Method of treatment of fluocarbon raw

FIELD: methods of treatment of fluocarbon raw.

SUBSTANCE: the invention is pertaining to the methods of treatment of fluocarbon raw. The method of treatment of fluocarbon raw provides for heating by means of high frequency induction of a heating zone of a reaction chamber up to the temperature of no more than 950°C, heating in the heating zone of fluocarbon raw, which contains at least one fluocarbon compound, so, that the fluocarbon compound dissociates with production of at least one predecessor of fluocarbon or its reactive kinds; and refrigerating of the predecessor of fluocarbon or its reactive kinds, in the result of which from the predecessor of fluocarbon or its reactive kinds forms at least one more desirable fluocarbon compound. The technical result is conversion of the fluocarbon raw into the useful products by the low-cost reliable non-polluting environment universal and easily controlled method.

EFFECT: the invention ensures conversion of the fluocarbon raw into the useful products by the low-cost reliable non-polluting environment universal and easily controlled method.

12 cl, 10 dwg, 3 tbl, 2 ex

 

The present invention relates to the processing of fluorocarbon materials, in particular to a method of processing fluorocarbon materials.

In accordance with this invention proposes a method of processing fluorocarbon feedstock, which provides:

heating using a high frequency induction heating zone to a high temperature;

providing opportunities for fluorocarbon feedstock which contains at least one fluorocarbon compound, such heating in the heating zone that fluorocarbon compound decomposes to receive at least one fluorocarbon precursor or reactive species; and

cooling of the fluorocarbon precursor or reactive species to education at the expense of that of the fluorocarbon precursor or reactive species at least one more desirable fluorocarbon compounds.

This heating zone may be provided in the reactor. The reactor may have an elongated cylindrical shell, which has a reaction chamber, which, in turn, has a heating zone and a container (holder) for raw material in the heating zone of the reaction chamber. The shell of the reactor is typically made of quartz, and its ends can be sealed for cooling water.

Vysokoye the hydrated induction heating can be performed using a high frequency induction furnace, having the induction coil inside which a localized heating zone of the reactor. In other words, the induction heating coil covers that part of the shell of the reactor, which contains the heating zone.

In accordance with one embodiments of the present invention, the shell of the reactor can be vertical and stationary. We can assume that this configuration is particularly well suited for processing raw materials in the form of no filler, not directly used material that will be described later.

However, in accordance with another variant of the present invention, the shell of the reactor can be set at an angle to the vertical, for example, at an angle from approximately 5° to 60° to the vertical, and can rotate or oscillate (vibrate). In this case, the reactor may be equipped with a graphite crucible having a transverse partition for regulating the retention time of the feedstock in the reactor. We can assume that this configuration is particularly well suited for processing raw materials in the form of a material with a filler, which is not used directly, which will be described later, when the material with the filler passes in a downward direction in the lower part of the reactor, it depolymerizes and evaporates, thus obtained products are up and out of the reactor, while the remainder of the material on which alnilam comes from below through the base of the reactor. Instead, the vertical reactor can be used for processing material with a filler; however, such a reactor should be equipped at its lower end a detachable bottom for drainage filling material.

Raw materials, at least in principle, can be gaseous, liquid, or can be in the form of a solid powder or a mixture of two or more of these types.

When raw material is liquid, it may be more or less pure raw materials, which contains a single fluorocarbon compound, such as C6F14; however, it is not excluded the case when the raw material normally is not used directly fluorocarbon product that contains two or more of such fluorocarbon compounds as C5F12C6F14C7F16C8F18C4F8O, C8F16O, (C3F7)3N, C6F13H6F12H2etc. Normally one component is present in this product as the dominant component, i.e. forms a large part of such product. Raw materials in such case may be served in the reactor from the bottom.

When the raw material has the form of a solid powder is a solid powder form), it can be a material with a filler or material without filler, which may not be used in isulan directly such as polytetrafluoroethylene (PTFE), a tetrafluoroethylene HEXAFLUOROPROPYLENE vinylidenefluoride (THV), fluorinated copolymer of ethylene and propylene (FEP), perforamce copolymer (PFA) and other Material with the filler is such fluorocarbon feedstock, which may contain elements and substances such as silicon dioxide, copper, carbon, etc. which are initially added in fluorocarbon material to give it specific properties. After using this material, when it becomes mechanical, material which cannot be used directly, but it is desirable to use as raw material in the method in accordance with the present invention, it still contains these elements. In the method in accordance with the present invention these materials will depolymerized and from them form more desirable fluorocarbon compound.

If desired or necessary, the solid powder raw material may be subjected to preliminary treatment for the removal of surface contaminants such as oil and dirt, for example, by means of solvent extraction.

Typical products that can be obtained are terraformer (CF4), tetrafluoroethylene (C2F4), exaptation (C2F6), HEXAFLUOROPROPYLENE (C3F6), hexaferrite (C4F6), the loop is the definition octafluorotoluene (c-c 4F8), decaptivation (C4F10), OCTAFLUOROPROPANE (C3F8) and other CxFychain, in which x and y are integers.

The reactor can operate with disposable loading and semi-continuous or continuous manner. Thus, the method in accordance with the present invention provides for the feeding of raw material into the reactor batch, semi-continuous or continuous. Under the "party" understand specified number of fluorocarbon, which is loaded into the reactor and injected into the reaction with the hot gaseous plasma to complete the reaction. Under semi-continuous feeding understand the filling of the hopper with raw materials and the subsequent filing of this raw material into the reactor continuously, mainly with a constant feed rate, up until the hopper is empty, after which the hopper may again be filled. Under continuous feed realize that the raw material is fed into the reactor continuously, usually with more or less constant feed rate.

While the raw material is, in principle, can be introduced into the cavity or into the first zone of the reaction chamber in any way, can be applied, in particular, flow by gravity, as it can easily be used relatively large particles of the raw material, for example, particles with sizes from 1 to 10 mm, and mainly 3 to 5 mm. Thus, the raw materials may, at tapati vertically by gravity into the chamber, directly above the heating area.

Cooling varieties or fluorocarbon precursor can be carried out in the second zone of the reaction chamber above the first zone or heating zone. Cooling can be carried out using a probe quenching, which can be self-cleaning probe. Self-cleaning probe quenching may have an outer cylindrical component mounted on the reactor, having a Central passage and adapted to cool the hot gas passing through the passage; many are placed at intervals around the circumference of the elongated teeth or scrapers projecting inward from the external component into the passageway; an inner cylindrical component that is installed with a clearance within the outer component and the inner component is also adapted to cool the hot gas passing through the peripheral gap between the components; many are placed at intervals around the circumference of the elongated teeth or scrapers projecting from the inner component to pass, and these teeth or scrapers are staggered relative to the teeth or Skrepka on the external component; and a tool actuator for bringing one cylindrical component in the oscillation relative to the other cylindrical component. By means of the actuator may be the, for example, a spring-loaded lever driven by a piston.

However, instead of the specified can be used any other suitable method of fighting, such as the rapid expansion of the resulting gas quenching (quenching) of gas with another cold gas, etc.

Reaction chamber can operate at pressures in the range from near vacuum to high pressure, depending on the more desirable fluorocarbon compounds obtained in the form of product, and other process variables. Delete (received product) can be done through the probe fighting.

Usually formed dispersion obtained in the form of the product of fluorocarbon, therefore, the method may include the separation of different products from each other.

Hereinafter the invention will be described in more detail with reference to the accompanying drawings, and to figures 1, 3-5 illustrates the block diagram in simplified form.

Figure 1 shows an installation for implementing the method of processing fluorocarbon materials in accordance with the first variant of the present invention.

Figure 2 shows a three-dimensional image of the probe quenching of the reactor 1.

Figure 3 shows an installation for implementing the method of processing fluorocarbon feedstock in accordance with a second embodiment of the present invention.

Figure 4 shows the adjustment made is tvline processing method fluorocarbon materials in accordance with the third variant of the present invention.

Figure 5 shows the installation for implementing the method of processing fluorocarbon materials in accordance with the fourth variant of the present invention.

Figure 6 shows (TFE raw materials) schedule pressure of the reactor relative to the temperature of the reactor when the reactor has a constant volume, for Example 2.

7 shows (FEP raw materials) the graph of the yield against the pressure of the reactor, for Example 2.

On Fig-10 shows the sampling schedule 7, for each of the products shown in Fig.7.

In figure 1 the position of the 10 designated in General, the installation for implementing the method of processing fluorocarbon materials in accordance with the first variant of the present invention.

The installation 10 includes a reactor 16. The reactor 16 contains a high-frequency power source (generator) 12, having the induction coil 14.

The reactor 16 also includes a stationary quartz sheath or tube 18 within which is located a graphite holder or the crucible 20. The reactor 16 has an elongated shape and is installed vertically.

The lower end of the quartz tube 18 is sealed and is water-cooled (not shown), while self-cleaning probe extinguishing 22 is in its upper end. Self-cleaning probe extinguishing 22 includes an elongated cylindrical outer component is water cooled 24, which is attached to the reactor 16. External the component 24 has a Central passage, in which are placed at equal intervals of elongated protruding radially inward of the teeth or scrapers 26. Inside the entrance of the external component 24 is located with peripheral clearance elongated cylindrical inner component 28 with water cooling. Placed at equal intervals of elongated protruding radially outward teeth or scrapers 30 are provided on the inner component 28, the teeth 30 are displaced circumferentially relative to the teeth 26. The teeth 26, 30 can move along the entire length of the components 24, 28, and the components 24 and 28 have mainly the same length. Internal component 28 is supplied by means of a drive (not shown)such as a spring-loaded lever driven by a piston, to create its oscillations with respect to the outer component 24, as shown by the arrow 32. Thus, the removal of solid contaminants from components 24, 28 are produced by fluctuations of teeth 26, 30.

Thus, the quenching probe 22 is a double annular water-cooled probe, designed for cooling gas, which is formed inside the reactor 16, as has already been mentioned here previously, to a temperature below 200°With a speed of about 105°in second. The probe is self-cleaning to prevent clogging (contamination), as in working condition on the surfaces of the probe osadetz the frozen or freeze-dried material.

The pipeline for the supply of raw materials leads 54 in a quartz tube 18 above the crucible 20, and gravity feeder 56 is connected to the pipe 54 through a pipe or tube 58.

Pipeline removal product 31 moves away from the upper end of the probe extinguishing 22 and goes to the vacuum pump 33, while the pipe 34 is from issuance of pump 33 to the compressor 36. The pipe 38 proceeds from issuance of compressor 36 to the reservoir for storage of the product 40. Pipeline removal product 42 goes from the storage tank 40 in the advanced stage of processing 44, such as a scrubber (scrubber). The pipe 46 is from the pipe 42 to the compressor 48 and the exhaust of the compressor 48 is connected by pipeline with the analytical system 52.

In the operating condition of a high temperature in the high temperature reaction chamber of the reactor 18. Using the induction coil 14 of the crucible 20, located in the zone of high temperature, is heated by induction heating. Upon reaching the desired operating temperature in the heating zone serves solid fluorocarbon powder raw material in the crucible 20 by the feeder 56 and conduits 58, 54. Generated sufficient heat for the depolymerization of raw material in the crucible 20, with the formation of gaseous products.

Then there is an immediate quenching of the gaseous products by means of probe g is the solution 22, resulting in a more desirable fluorocarbon compound which is removed through the pipes 31, 34, 38, through the vacuum pump 33 and the compressor 36, the storage tank 40. The product can be further processed in step 44, for example, to highlight specific more desirable fluorocarbon compounds from other less desirable products formed.

We now turn to a consideration of figure 3, in which position 100 is indicated in General installation for implementing the method of processing fluorocarbon feedstock in accordance with a second embodiment of the present invention.

The unit 100, which is similar to the nodes described here previously installed 10 have the same reference designators.

In the installation 100, a quartz tube or sheath 18 of the reactor 16 is inclined at an angle of between 5° and 60° the vertical and contains graphite crucible 20, having a cross, for example, annular, the inner walls (not shown). Tube 18 rotates or vibrates (oscillates). Raw material enters the upper end of the tube 18, while depolimerizovannogo gases, i.e. gaseous products out of the lower end of the tube. Extracted material of the filler leaves from the base of the tube 18, as shown by the arrow 102.

We now turn to a consideration of figure 4, in which position 50 is indicated in General installation for implementing the method of processing fluorocarbon materials in accordance with the third variant of the present invention.

The unit 150, which is similar to the nodes described here earlier units 10, 100 have the same reference designators.

To install 150 provides for the supply of the liquid raw material from the source 152. The pipeline 154 runs from source 152 to the base of the quartz tube 18 of the reactor 16 and enters the layer 156 of graphite granules.

When working layer of graphite 156 is heated using an induction coil 14. Liquid raw materials through the base of the quartz tube passes up through a layer of graphite and heated and dissociates, as has been described here previously.

We now turn to a consideration of figure 5, in which position 200 is indicated in General installation for implementing the method of processing fluorocarbon materials in accordance with the fourth variant of the present invention.

The unit 200, which is similar to the nodes described here earlier units 10, 100, and 150 have the same reference designators.

Install 200 comprises a hopper 202 for solid powder material. The hopper 202 is installed on the screw feeder 204, which is connected through pipe 206 from the base of the quartz tube 18.

When working solid powder raw material served up from the base of the reactor 16. When the solid powder raw material passes upward through the reactor 16 and the graphite crucible 20, it comes to having a high temperature zone in the roar of the reactor, dissociates and then extinguished with the help of probe 22, as has been described here previously.

The following examples, which used high-frequency generator 10 kW, 800 kHz, operating at a power of 8 kW, which is included in the installation 10 figure 1. Stationary quartz tube reactor 18 16 has a nominal diameter of 70 mm and a length of 300 mm, the Pumping system was carried out through a filter (not shown) using a reliable dry vacuum pump 33. All pressure ratings are in kPa, while the yield of the product specified in the relative volume%.

Example 1

System 10 operates continuously, with about 2 kg/h material powder of PTFE without filler or depleted PTFE continuously fed into the crucible 20.

It was found that the reactor 16 must be evacuated to a relatively high vacuum, in order to maximize the output of TFE. For different formulations of products require different raw materials (raw) materials and process parameters. For the desired composition of the product requires specific ranges of temperature and pressure. For example, for depolymerization of PTFE and receive TFE as the main product in the reactor 16, you must create a reaction temperature between 400°700°and a pressure below atmospheric.

It was found that the required heating time of about 5 minutes to achieve a slave who whose temperature between 400° With up to 700°C. during this time a number of raw materials available in the crucible 20, although the feeder is not yet powered. This raw material is softened and begins to depolimerizatia. When reaching the operating temperature include feeder 56 to provide feeding performance of about 2 kg/H. optionally, the feed rate of material to install 10 kW can be varied from 1 kg/h to 10 kg/h

At operating temperatures between 400°700°and a pressure below atmospheric (about 1 kPa) is immediate depolymerization of PTFE using pyrolysis, with PTFE evaporates and decomposes with the generation of fluorocarbon precursor or reactive species. These precursor or reactive species of fluorocarbon immediately extinguished by quenching probe 22, which allows to obtain a TFE. Due to the re-polymerization of gaseous TFE observed the deposition of fine white powder on all cold surfaces of the reactor 16, which is then cleaned with self-cleaning probe quenching. The results obtained are summarized in Table 1.

Table 1
Analytical results
ProductsExample 1 - gaseous products
F 4(%)-
With2F6(%)0,062
With2F4(%)83,9
With3F6(%)6,83
c-C4F8(%)9,01

Successful depolymerization of PTFE in this example occurs when the specific energy of about 1 kWh/kg of PTFE. Not expected to have significant problems with the process parameters for the volume change of the installation.

Installation or system 10 has been specially adapted for processing not used directly PTFE material, in addition to receiving TFE (C2F4), which is a precursor for the production of other complex fluorocarbons, for example, C-C4F8. This processing may be performed in step 44.

Table 1 shows a surprisingly high yield of C2F4especially if to take into account that the configuration of the installation 10 has not been optimized.

Example 2

In this example we have studied the conversion of waste material FEP (fluorinated copolymer of ethylene and propylene) into useful products of high quality, such as TFE (tetrafluoroethylene), HFP (HEXAFLUOROPROPYLENE) or C-C4F8(circular octafluorotoluene), in function of the reactor pressure vessel, for two separate profiles the temperature is s.

During the preliminary test runs found that the efficiency of the reaction, and the formed products are very sensitive to the pressure of the reactor, and the temperature of the crucible. To determine reference data concerning the dependence on pressure is primarily conducted one preliminary run. In this preliminary run was used a closed container of fixed volume defined inside temperature sensors and pressure, for the gradual heating of a fixed quantity of material TFE with a temperature gradient, at check gas pressure in function of temperature. Figure 6 shows the data obtained, and figure 6 shows a series of superimposed tabs on gradually increasing the podium on a regular R/T curve of constant volume. This shows that the formation of different products at different temperatures with a corresponding pressure change, if you change the volume (number of molecules). During the recombination reaction pressure falls, and during the reaction dissociation pressure increases. A careful study of the bending pressure in combination with the available information about the reaction allows to identify the predominant product for each area of the temperature, which is also shown in Fig.6. For example, TFE begins to recombine with the formation of the SS 4F8at a temperature of 270°C. In turn, C-C4F8starts dissociate at a temperature of 450°with the formation of HFP. These products are stable after blanking. As the production of HFP is a predominant task for subsequent test runs, the temperature of the crucible were selected about 600°C.

When conducting subsequent test runs installation 10 figure 1 and 2 again worked in continuous mode, the continuous supply of FEP in the crucible (ID=54 mm, OD=64 mm, length=180 mm) (where the ID and OD of the inner and outer diameters, respectively), which was melting and chemical cracking of the material. Coil surrounding the crucible was modified to uneven heating and create a temperature profile which increases from bottom to top. Primarily this was done to prevent condensation of liquid or solid product earlier achievements probe quenching. Secondly, because the depolymerization reaction mainly takes place at the base of the crucible at the end of lower temperature), the upper end of the crucible should be heated stronger to ensure full sublimation vapor. Thirdly, the hot zone is a pre-heating zone for FEP particles when they come into the crucible. During the first run of the crucible was heated to a temperature of from 630°do° With center at 710°C, and the run was named as "630°". The second run was carried out between 600°and 780°With center at 700°and accordingly he was called as "600°". The results obtained are summarized in Table 2.

Table 2
630°
Pressure2030506080100120
TFE52302517
HFP38505264
with the-C4F810171814
600°
TFE6247332523
HFP3237414244
with the-C4F8of 5.417272828

Table 3
The power input (kW)4
Enthalpy (kWh/kg)1,6
The mass flow rate of FEP (kg/h)2,4
Running time (h)4
C2F4(kg/h)1,04
With3F6(kg/h)0,782
c-c4F8(kg/h)0,31
The balance of fluorine100%
A full mass balance89%

The results in Table 2 are shown graphically in Fig.7, where the apparent dependence of the yield of the product of pressure and temperature. On Fig-10 shows a sample of schedule 7, one for each product. Table 3 shows the operating conditions, the balance of fluorine and a complete mass balance. With the full mass balance 89%, a loss of 11% of the mass is caused mainly due to the formation of solids on the cold surfaces.

7 shows that as a rule if the pressure output TFE decreases (see also Fig), exit c-c4F8passes through a maximum (see also Fig.9), and the output of HFP increases (see also figure 10). Temperature significantly affected by n the last two materials, in the sense that the higher the temperature profile of the crucible substantially increases the yield of HFP and reduces the output with the-C4F8. It can be assumed that the retention time of the gaseous product at a higher temperature sufficient for the formation of a larger number of HFP due to the decomposition of C-C4F8. In contrast, the much softer the effect of temperature is observed in the production of TFE (Fig). This is probably caused by the fact that in both runs the production of TFE at appropriate temperatures in the crucible was completed at that time (see Fig.6), when the gas reaches the probe quenching, and there is a dissociation rate TFE for the next two product selectivity which depends on the temperature of the crucible.

From the preceding it is obvious that can be obtained for more standard experimental sets of parameters of temperature and pressure to optimize control of selectivity at least for most combinations of desirable products. It is also clear that the process can be extended to include the conversion of the feedstock in the form of liquid is not used directly fluorocarbon.

This method of conversion FEP into useful products is cheap, reliable, does not create pollution, versatile and have easy control is selected. In combination with well-developed distillation installations of high purity can be obtained valuable products of high quality.

Typical products that can be obtained by the method in accordance with the present invention, are CxFychain, in which x and y are integers. In such chains in the production of TFE main product represents approximately 90% TFE.

Found that induction generator 12 is highly effective, and in the environment loses little energy. The installation 10 has a very short start-up time.

The advantage of the method in accordance with the present invention is that it is not required to transport the gas, and the resulting products are relatively clean. Therefore, usually require only a relatively simple stage distillation for separating the received TFE obtained from other products.

According to the method in accordance with the present invention is not directly used fluorocarbon materials with or without filling can be depolymerizer and transformed in a relatively clean, high-value products through pyrolysis, with minimum requirements for distillation downstream.

1. The method of processing fluorocarbon materials, including:

heating using Vysokoye the Noah induction heating zone of the reaction chamber to a temperature of not more than 950° C;

the heating in the heating zone fluorocarbon feedstock which contains at least one fluorocarbon compound;

the selection pressure in the reaction chamber and the temperature of the heating zone so that the fluorocarbon compound dissociates or depolymerized with getting at least one more desirable fluorocarbon compounds;

education hot gaseous product that contains more than the desired fluorocarbon compound, and

the damping of the hot gaseous product to stabilize more desirable fluorocarbon compounds.

2. The method according to claim 1, characterized in that use reaction chamber of the reactor, which has an elongated cylindrical shell, and the reaction chamber has a heating zone, the heating zone of the reaction chamber provides a container for raw materials.

3. The method according to claim 2, characterized in that the high-frequency induction heating is carried out using a high frequency induction furnace having an induction coil inside the heating zone of the reactor.

4. The method according to claim 2 or 3, characterized in that the shell of the reactor is stationary and is held vertically.

5. The method according to claim 2 or 3, characterized in that the shell of the reactor is inclined at an angle to the vertical and rotates the sludge is oscillates.

6. The method according to claim 3, characterized in that the reactor comprises a graphite crucible having a transverse partition for regulating the retention time of the feedstock in the reactor.

7. The method according to one of claim 2 to 6, characterized in that the raw material is a fluorocarbon liquid, and pure raw material contains a single fluorocarbon compound or not used directly fluorocarbon product that contains two or more fluorocarbon compounds, one compound is present in the product as the main component so that it forms a large part of the product, the raw materials were fed into the reactor from below.

8. The method according to one of claim 2 to 6, characterized in that the raw material is a fluorocarbon solid powder, such as is not used directly material filler with or without it, which can be pre-treated to remove the surface contamination, the raw materials were fed into the reactor at the top or bottom.

9. The method of claim 8, wherein the fluorocarbon feedstock is introduced into the reaction chamber through a vertical gravity feed to the reaction chamber, directly above the heating zone, and the particles of the raw material have a size of 1-10 mm

10. The method according to one of claim 2 to 9, characterized in that the damping of the hot gaseous product is carried out in the second zone of the reaction chamber above the e first zone or heating zone.

11. The method according to claim 10, in which the quenching is carried out with the help of self-cleaning probe fighting

12. The method according to claim 11, characterized in that a self-cleaning probe extinguishing contains an outer cylindrical component mounted on the reactor, having a Central passage and adapted to cool the hot gas passing through the passage; many are placed at intervals around the circumference of the elongated teeth or scrapers projecting inward from the external component into the passageway; an inner cylindrical component that is installed with a clearance within the outer component and the inner component is also adapted to cool the hot gas passing through the peripheral gap between the components, many are placed at intervals around the circumference of the elongated teeth or scrapers projecting from the inner component to pass, moreover, these teeth or scrapers are staggered relative to the teeth or Skrepka on the external component and the tool actuator for bringing one cylindrical component in the oscillation relative to the other cylindrical component.



 

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Reactor // 2259873

FIELD: processes of fluoride technology in reworking titanium-containing raw material, for example, ilmenite concentrates in production of titanium dioxide.

SUBSTANCE: proposed reactor has housing made in form of body of revolution, reaction component mixing unit, heating unit located outside the reactor, solid reaction component loading unit, reaction product unloading unit, reagent supply unit and gas discharge branch pipe. Reaction component mixing unit is made in form of drive for rotation of reactor housing; it is made in form of truncated cone at inclination of generatrix to longitudinal axis of housing up to 10° which is mounted for rotation about longitudinal axis which forms lesser angle of inclination of generatrix to longitudinal axis of housing towards reaction product unloading unit; solid reaction component loading unit is made in end part of reactor housing with lesser transversal sizes and reaction product unloading unit is made in opposite end part of reactor housing. Reactor cavity is divided into two reaction zones which are heat-insulated relative to each other. Reaction zone adjoining solid reaction component loading unit is provided with coat made from material resistant to action of fluoride-containing materials which retains strength at temperature of not below 400°C, for example magnesium; reaction zone adjoining the reaction product unloading unit is provided with coat made from material retaining strength at temperature not below 900°C, preferably from silicon oxide; besides that, reactor is hermetic and is connected with vapor source. External envelope of reactor consists of two parts whose length is equal to length of respective reaction zones; they are made from heat-resistant structural materials which are resistant to action of fluoride-containing materials and are heat-conducting, for example metal alloys. Parts of reactor external envelope are rigidly and hermetically interconnected and are heat-insulated relative to each other. Proposed reactor has increased serviceability at pyrohydrolysis of ammonium oxofluorotitaniums at simultaneous obtaining titanium dioxide of high degree of whiteness.

EFFECT: enhanced reliability and serviceability of reactor.

5 cl, 1 dwg

The invention relates to methods of producing liquid glass hydrothermal alkaline treatment of silica-containing raw material and equipment for their implementation

The invention relates to a device for contacting the solid material in the form of loose particles of liquid or solid material from liquids and gases in the reactor by bringing the reactants into contact with each other, comprising a housing and a fixed sieve element, which is communication, with the sieve element is designed as a rotating drum 5

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a new method for preparing methanol and other aliphatic alcohols by gas-phase interaction of hydrocarbon gases with water vapor under effect of ultraviolet radiation. Methanol and other aliphatic alcohols are prepared by direct hydroxylation of hydrocarbon gas or mixture of hydrocarbon gases with water vapor. For this aim hydrocarbon gas and vapor or mixture of gases and vapor are fed into reactor wherein the reaction mass is subjected for effect of ultraviolet radiation in wavelength range 240-450 nm at temperature lower vapor formation point. The end product is isolated from vapor-gaseous mixture by condensation and unreacted gas or mixture of gases removed from the reaction zone is purified from the end product by bubbling through water layer and recovered into reactor by adding the parent gaseous component in the amount equal to consumed one. The process is carried out for a single stage and can be realized under atmosphere pressure. Invention can be used in chemical, petroleum chemical, petroleum processing and petroleum and gas extracting industry.

EFFECT: improved preparing method.

2 cl, 1 tbl, 8 ex

FIELD: liquid-phase reforming.

SUBSTANCE: the invention is pertaining to liquid-phase reforming of hydrocarbons or oxygen-containing compositions. The method is exercised by interaction of a hydrocarbon or an oxygen-containing organic composition with water using a pulse electrical discharge in a liquid containing the indicated hydrocarbon or a oxygen-containing organic composition and water. Such a method is exercised in the apparatus, that includes a reactor, electrodes positioned inside the pointed reactor, a direct-current source for feeding the direct current to the pointed electrodes and an outlet opening for withdrawal of produced as a result of it hydrogen and carbon monoxide. The given invention allows realization of the process at normal temperature and a pressure, and at that there is no necessity for an additional stage of separation of products of the unreacted substances. Moreover the by-products such as acetylene are dissolved and absorbed in the liquid and again interact with the following conversion into synthesis gas.

EFFECT: the invention allows realization of the process at normal temperature and a pressure, excluding necessity for an additional stage of separation of products of the unreacted substances.

16 cl, 5 dwg, 3 ex, 3 tbl

FIELD: production of nanodispersed powders of refractory inorganic materials and compounds, in particular, installations and methods for realization of plasmochemical processes of production of nanodispersed powder products.

SUBSTANCE: the installation comprises production-linked: microwave oscillator 1, microwave plasmatron 2, gas-flow former 3, discharge chamber 4, microwave radiation absorber 5, reaction chamber 6, heat-exchanger 7, filter-collector of target product (powder) 8, device for injection of the source reagents in a powdered or vapors state into the reaction chamber, the installation has in addition a device for injection of the source reagents in the liquid-drop state, it has interconnected proportioner 9 in the form of cylinder 10, piston 11 with gear-screwed electric drive mechanism 12 adjusting the speed of motion of piston 1, evaporative chamber 13 with a temperature-controlled body for regulating the temperature inside the chamber that is coupled to the assembly of injection of reagents 14 in the vaporous state and to the assembly of injection of reagents 15 in the liquid-drop state, injection assembly 14 is made with 6 to 12 holes opening in the space of the reaction chamber at an angle of 45 to 60 deg to the axis of the chamber consisting at least of two sections, the first of which is connected by upper flange 16 to the assemblies of injection of reagents, to discharge chamber 4, plasmatron 2, with valve 17 installed between it and microwave oscillator 1, and by lower flange 18, through the subsequent sections, it is connected to heat exchanger 7, the reaction chamber has inner water-cooled insert 20 rotated by electric motor 19 and metal scraper 21 located along it for cutting the precipitations of powder of the target product formed on the walls of the reaction chamber, and heat exchanger 7 is made two water-cooled coaxial cylinders 22 and 23, whose axes are perpendicular to the axis of the reaction chamber and installed with a clearance for passage of the cooled flow, and knife 24 located in the clearance, rotating about the axis of the cylinders and cleaning the working surfaces of the cylinders of the overgrowing with powder, powder filter-collector 8 having inside it filtering hose 25 of chemically and thermally stable material, on which precipitation of powder of the target product from the gas flow takes place, in the upper part it is connected by flange 26 to the heat exchanger, and in the lower part the filter is provided it device 27 for periodic cleaning of the material by its deformation, and device 28 with valve 29 for sealing the inner space of the filter. The method for production of nanodispersed powders in microwave plasma with the use of the claimed installation consists in injection of the source reagents in the flow of plasma-forming gas of the reaction chamber, plasmochemical synthesis of reagents, cooling of the target product and its separation from the reaction chamber through the filter-collector, the source reagents are injected into the flow of plasma-forming gas, having a medium-mass temperature of 1200 to 3200 K in any state of aggregation: vaporous, powdered, liquid-drop or in any combination of them, reagents in the powdered state are injected in the form of aerosol with the gas-carrier into the reaction chamber through injection assembly 35 with a hole opening into the space of the reaction chamber at an angle of 45 to 60 deg to the chamber axis, reagents in the liquid-drop or vaporous state are injected into the reaction chamber through injection assemblies 15 or 14, respectively, in the form of ring-shaped headers, the last of which is made with 6 to 12 holes opening into the space of the reaction chamber at an angle of 45 to 60 deg to the chamber axis, each of them is blown off by the accompanying gas flow through the coaxial ducts around the holes, at expenditure of the source reagents, plasma-forming gas, specific power of microwave radiation, length of the reaction zone providing for production of a composite system and individual substances with preset properties, chemical, phase composition and dispersity.

EFFECT: universality of the industrial installation, enhanced capacity of it and enhanced duration of continuous operation, as well as enhanced yield of nanodispersed powders and expanded production potentialities of the method.

20 cl, 1 dwg, 4 ex

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