Title of Invention

INSTALLATION FOR SYNTHESIS OF TITANIUM DIOXIDE AND PLASMA CHEMICAL REACTOR

Abstract The installation for synthesis of titanium dioxide contains a plasmotron, connected to a source of oxygen, a plasma chemical reactor connected to a consumable vessel of titanium tetrachloride, a hardening chamber having in its bottom portion a pneumatic pulsed generator, a heat exchanger of 'tube in tube' type, which is coupled coaxially and directly to an output radial tube of the hardening chamber, a cyclone, having a quenching chamber and a filter. Injectors are mounted in the median zone of the body of plasma chemical reactor to ensure injection of titanium tetrachloride; beneath that level, a circular muzzle is located, having a form of a annular channel adjacent to the wall meant for the injection of a protection gas (oxygen) forming a thin whirlwind layer of a protection gas curtain.
Full Text FORM 2
THE PATENT ACT 1970
(39 of 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See section 10 and rule 13)
1. INSTALLATION FOR SYNTHESIS OF TITANIUM DIOXIDE AND
PLASMA CHEMICAL REACTOR
2. 1.
(A) GOROVOI, Yury Mikhailovich
(B) RUSSIA
(C) ul. Senjukova, 41-73, Ukhta, 169300, Respublika Komi Russia.
2.
(A) KLYAMKO, Andrei Stanislavovich
(B) RUSSIA
(C) ul. Michurinskaya, 1-191, St.Petersburg, 197046 Russia.
3.
(A) PRANOVICH, Alexandr Alexandrovich
(B) RUSSIA
(C) ul. Dzerzhinskogo, 29-195, Ukhta, 169300, Respublika Komi Russia.
4.
(A) VLASENKO, Viktor Ivanovich
(B) RUSSIA
(C) ul. Naberezhnaya Neftyanikov, 15-7, Ukhta, 169300, Respublika Komi Russia.
5.
(A) KORZHAKOV, Vladimir Viktorovich
(B) RUSSIA
(C) ul Pervomaiskaya, 7-26, Ukhta, 169300, Respublika Komi Russia.
The following specification particularly describes the invention and the manner in which it is to be performed.


Pertinent art
The invention belongs to manufacturing of powdery materials and can be used for producing of the titanium dioxide by the chloride technique.
Previous background
Among the background the Installation for synthesis of titanium dioxide by the chloride technique, containing series connected plasmatron connected to the oxygen source or the oxygen-containing gas source, the plasmachemical reactor connected to the supply tank of the titanium tetrachloride, the hardening chamber, the heat exchanger and the synthesis products separation block consisting of the cyclone and the filter (RU 2057714 CI, CO1G23/047, 1996) is known. The main shortcoming of the known solution is constant clogging of the heat exchanger and the cyclone with sediments of the titanium dioxide, that requests the suspensions of productions for cleanings, and the presence of several outlets of the titanium dioxide that complicates the structure and weakens the work of the Installation in whole.
It is also known the plasmachemical reactor for producing of the titanium dioxide by the chloride technique, containing axisymmetrical case with water-cooled walls and the outlet in the bottom part, the plasma generator, placed in the top part of the case, and the injection valve for the batching, set in the middle body of the case, which jets are directed to the outlet, (RU 2052908 CI, H05H1/42, 1996; WO 97/19895 Al, H05H1/42, 1997). The capacity of building-up of stubborn tags on the wall of the reactor below the injection valves during producing of the titanium dioxide that results in trouble of conditions of the process course, to deterioration of the derivable product and to loss in reliability of work of the reactor and


Installation for synthesis of the titanium dioxide by the chloride technique in whole should be referred to the shortcomings of this reactor structure.
Disclosure of the invention
The invention is aimed to upgrading of efficiency and reliability of work of the Installation for synthesis of the titanium dioxide and improvement of the operational characteristics of the plasmachemical reactor by exception of building-up of growth of tubercles on the wall of the reactor in the jet zone of the atomization of precursors by the injection valves.
The solution of the assigned task is provided that in the Installation for synthesis of the titanium dioxide, containing series connected the plasmatron connected to the oxygen source or the oxygen-containing gas source, the plasmachemical reactor, connected to the supply tank of the titanium tetrachloride, the hardening chamber, the heat exchanger and the synthesis products separation block consisting of the cyclone and the filter, pursuant to the invention, the hardening chamber is made with the cylindrical case to which conic bottom the bunker of the coarse fraction of the titanium dioxide is connected, and radially located outlet nozzle, and additionally supplied with the air-impact generator which trunk is set in the bottom part of the cylindrical case coaxially and diametrally opposite to the radial outlet nozzle, moreover the heat exchanger is made as one-tubular one such as «a pipe in a pipe» and coaxially - is directly connected to the radial outlet nozzle of the hardening chamber, and the cyclone of the synthesis products separation block, which input is connected to the heat exchanger, made with the axisymmetrical damping chamber coaxially placed between the case and the branch pipe at the following ratio rating of geometric parameters:


d/D = (0.1-0.7),
where d - the maximum diameter of the damping chamber;
D - diameter of the cylindrical case.
Besides the inlet nozzle of the ash-laden gas of the bag filter of the synthesis products separation block is connected to the branch pipe of the cyclone, and the outlet nozzle of retained particles is connected by the traffic artery to the perimeter zone of the top part of the cylindrical case of the cyclone which is made with the conic bottom supplied with the pneumatic Installation of the titanium dioxide.
The solution of the assigned task is also provided that in the plasmachemical reactor containing the axisymmetrical case with water-cooled walls and the outlet in the bottom part, the plasma generator placed in the top part of the case, and the injection valve for the batching, set in the middle body of the case which jets are directed to the outlet, pursuant to the invention, on the wall of the case the annular jet is made in the form of the wall annular channel directed coaxially to the outlet, formed by the annular collar of the case and the internal wall of the collector ring for input of the protective gas, supplied with equally spaced tangential holes, moreover the exit plane of the annular jet is placed below the level of the nozzle exit of the injection valves equally spaced on a circle, in the distance
H where H - distance between the exit plane of the annular jet and the level of the placement of the outlets of the injection valves;
DI - diameter of the case;
D2 - diameter of the circle on which the injection valves are set;
a - a spray-cone angle of the injection valves.


Preferably, one central injection valve coaxially should be placed, in the middle body of the case, mainly in a low-power reactor.
And the plasma generator - the plasmatron can be made with cathode and anode packs, which are set at an angle with each other and are supplied with oxygen supply nozzles.
Presence of the annular jet with the collector ring, placed below the level of nozzle exits of the injection valves in the distance, provides forming of the thin layer of the gas haze in the form of the rotating flow of protective gas at the wall of the reactor case below the level of placement of the injection valves which prevents touchdown of unreacted drops of reagents with the wall and building-up of growths of tubercles, but which light gauge excludes the negative influence on course of processes in the space of the reactor.
Placement of the air-impact generator in the hardening chamber and performance of the heat exchanger in the form of one-tubular one such as «a pipe in a pipe» with coaxial - direct connection of it to the radial outlet nozzle of the hardening chamber allows to send periodically pneumatic pulses from the generator through its trunk to the channel of the heat exchanger, under the influence of which the destruction of sediments of the titanium dioxide is taken place, that excludes the possibility of clogging of the heat exchanger with titanium dioxide, and their effective removal -taking away from the channel of the heat exchanger is made by the powder-gas flow proceeding with the weight rate - the mass flow density from 5 up to 80 kg / m2 sec.
Moreover the declared structure of the cyclone with presence of the damping chamber which is the additional nonsolvent, promotes efficiency


upgrading of sedimentation of fine fractions of the titanium dioxide powder up to 82 ¸ 97 %. Besides, the connection of the outlet nozzle of retained particles of the bag filter by the traffic artery to the perimeter zone of the top part of the cylindrical case of the cyclone reduces the number of outlets of the titanium dioxide, that also promotes simplification of the structure and improvement of reliability of work of the Installation.
The brief description of figures of drawings
On Fig. 1 the chart of the Installation for synthesis of the titanium dioxide is represented; on Fig. 2 the longitudinal section - the general view of the plasmachemical reactor is represented; on figs. 3 - cross-section A-A on fig. 2; on fig. 3 - the view B on fig. 2.
The best variant of realization of the invention
The Installation (Fig. 1) contains series connected plasmatron 1 to which the oxygen source 2 is connected, the plasmachemical reactor 3 which is connected to the supply tank 4 by the pump 5 of the input of the titanium tetrachloride, the hardening chamber 6 supplied with the air-impact generator 7, the heat exchanger 8 which is made in the form of one-tubular one such as «a pipe in a pipe» as a straight pipe or rectangular coils of straight pipes with smoothly rounded interfaces and it is connected coaxially - directly by the inlet to the radial outlet nozzle 9 of the hardening chamber 6, and the synthesis products separation block 10, including the cyclone 11, the tangential inlet nozzle 12 of which is connected to the heat exchanger 8, and the bag filter 13. The exhaust trunk 14 of the air-impact generator 7 is set in the wall of the bottom part of the cylindrical case of the hardening chamber 6 coaxially and diametrally opposite to the radial outlet nozzle 9 and, accordingly, to the inlet of the heat exchanger 8. The cyclone 11 is


made with the axisymmetrical cone-cylindrical damping chamber 15, the maximum diameter «d» of which ranges from 0.1 up to 0.7 of diameter «D» of the cylindrical case, in which conic bottom the pneumatic Installation 16 is set. The branch pipe 17 of the cyclone 11 is connected to the inlet nozzle 18 of the ash-laden gas of the bag filter 13, the outlet nozzle 19 of retained particles of which is connected by the traffic artery 20 (the screw conveyor) to the perimeter zone of the top part of the cylindrical case of the cyclone 11. The plasmachemical reactor 3 (Fig. 2, 3 and 4) contains the case made from water-cooled top part 21 in which cathode and anode packs 22 and 23 of the two-spool plasma generator - a plasmatron 1 are set, and bottom part 24 with the outlet 25, and set in the middle body of the case (in the bottom of the top part 21) the injection valves 26 for batching with branch pipes 27 for input of the liquid titanium tetrachloride, which jets are directed to the outlet 25. Between the top and bottom parts 21 and 24 of the case the collector ring 28 for input of protective gas is set, and the top part 21 of the case is supplied below with the fillet 29, forming with the internal wall 30 of the collector rings 28 which is made with equally spaced tangential holes 31, the annular jet 32 in the form of the wall annular channel, directed coaxially to the outlet 25. Moreover the exit plane of the annular jet 32 is placed below the level of nozzle exits of the injection valves 26 equally spaced on a circle, in the distance
H where H - the distance between the exit plane of the annular jet and the level of the placement of the outlets of injection valves;
D1 - diameter of the case;
D2 - diameter of the circle on which the injection valves are set;
a - spray-cone angle of the injection valves.


The declared invention is carried out as follows.
In cathode 23 and anode 24 packs of the plasma generator - the plasmatron 1 from the source 2 the oxygen which in the bridge of the plasmatron 1 is heated up to the plasma state is supplied. From the plasmatron 1 the jets of oxygen plasma enter into the internal space of the top part 21 of the case of the plasmachemical reactor 3 where the flow of oxygen plasma which fills in all area of cross section of the case is formed, and, flowing around the injection valves 26, goes to the outlet 25. To the injection valves 26 through the branch pipes 27 from the supply tank 4 by the pump 5 the liquid titanium tetrachloride (TiC14) is supplied under the pressure, and to the collector ring 28 trough the branch pipe 33 the protective gas - oxygen is supplied, moreover the jets of oxygen, proceeding through tangential holes 31 of the collector rings 28, is twisted and go to the wall of the case of the reactor tangentially, and the fillet 29 prevents the distribution of jets of oxygen in radial direction deep into the space of the reactor. The injection valves 26 spray the titanium tetrachloride, the jet of the atomization is mixed up with plasma of oxygen, forming the reacting stream in which the titanium tetrachloride is volatilized and the vapors are acidified to the titanium dioxide. The stream of protective gas - oxygen flowing out of the annular jet 32 in the axial direction forms thin vortical layer of the gas haze in a zone of jets of the atomization of the injection valves, preventing the fall of large drops of the titanium tetrachloride on the wall of the case of the reactor, which have not time to volatilize and when contacting with the wall of the case of the reactor can form stubborn tags that improve stability and reliability of work of the reactor, promotes


improvement of operational characteristics of the Installation for synthesis of the titanium dioxide and improvement of quality of the received product.
The products of reaction, leaving the reactor - of synthesis of the titanium dioxide which are the powder-gas flow - the gas suspension of particles of the titanium dioxide with the size 0.2 ¸1.0 microns in the chlorine - gas consisting of chlorine and exuberant oxygen, enters into the hardening chamber 6 where their partial cooling is taken place and sedimentation of the coarse fraction of the titanium dioxide which collects in the bunker 34 of the coarse fractions attached to the conic bottom of the cylindrical case of the hardening chamber 6, and then goes for processing. The powder-gas flow of products of reaction from the hardening chamber 6 through the radial outlet nozzle 9 is directed to the rectilinear inlet of the heat exchanger 8 in which their final cooling is taken place. From the heat exchanger 8 through the tangential inlet nozzle 12 the powder-gas flow enters into the top part of the cylindrical case of the cyclone 11 where under the centrifugal effect the sedimentation of the titanium dioxide from the powder-gas flow into the conic bottom is taken place. The twirled powder-gas flow from the case of the cyclone 11 enters into the damping chamber 15 at which wall the tangential speed of flow is much higher than tangential speed at the wall of the case that provides more full sedimentation of fine particles of the titanium dioxide. Chlorine - gas with the residual titanium dioxide from the damping chamber 15 through the branch pipe 17 is supplied to the inlet nozzle 18 of the ash-laden gas of the bag filter 13 where the clearing of chlorine - gas from the residual titanium dioxide is taken place. Chlorine - gas from the bag filter 13 goes to the consumer, and the caught titanium dioxide from the outlet nozzle 19 of retained particles


through the traffic artery 20 (the screw conveyor) is directed to the perimeter zone of the top part of the cylindrical case of the cyclone 11. Settled in the conic bottom of the cyclone 11 the fine particles of the titanium dioxide are transferred to the further processing by means of the pneumatic Installation 16.
During the synthesis of the titanium dioxide the air-impact generator 7, the exhaust trunk 14 of which is set in the wall of the bottom part of the cylindrical case of the hardening chamber 6 coaxially and diametrally opposite to the radial outlet nozzle 9 and, accordingly, to the input - opening straight-line portion of the heat exchanger 8, periodically sends pulses of pressure and underpressure to the flowing internal channel of the heat exchanger 8 which destroy the sediments of the titanium dioxide on the internal walls of the heat exchanger 8, and the taking away of the fractions of the titanium dioxide from the heat exchanger 8 is carried out by the powder-gas flow with the following flow parameters :
G / F = pu = 5 ¸ 80 kg/m2sec,
where G / F- weight rate of the powder-gas flow;
pu - the mass flow density of the powder-gas flow;
G - the weight rate of the cooled medium through the channel, kg /sec;
F - the area of cross section of the channel of the heat exchanger,
p- density of the cooled medium, kg;
u - flow rate of the cooled medium,
Moreover the presence of clogging of the channel of the heat exchanger 8 arises at pu 80 kg/m sec hydraulic resistance of the heat exchanger 8 sharply grows.


Operating conditions of process of producing of the titanium dioxide, confirming efficiency and reliability of work of the Installation, are given in the table 1, and the work effectiveness measure of the cyclone are given in the table 2.
The table 1

The powerof theplasmo tronkW, Component consumption of Yield of titaniumdioxide kg/h Parameters ofthe heatexchanger The mass flowdensitypu,kg/(sec*m2) Presenceof cloggingof thechannel oftheheatexchanger
TiC14,kg/h titaniumdioxidekg/h totalkg/sec Diame ter of chann el, m crosssection,m2
55 106 22 0,0375 44 0,1 7,85 103 4,85 Present
60 117 25 0,0394 49 0,1 7,85 .10-3 5,00 Absent
120 235 50 0,0792 98 0,1 7,85. 10-3 10,08 Absent
240 470 100 0,1583 196 0,1 7,85. 10-3 20,16 Absent
150 290 60 0,097 120 0,05 2,00. 10-3 48,5 Absent
240 475 100 0,16 200 0,05 2,00. 10-3 80 Absent


The table 2
The case of the cyclone DamperDiameter d, m Ratio d/D Efficiencyof thedustsettling Presence of theclogging of thecyclone
Diameter D, m Height m
3 3 1,2 0,4 97 Absent
3 3 0,3 0,1 82 Absent
3 3 0,24 0,08 75 Absent
3 3 2,25 0,75 80 Absent
3 3 2,1 0,7 87 Absent
2 1,6 0,4 0,2 85 Absent
3 3 1,5 0,5 95 Absent
1.6 1.6 0.6 0.4 97 Absent


I Claim:
1. The Installation for synthesis of the titanium dioxide, containing series connected the plasmatron connected to the oxygen source or the oxygen-containing gas source, the plasmachemical reactor connected to the supply tank of the titanium tetrachloride, the hardening chamber, the heat exchanger and the synthesis products separation block consisting of the cyclone and the filter, characterized by that the hardening chamber is made with the cylindrical case to which conic bottom the bunker of the coarse fraction of the titanium dioxide is connected, and radially located outlet nozzle, and is additionally supplied with the air-impact generator which trunk is set in the bottom part of the cylindrical case coaxially and diametrally opposite to the radial outlet nozzle, moreover the heat exchanger is made in the form of the one-tubular one such as «a pipe in a pipe» and is coaxially - directly connected to the radial outlet nozzle of the hardening chamber, and the cyclone of the synthesis products separation block, which input is connected to the heat exchanger is made with the axisymmetrical damping chamber coaxially placed between the case and the branch pipe at the following ratio rating of geometric parameters:
d/D = (0.1¸0.7),
where d - maximum diameter of the damping chamber;
D - diameter of the cylindrical case.
2. The Installation for synthesis of the titanium dioxide under the article 1, characterized by that the inlet nozzle of the ash-laden gas of the bag filter of the synthesis products separation block is connected to the branch pipe of the cyclone, and the outlet nozzle of retained particles is connected by the traffic artery to the perimeter zone of the top part of the cylindrical case of


the cyclone which is made with the conic bottom supplied with the pneumatic Installation of the titanium dioxide.
3. The plasmachemical reactor containing the axisymmetrical case
with water-cooled walls and the outlet in the bottom part, which top part is
connected to the plasma generator, and the injection valves for batching of
titanium tetrachloride, set in middle body of the case, which jets are directed
to the outlet, characterized by that on the wall of the case the annular jet is
made in the form of the coaxially directed to the outlet of the wall annular
channel, formed by the annular collar and the internal wall of the collector
ring for input of the protective gas, supplied with equally spaced tangential
holes, moreover the exit plane of the annular jet is placed below the level of
nozzle exits of the injection valves equally spaced on a circle, in the distance
H where H - distance between the exit plane of the annular jet and the level of the placement of the outlets of the injection valves;
D1 - diameter of the case;
D2 - diameter of the circle on which the injection valves are set;
a - the spray-cone angle of the injection valves.
4. Installation for synthesis of the titanium dioxide and the
plasmachemical reactor as herein described with forgoing description and
drawings.


Abstract
The Installation for synthesis of the titanium dioxide contains the plasmatron connected to the oxygen source, the plasmachemical reactor connected to the supply tank of the titanium tetrachloride, the hardening chamber with the air-impact generator set in the bottom part, the heat exchanger such as «a pipe in a pipe», is coaxially - directly connected to the radial outlet nozzle of the hardening chamber, the cyclone made with the damping chamber, and the filter. In the middle body of the case of the plasmachemical reactor the injection valves for input of the titanium tetrachloride are set, the annular jet in the form of the wall annular channel with the collector ring for input of protective gas - the oxygen forming the thin vortical layer of the protective gas haze is made lower its level.


Documents:

04-mumnp-2008-abstract.doc

04-mumnp-2008-abstract.pdf

04-mumnp-2008-claims.doc

04-mumnp-2008-claims.pdf

04-mumnp-2008-correspondence-others.pdf

04-mumnp-2008-correspondence-received.pdf

04-mumnp-2008-description (complete).pdf

04-mumnp-2008-form-1.pdf

04-mumnp-2008-form-2.doc

04-mumnp-2008-form-2.pdf

04-mumnp-2008-form-3.pdf

04-mumnp-2008-form-5.pdf

04-mumnp-2008-pct-search report.pdf

4-MUMNP-2008-ABSTRACT(1-1-2008).pdf

4-MUMNP-2008-ABSTRACT(GRANTED)-(26-9-2011).pdf

4-MUMNP-2008-CANCELLED PAGES(20-7-2011).pdf

4-MUMNP-2008-CLAIMS(AMENDED)-(20-7-2011).pdf

4-MUMNP-2008-CLAIMS(GRANTED)-(26-9-2011).pdf

4-MUMNP-2008-CLAIMS(MARKED COPY)-(20-7-2011).pdf

4-mumnp-2008-correspondence(17-1-2008).pdf

4-MUMNP-2008-CORRESPONDENCE(IPO)-(27-9-2011).pdf

4-MUMNP-2008-DESCRIPTION(GRANTED)-(26-9-2011).pdf

4-MUMNP-2008-DRAWING(1-1-2008).pdf

4-MUMNP-2008-DRAWING(20-7-2011).pdf

4-MUMNP-2008-DRAWING(GRANTED)-(26-9-2011).pdf

4-mumnp-2008-form 1(17-1-2008).pdf

4-MUMNP-2008-FORM 18(14-1-2008).pdf

4-MUMNP-2008-FORM 2(GRANTED)-(26-9-2011).pdf

4-MUMNP-2008-FORM 2(TITLE PAGE)-(1-1-2008).pdf

4-MUMNP-2008-FORM 2(TITLE PAGE)-(GRANTED)-(26-9-2011).pdf

4-mumnp-2008-form 26(17-1-2008).pdf

4-mumnp-2008-form 3(17-1-2008).pdf

4-MUMNP-2008-FORM 3(20-7-2011).pdf

4-mumnp-2008-form 5(17-1-2008).pdf

4-MUMNP-2008-REPLY TO EXAMINATION REPORT(20-7-2011).pdf

4-mumnp-2008-wo international publication report(1-10-2008).pdf

abstract1.jpg


Patent Number 249038
Indian Patent Application Number 4/MUMNP/2008
PG Journal Number 39/2011
Publication Date 30-Sep-2011
Grant Date 26-Sep-2011
Date of Filing 01-Jan-2008
Name of Patentee GOROVOI YURY MIKHAILOVICH
Applicant Address UL. SENJUKOVA, 41-73, UKHTA, 169300, RESPUBLIKA KOMI, RUSSIA.
Inventors:
# Inventor's Name Inventor's Address
1 KLYAMKO, ANDREI STANISLAVOVICH UL. MICHURINSKAYA, 1-191, ST. PETERSBURG 197046
2 PRANOVICH, ALEXANDR ALEXANDROVICH UL. DZERZHINSKOGA, 29-195, UKHTA, 169300, RESPUBLIKA KOMI
3 VLASENKO, VIKTOR IVANOVICH UL. NABEREZHNAYA NEFTYANIKOV, 15-7, UKHTA, 169300, RESPUBLIKA KOMI
4 KORZHAKOV VALDIMIR VIKTOROVICH UL. PERVOMAISKAYA, 7-26, UKHTA 169300 RESPUBLIKA KOMI
5 GOROVOI YURY MIKHAILOVICH UL. SENJUKOVA, 41-73, UKHTA, 169300, RESPUBLIKA KOMI, RUSSIA.
PCT International Classification Number C01G23/047
PCT International Application Number PCT/RU2006/000185
PCT International Filing date 2006-04-13
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 2005118054 2005-06-14 Russia
2 2005118051 2005-06-14 Russia