RU2794482C1 - Reactor for processing titanium-containing raw materials - Google Patents

Abstract

FIELD: reactor for processing of titanium-containing raw materials.

SUBSTANCE: invention can be used to obtain fine powders of titanium dioxide from titanium-containing raw materials (ilmenite or rutile concentrate) using the hydrofluoride method. Reactor contains a cylindrical body, the upper end of which is connected by means of a pipeline to a container for storing solid raw material, and the lower end is connected to the inlet pipeline of the heating unit. In the upper part of the cylindrical reactor body there is the first branch pipe for connection by means of a pipeline to the scrubber unit, containing a scrubber with a cooling system and the second branch pipe for connection by means of a pipeline to a container for storing liquid raw material. Under the specified branch pipes there is the third branch pipe for connection with the outlet pipeline of the heating unit. The heating unit contains a coil connected to the inlet and outlet pipelines, and an ultrasonic resonator is installed in the inlet pipeline.

EFFECT: increase in reliability and operability of the reactor under the conditions of using a highly aggressive reagent/group of reagents while eliminating the loss of quality of the resulting product.

5 cl, 2 dwg

Description

FIELD OF TECHNOLOGY

The invention relates to a reactor for the processing of titanium-containing raw materials and can be used to obtain fine powders of titanium dioxide by the hydrofluoride method from titanium-containing raw materials (ilmenite or rutile concentrate).

BACKGROUND OF THE INVENTION

The prior art reactor disclosed in RU 2263072 C1, publ. 10/27/2005, prototype. The reactor contains a body including a tubular wall with a bottom and a lid. The drive shaft with agitators is located in the reactor cavity. The heat supply unit is outside the reactor cavity. The reactor has loading and unloading nodes. The surface of the cavity of the reactor vessel is made of magnesium; the surface of the parts placed in the cavity of the reactor is made of a material resistant to the effects of solutions of fluoride-containing reagents. Housing elements are hermetically connected, loading and unloading units are sealed. The reactor lid is equipped with a gas outlet connected to the unit for utilization of the gaseous reaction products. An unloading hatch is located at the bottom of the reactor.

The disadvantage of the reactor disclosed above is:

1. The presence of an unloading hatch, which prevents the reaction from being continuous or partially continuous.

2. The presence of magnesium as the material of the reactor cavity wall, which contaminates the reaction products due to metal losses in the region of the boiling boundary.

3. The presence of a mechanical stirrer, which creates at least one additional node, suggesting the loss of ammonia.

DISCLOSURE OF THE INVENTION

The objective of the claimed invention is the development of a reactor for producing fine powders of titanium dioxide by the hydrofluoride method.

The technical result of the invention is to increase the reliability and operability of the reactor under the conditions of using a highly aggressive reagent/group of reagents while eliminating the loss of quality of the resulting product.

The specified technical result is achieved due to the fact that the reactor for processing titanium-containing raw materials contains a cylindrical body, the upper end of which is connected by means of a pipeline to a container for storing solid raw material, and the lower end is connected to the inlet pipeline of the heating unit. At the same time, in the upper part of the cylindrical reactor vessel, the first branch pipe is located for connection using a pipeline with a scrubber unit, containing a scrubber with a cooling system and a second branch pipe for connection using a pipeline with a storage tank for liquid raw material, and under these pipes there is a third branch pipe for connecting with the outlet pipeline of the heating unit. Moreover, the heating unit contains a coil connected to the inlet and outlet pipelines, and an ultrasonic resonator is installed in the inlet pipeline.

At the lower end of the reactor vessel there is a slurry outlet.

Ammonia water outlet fitting is installed at the lower end of the housing.

In the upper lateral part of the scrubber body, a fitting for removing residual gases with a filter is installed.

The cooling system is a closed circuit with a convection cooler filled with water.

BRIEF DESCRIPTION OF THE DRAWINGS

The invention will be better understood from the description, which is not restrictive and given with reference to the accompanying drawings, which show:

Fig. 1 - Scheme of the claimed reactor.

Fig. 2 - Scheme of hydrofluoride technology.

1 - heating block; 1.1 - coil; 1.2 - pump; 1.3 - pump motor; 2 - dispenser of liquid raw material; 3 - dispenser of solid raw material; 4 - reaction zone; 4.1 - reactor vessel; 4.2 - fitting for supplying liquid raw material; 4.3 - pulp outlet; 5 - scrubber block; 5.1 - ammonia water outlet; 5.2 - gas supply fitting; 5.3 - scrubber; 5.4 - fitting for the removal of residual gases; 5.5 - filter; 6 - container for storing solid raw material; 7 - container for storing liquid raw material; 8 - ultrasonic resonator; 9 - pressure control valve; 10 - convection refrigerator.

IMPLEMENTATION OF THE INVENTION

The reactor for processing titanium-containing raw materials contains a cylindrical body 4.1, the upper end of which is connected by means of a pipeline to a container 6 for storing solid raw material, and the lower end is connected to the inlet pipeline of the heating unit (1). At the same time, in the upper part of the cylindrical body 4.1 of the reactor, there is a first branch pipe for connection via a pipeline with a scrubber unit 5, containing a scrubber 5.3 with a cooling system and a second branch pipe for connection via a pipeline with a container 7 for storing liquid raw material, and under these pipes there is the third branch pipe for connection with the outlet pipeline of the heating unit 1. In the pipeline connecting the body 4.1 with the tank 6, a dispenser 3 of solid raw material (ilmenite or rutile concentrate) in the form of a powder with a particle size of 0.05-0.5 mm is installed, and in the pipeline connecting the body 4.1 with the tank 7, a liquid material dispenser is installed (saturated solution of ammonium fluoride or bifluoride).

The heating block (1) contains a heated coil connected to the inlet and outlet pipelines, and an ultrasonic resonator (8) is installed in the inlet pipeline.

At the lower end of the body 4.1 of the reactor, a fitting 4.3 is installed to remove the pulp.

In the pipeline for connecting the reactor 4.1 with the scrubber 5.3, a pressure control valve 9 is installed through the gas supply fitting 5.2. At the lower end of the scrubber body 5.3, an ammonia water outlet is installed.

In the upper side part of the scrubber body, a fitting 5.4 for removing residual gases with a filter 5.5 is installed.

The cooling system is a closed circuit of pipelines with a convection cooler 10 filled with water. The closed loop is connected to the inlet (lower) and outlet (upper) side fittings of the scrubber 5.3.

The claimed reactor for processing titanium-containing raw materials works as follows.

From the container 7 for storing liquid raw material through the dispenser 2 liquid raw material into the reaction zone 4 located inside the vessel 4.1 of the reactor is supplied with a saturated solution of ammonium fluoride.

From the solid raw material storage tank 6, ilmenite powder is supplied through the solid raw material dispenser 3 .

In the reaction zone (4) of the reactor, a slurry is formed with a temperature of 109°C. The reactor is a container resistant to temperatures up to 120°C, to ammonium fluoride, steam-gas mixture - steam-ammonia and to transient processes at the boiling point (polycarbonate, polypropylene, epoxy-cellulose composite).

Heating and mixing (bubbling) of the pulp is carried out due to a closed heating circuit filled with a coolant consisting of a heating element in the form of a coil 1.1 made of a material resistant to a hot mixture of steam-ammonia and a "pump" 1.2 made of a material resistant to a hot mixture of steam-ammonia (aluminum, monel alloy, reinforced silicones, etc.).

As a heat carrier, a mixture is used - steam-ammonia, which is the product of the reaction of ammonium fluoride with ilmenite concentrate. The coolant with the help of a pump 1.2, powered by the engine, enters the reactor from below, passes through it and thereby heating and mixing the pulp, the cooled coolant enters the coil 1.1 heated by known methods, for example, by heating a nichrome coil. After the coil 1.1 hot coolant enters the reactor. With the help of an ultrasonic resonator 8, the reaction of titanium dioxide formation is accelerated due to the fact that a standing ultrasonic wave is created in the coolant (pressure drops at the reactor inlet are excluded), transmitting vibrations to the liquid raw material inside the reactor vessel.

Excess ammonia in the form of a water-ammonia gas-vapor mixture formed in the reactor vessel 4.1 is fed into the scrubber 5.3 through the gas supply fitting 5.2 through a pipeline containing a pressure control valve (9) that regulates the pressure in the reactor. When the specified vapor-gas mixture interacts with the cooling water, which enters the scrubber 5.3 through the inlet lower side fitting, as a result, ammonia, passing through the water, dissolves in it with the formation of ammonium hydroxide (ammonia water), and the condensed water vapor increases the volume of water. The heated water from the scrubber 5.3 through the upper outlet side fitting through the pipeline enters the convection cooler 10, where it is cooled and again enters the scrubber 5.3. Ammonia water is discharged through the 5.1 ammonia water outlet 5.1.

The remains of undissolved gases are discharged into the atmosphere through the outlet 5.4 of the residual gases with a filter 5.5.

The reaction products (a fine suspension of insoluble ammonium fluoroferrates in a solution of ammonium fluorotitanates) are discharged for subsequent use through the pulp outlet 4.3.

The claimed technical result is achieved by excluding moving elements from the reactor operation scheme by mixing and heating the pulp by bubbling the coolant, which is used as the reaction products of solid and liquid raw materials, as well as the use of materials in the structural elements of the reactor that can withstand aggressive environments.

The invention has been described above with reference to a specific embodiment. For specialists, other embodiments of the invention may be obvious, without changing its essence, as it is disclosed in the present description. Accordingly, the invention is to be considered limited in scope by the following claims only.

Claims (5)

1. A reactor for the processing of titanium-containing raw materials, containing a cylindrical body, the upper end of which is connected by means of a pipeline to a storage tank for solid raw material, and the lower end is connected to the inlet pipeline of the heating unit, while in the upper part of the cylindrical reactor body there is a first branch pipe for connecting by means of a pipeline with a scrubber block containing a scrubber with a cooling system, and a second branch pipe for connection by means of a pipeline with a container for storing liquid raw material, and under these pipes there is a third branch pipe for connection with the outlet pipeline of the heating block, and the heating block contains a coil, connected to the input and output pipelines, and an ultrasonic resonator is installed in the input pipeline. 2. The reactor according to claim. 1, characterized in that at the lower end of the reactor vessel there is a fitting for removing the pulp. 3. The reactor according to claim. 1, characterized in that at the lower end of the scrubber body there is a fitting for removing ammonia water. 4. The reactor according to claim. 1, characterized in that in the upper side part of the scrubber body there is a fitting for removing residual gases with a filter. 5. Reactor according to claim 1, characterized in that the cooling system is a closed circuit with a convection cooler filled with water.

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