of charge at temperatures above 1750°leads to partial education and gaseous compounds of aluminium and reduce extraction Al 2 O 3 in the target product.

Introduction ammonium in the amount of 0.4 to 14% of the weight of the SPECA allows you to delete silicon dioxide (1-3%), which reduces its content in the product. Adding ammonium an amount of less than 0,4% is insufficient, and more than 14% of the excess in terms of the ratio of residual silicon dioxide and ammonium for the most complete translation of silicon dioxide in flying form (NH 4 ) 2 SiF 6 .

Calcination reaction mixture at 700-900°provides additional cleaning of the derived product of silicon dioxide. At temperatures below 700oC no complete purification from volatile compounds of silicon, and hardening at temperature above 900ºc leads to unreasonable increase of energy intensity of ways.

The totality of the above features is necessary and sufficient to obtain a technical result of the invention, consisting in the increase of degree of extraction of aluminium oxide, ensuring its high content in product and reduction of impurity silicon oxide, as well as in reducing the energy intensity of the way.

In particular cases, the implementation of an invention is preferable following specific operations and operational parameters.

Excerpt charge for 4-6 hours at a maximum temperature of roasting provides preemptive destruction of silicon in the form of his monoxide compared with the compounds of aluminium, when maintaining high extraction of aluminium oxide leads to the increase of its relative content in the resulting product. Excerpt charge less than 4 hours is insufficient for complete decomposition of thermally sustainable mullite, due to that there is incomplete removal of silicon and increase of its content in the final product. For shutter speeds longer than 6 hours together with silicon formed and removes gaseous compounds of aluminium, which leads to the decrease of its extraction in the product and to the unjustified increase in the energy intensity of the way.

Sintering 10-20% hydrochloric acid before it can be processed ammonium provides a more complete treatment of residual impurity silicon and titanium and iron. Sintering of hydrochloric acid with a concentration of less than 10% is not sufficient to dissolve and remove impurities from SPECA. When the concentration of hydrochloric acid over 20% together with impurities are removed and aluminum compounds, which reduces its extraction in the target product.

The above private features of the invention shall allow a method in optimal mode.

The essence of the method and the results being achieved more clearly can be illustrated by the following examples.

Example 2. Take 100 g of concentrate composition in Example 1 and mixed with 8 g of carbonaceous reducing agent (7.5%) and 12 g supplements in the form of ammonium sulfate (10%). The resulting mix of grind before the content of particles with krupnostju 50-75 microns 84% and okomkovyvayut. Then firing exercise received pellets in carbon filling at a temperature of 1700°With delayed 4 hours before the formation of gaseous silicon monoxide, which removed the hood as education. The resulting spectra are crushed and treated 6 g ammonium (13% by weight of SPECA). Reaction mass is calcined at 700oC obtaining aluminum-containing product that contains, mass%: Al 2 O 3 - 94,31, SiO 2 - 0,85. The degree of extraction of Al 2 O 3 in product is 87,8%.

Example 3. Take 100 g of concentrate composition in Example 1 and mixed with 8 g of carbonaceous reducing agent (7.5%) and 26 g supplements in the form of ammonium sulfate (20%). The resulting mix of grind before the content of particles with krupnostju 50-75 microns 84 wt.% and okomkovyvayut. Then firing exercise received pellets in carbon filling at a temperature of 1700°With delayed 6 hours prior to the formation of gaseous silicon monoxide, which removed the hood as education. The resulting spectra are crushed and treated 4.8 g ammonium (11% of the mass of the SPECA). Reaction mass is calcined at 900ºc obtaining aluminum-containing product that contains, mass%: Al 2 O 3 - 96,5, SiO 2 - 0,36. The degree of extraction of Al 2 O 3 in product is 95,7%.

Example 4. Take 100 g of concentrate composition in Example 1 and mixed with 8 g of carbonaceous reducing agent (7.5%) and 26 g supplements in the form of ammonium sulfate (20%). The resulting mix of grind before the content of particles with krupnostju 50-75 microns 84% and okomkovyvayut. Then firing exercise received pellets in carbon filling at a temperature of 1750°With delayed 6 hours prior to the formation of gaseous silicon monoxide, which removed the hood as education. The resulting spectra are crushed, treated with 10% hydrochloric acid with s:l=1:10, and then treated 4.9 g ammonium (11.7% of the mass of the SPECA). Reaction mass is calcined at 800 degrees C to produce aluminium-containing product that contains, mass%: Al 2 O 3 - 96,3, SiO 2 - 0,35. The degree of extraction of Al 2 O 3 in product is 96%.

Example 5. Take 100 g of concentrate composition in Example 1 and mixed with 8 g of carbonaceous reducing agent (7.5%) and 26 g supplements in the form of ammonium sulfate (20%). The resulting mix of grind before the content of particles with krupnostju 50-75 microns 84% and okomkovyvayut. Then firing exercise received pellets in carbon filling at a temperature of 1750°With delayed 6 hours prior to the formation of gaseous silicon monoxide, which removed the hood as education. The resulting spectra are crushed, treated with 20% hydrochloric acid with s:l=1:10, and then treated 0.17 g ammonium (0.4% by weight of the SPECA). Reaction mass is calcined at 800 degrees C to produce aluminium-containing product that contains, mass%: Al 2 O 3 - 97,7, SiO 2 - 0,13. The degree of extraction of Al 2 O 3 in product is 92%.

Example 6 (the prototype). Take 100 g of concentrate that contains, mass%: Al 2 O 3 - 63,17, SiO 2 - 31,85, Fe 2 O 3 - 2,0, TiO 2 - 1,12, and mixed with 8 g of carbonaceous reducing agent (7.5%) and 29 g supplements in the form of ammonium sulfate (21,5%). The resulting mixture okomkovyvayut and firing exercise received pellets in carbon filling at a temperature of 1800 degrees With delayed 4 hours before the formation of gaseous silicon monoxide, which removed the hood as education. The resulting spectra are crushed and treated with 9 g ammonium (21.4% of the mass of the SPECA). Reaction mass is calcined at 1250°obtaining aluminum-containing product that contains, mass%: Al 2 O 3 - 92,52, SiO 2 - 1,15. The degree of extraction of Al 2 O 3 in product is 86,1%.

The given Examples show that the proposed method of processing concentrate allows compared with the prototype increase of 1.3-9,9% degree of extraction of aluminium oxide concentrate. The content of aluminium oxide in the product reaches 97,7% with the admixture of silicon oxide 0,13-1,0%. Option is less energy-consuming and can be implemented with the involvement of the standard process equipment.

1. Method for processing concentrate, including mixing concentrate, carbonaceous reducing agents or supplements in the form of ammonium sulfate, pelletizing resulting charge, firing with exposure at the maximum temperature with the restoration of silicon dioxide to the gaseous monoxide, grinding received SPECA, processing ammonium and calcination reaction mass with obtaining of aluminum-containing product, wherein ammonium sulfate is taken in the amount of 10-20% by weight of concentrate, before blend palletizing charge by grinding to a particle size of 50 to 75 microns not less than 80%, the firing of charge carried out at a temperature 1690-1750°, ammonium take in the amount of 0.4 to 14% by weight of SPECA and calcination reaction mass is conducted at 700-900°N

2. The method according to claim 1, characterized in that the exposure of the charge are for 4-6 hours