CN106422988B - Reaction device with secondary reactor - Google Patents

Abstract

A reaction device with a secondary reactor comprises a first reactor, a first dust remover, a second reactor and a second dust remover which are connected in sequence; the first reactor comprises a first material bin pipe, a preheating pipe and a reaction pipe; the bottom of the first bin pipe is provided with a horn-shaped expansion pipe, and the expansion pipe is gradually narrowed inwards from an opening at the upper end of the expansion pipe to an opening at the lower end of the expansion pipe; the upper end of the preheating pipe is connected with the opening at the lower end of the dilatation pipe, and the lower end of the preheating pipe is communicated with the reaction pipe; the two ends of the reaction tube are provided with first air inlets; the second reactor comprises a second material bin pipe, a gas collecting pipe, a heating sleeve and a third exhaust pipe; the gas collecting pipe is arranged at the bottom of the second material bin pipe; the top of the gas collecting tube is provided with an opening and is communicated with the inside of the second material bin tube; a sieve plate is arranged at the top opening of the gas collecting tube; the heating sleeve penetrates through the second bin pipe; a heating pipe is arranged in the heating sleeve. The reaction device has high reaction efficiency, high product purity and good dust removal effect.

Description

Reaction device with secondary reactor

Technical Field

The invention relates to the field of reaction equipment, in particular to a reaction device with a secondary reactor.

Background

Carbon tetrafluoride is an important plasma etching gas in the microelectronics industry at present, and is widely used for etching thin film materials such as silicon, silicon dioxide, silicon nitride, phosphosilicate glass, tungsten and the like, and has a great deal of application in the aspects of surface cleaning of electronic devices, production of solar cells, laser technology, low-temperature refrigeration, gas insulation, leakage detection agents, detergents, lubricants, brake fluid and the like in the production of printed circuits. Many methods for synthesizing carbon tetrafluoride include the direct contact reaction of carbon tetrafluoride with fluorine gas, chlorofluorocarbon with hydrogen fluoride in the presence of a catalyst, and fluorine gas with a carbon source to produce carbon tetrafluoride, and the like. The prior mature technology adopts carbon hydrofluoride and chlorofluoride as carbon sources to prepare carbon tetrafluoride, the raw materials are expensive and easy to explode, and the synthesized product contains impurities which are not easy to remove; the fluorocarbon is prepared by a fluorocarbon direct contact reaction method, and the method can be used for preparing the fluorocarbon through continuous development and perfection.

However, the existing reactor has low reaction efficiency, low reactant utilization rate and poor dust removal effect, and is unfavorable for the preparation of carbon tetrafluoride.

Disclosure of Invention

The invention aims to provide a reaction device with a secondary reactor, which can overcome the defects in the prior art, and has the advantages of high reaction efficiency, high product purity and good dust removal effect.

To achieve the purpose, the invention adopts the following technical scheme:

a reaction device with a secondary reactor comprises a first reactor, a first dust remover, a second reactor and a second dust remover which are connected in sequence;

the first reactor comprises a first material bin pipe, a preheating pipe and a reaction pipe;

the bottom of the first bin pipe is provided with a horn-shaped expansion pipe, and the expansion pipe gradually narrows inwards from an opening at the upper end of the expansion pipe to an opening at the lower end of the expansion pipe;

the first bin pipe, the dilatation pipe and the preheating pipe are all arranged vertically, and the reaction pipe is arranged transversely;

the upper end of the preheating pipe is connected with the opening at the lower end of the dilatation pipe, and the lower end of the preheating pipe is communicated with the reaction pipe;

the two ends of the reaction tube are provided with first air inlets;

the first bin pipe is provided with a first exhaust pipe which is connected with the first dust remover;

the second reactor comprises a second material bin pipe, a gas collecting pipe, a heating sleeve and a third exhaust pipe;

the gas collecting pipe is arranged at the bottom of the second material bin pipe;

the top of the gas collecting tube is provided with an opening and is communicated with the inside of the second material bin tube;

a sieve plate is arranged at the top opening of the gas collecting tube;

the gas collecting tube is provided with a third gas inlet tube which is connected with the first dust remover;

the third exhaust pipe is connected to the second dust remover;

the heating sleeve is hollow and transversely penetrates through the second bin pipe;

and a heating pipe is arranged in the heating sleeve.

Further, a first feeding pipe and a blow-down pipe are arranged at the top of the first bin pipe;

one end of the first feeding pipe and one end of the blow-down pipe are respectively communicated with the top of the first material bin pipe;

the other end of the first feeding pipe and two ends of the reaction pipe are both provided with a flange and a flange cover, and the flange cover is installed on the flange.

Further, the first reactor further comprises a cooling tank;

the reaction tube is arranged in the cooling box, and two ends of the reaction tube protrude out of the cooling box.

Further, the cooling box is a rectangular box body, and an opening is formed in the top of the cooling box;

at least one water inlet pipe is arranged on the outer wall of the bottom of one side wall of the cooling box;

the outer wall of the top proximal end of one side wall of the cooling box is provided with at least one overflow pipe;

the reaction tube is provided with at least one thermometer sleeve;

the lower end of the thermometer sleeve is closed and positioned in the reaction tube;

a temperature detector is arranged in the thermo-well tube.

Further, the first dust remover comprises a dust removing pipe and a partition plate;

the partition board comprises an upper partition board and a lower partition board, and the number of the upper partition board and the number of the lower partition board are at least one;

the upper partition plate and the lower partition plate are welded in the dust removing pipe at equal intervals;

the upper partition plate and the lower partition plate which are adjacent to each other form a dust removing air passage;

the outer wall of the dust removal pipe is provided with a second air inlet pipe and a second air outlet pipe which are communicated with the inside of the dust removal pipe, and the first air outlet pipe is connected with the second air inlet pipe.

Further, both ends of the dust removal pipe are provided with flange covers and flanges, and the flange covers are arranged on the flanges so as to seal the dust removal pipe;

the top of the upper partition plate is attached to the lower surface of the flange cover at the top end of the dust removal pipe, and the bottom of the lower partition plate is attached to the upper surface of the flange cover at the bottom end of the dust removal pipe;

the first dust remover also comprises a baffle;

the baffle is fixed on the flange cover and is respectively positioned at two sides of the welding part of the upper baffle plate or the lower baffle plate;

the bottom end of the dust removing pipe is provided with a horn-shaped sealing pipe;

the flange cover at the bottom end of the dust removal pipe is provided with a first blow-down pipe communicated with the inside of the dust removal pipe, and the first blow-down pipe is provided with a valve.

Further, a second feeding pipe is arranged at the top of the second material bin pipe, one end of the second feeding pipe is communicated with the inside of the second material bin pipe, a flange and a flange cover are arranged at the other end of the second feeding pipe, and the flange cover is arranged on the flange;

the third exhaust pipe is arranged on the outer wall of the second feeding pipe;

the second reactor also comprises a temperature detector which is arranged on the second material bin pipe.

Further, the second dust remover comprises a dust collecting pipe, a second blow-off pipe and a fourth air inlet pipe;

the fourth air inlet pipe is communicated with the third air outlet pipe;

the bottom of the fourth air inlet pipe is positioned in the dust collecting pipe, and the top of the fourth air inlet pipe penetrates through the top of the dust collecting pipe;

the bottom of the fourth air inlet pipe is provided with a gas distributor, and a gas spoiler is arranged above the gas distributor;

the second blow-down pipe is arranged at the bottom of the dust collecting pipe;

the dust collecting pipe is provided with a fourth exhaust pipe which is positioned above the gas spoiler.

Further, the gas distributor is horn-shaped;

the gas distributor gradually expands outwards from an opening at the upper end of the gas distributor to an opening at the lower end of the gas distributor;

the gas distributor is fixed at the bottom of the fourth gas inlet pipe at the opening of the upper end of the gas distributor; and the gas distributor is provided with full air holes.

Further, the gas spoiler is horn-shaped;

the gas spoiler gradually narrows inwards from an opening at the upper end of the gas spoiler to an opening at the lower end of the gas spoiler, and the edge of the opening at the upper end of the gas spoiler is fixed on the inner wall of the dust collecting pipe;

the second blow-down pipe is inclined outwards;

an angle A formed by the top of one side of the second blow-down pipe and the bottom plane of the dust collecting pipe is an obtuse angle;

an angle B formed by the top of the other side of the second blow-down pipe and the bottom plane of the dust collecting pipe is an acute angle;

a drain outlet is arranged at the bottom of the second drain pipe;

the fourth exhaust pipe is arranged on the outer wall of the dust collecting pipe close to the top;

a semicircular baffle plate is arranged in the dust collecting pipe, is positioned on the side, close to the fourth exhaust pipe, of the fourth air inlet pipe, and is positioned below the fourth exhaust pipe;

the semicircular baffle is arranged in a downward inclined mode.

According to the invention, the reaction device with the secondary reactor is provided, and has high reaction efficiency and good dust removal effect.

The first reactor is used for generating carbon tetrafluoride by reacting fluorine gas with carbon, the carbon is placed in the first material bin pipe, the preheating pipe and the reaction pipe, and the first air inlets are arranged at two ends of the reaction pipe, so that on one hand, the amount of fluorine gas introduced into the reaction pipe in unit time can be increased, more fluorine gas is fully contacted with carbon, and the reaction efficiency is increased; the fluorine gas and the carbon generate chemical reaction to emit heat, and as the lower end of the preheating pipe is communicated with the reaction pipe, a large amount of heat can be transferred from carbon tetrafluoride serving as a reaction product to the carbon in the preheating pipe, the carbon is preheated, the reaction temperature is kept stable, and the reaction efficiency of the subsequent carbon and the fluorine gas is higher.

As the reaction proceeds, the carbon in the reaction tube is gradually consumed, and as the first bin tube, the capacity expansion tube and the preheating tube are vertically arranged, the carbon in the preheating tube can fall to the reaction tube under the action of gravity so as to ensure the continuous proceeding of the reaction, and improve the stability and the persistence of the work of the reaction tube; likewise, the carbon in the first bin tube may drop into the preheating tube to ensure that the carbon to be reacted is preheated, ready for subsequent reactions.

The horn-shaped expansion pipe has the effect of expanding the volume of the first bin pipe, and the expansion pipe gradually narrows inwards from the opening at the upper end of the expansion pipe to the opening at the lower end of the expansion pipe, so that the cross-sectional area of the first bin pipe connected with the opening at the upper end of the expansion pipe is larger than that of the preheating pipe connected with the opening at the lower end of the expansion pipe, and the volume of the first bin pipe is greatly increased under the condition that the first bin pipe and the preheating pipe are in the same length, thereby reducing the adding times of carbon and improving the working persistence of the first reactor.

When fluorine gas and carbon react, carbon tetrafluoride gas is generated, however, the utilization rate of the fluorine gas cannot reach one hundred percent, incompletely reacted carbon powder is mixed, the mixed gas mainly contains carbon tetrafluoride, carbon powder and fluorine gas, the mixed gas is discharged from the first exhaust pipe to the first dust remover for dust removal treatment, after primary dust removal, the carbon powder content in the mixed gas is reduced, the purity of the carbon tetrafluoride gas is improved, the mixed gas after primary dust removal enters the gas collecting pipe through the third gas inlet pipe, and the sieve plate is used for enabling the carbon powder in the mixed gas to fall into the gas collecting pipe so as to prevent blockage; fluorine gas and carbon tetrafluoride gas enter the second bin pipe through the sieve plate, and the gas collecting pipe is arranged at the bottom of the second bin pipe, so that the carbon powder can be cleaned more conveniently and rapidly.

Because the heating sleeve is hollow, the heating pipe is conveniently placed into the heating sleeve; since the heating sleeve has a plurality of heating sleeves which transversely penetrate through the second bin pipe, more carbon can be effectively loaded in the second bin pipe; heating the heating pipe to raise the temperature of the carbon supported by the heating sleeve, and when the fluorine gas and the carbon with raised temperature are in contact for reaction, the reaction efficiency is higher, carbon tetrafluoride gas can be generated more quickly, and then the carbon tetrafluoride gas is discharged from the third exhaust pipe to the second dust remover for secondary dust removal, so that the utilization rate of the fluorine gas reaches hundred percent, the content of carbon powder is reduced to the minimum, and the purity of the carbon tetrafluoride gas is greatly improved.

Drawings

FIG. 1 is a partial cross-sectional view of the front face of a first reactor according to one embodiment of the present invention.

FIG. 2 is a partial cross-sectional view of a side of a first reactor according to one embodiment of the invention.

Fig. 3 is a partial cross-sectional view of the front face of a first dust collector in accordance with one embodiment of the invention.

Fig. 4 is a partial enlarged view at C of fig. 3.

FIG. 5 is a schematic diagram of the front structure of a second reactor according to one embodiment of the present invention.

Fig. 6 is a schematic cross-sectional view of a header according to one embodiment of the present invention.

Fig. 7 is a perspective view of a second dust collector according to one embodiment of the present invention.

Wherein: the first reactor 2, the first bin pipe 21, the expansion pipe 211, the first exhaust pipe 212, the first charging pipe 213, the blow-down pipe 214, the support base 215, the preheating pipe 22, the reaction pipe 23, the first air inlet 231, the thermo-well pipe 232, the flange 261, the flange cover 262, the cooling tank 24, the water inlet pipe 241, the overflow pipe 242, the first dust collector 25, the dust collection pipe 251, the sealing pipe 2511, the partition 252, the upper partition 2521, the lower partition 2522, the dust collection air passage 253, the second air inlet 254, the second exhaust pipe 255, the baffle 256, the first blow-down pipe 257, the second reactor 3, the second bin pipe 31, the third exhaust pipe 311, the second charging pipe 312, the second support leg 313, the gas collection pipe 32, the screen 321, the third air inlet 322, the support column 323, the heating jacket 33, the temperature detector 34, the second dust collector 35, the dust collection pipe 351, the fourth exhaust pipe 3511, the semicircular baffle 3512, the second blow-down pipe 352, the first support leg 3522, the fourth air inlet 353, the gas distributor 354, the gas distribution plate 355, the gas flow-distribution plate 355, and the turbulent flow plate 355.

Detailed Description

The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings.

As shown in fig. 1 to 7, a reaction apparatus having a secondary reactor includes a first reactor 2, a first dust remover 25, a second reactor 3, and a second dust remover 35, which are sequentially connected;

the first reactor 2 comprises a first bin pipe 21, a preheating pipe 22 and a reaction pipe 23;

the bottom of the first bin pipe 21 is provided with a trumpet-shaped expansion pipe 211, and the expansion pipe 211 gradually narrows inwards from an opening at the upper end of the expansion pipe to an opening at the lower end of the expansion pipe 211;

the first bin pipe 21, the expansion pipe 211 and the preheating pipe 22 are all arranged vertically, and the reaction pipe 23 is arranged horizontally;

the upper end of the preheating pipe 22 is connected with the opening of the lower end of the capacity expansion pipe 211, and the lower end of the preheating pipe 22 is communicated with the reaction pipe 23;

the two ends of the reaction tube 23 are provided with first air inlets 231;

the first bin pipe 21 is provided with a first exhaust pipe 212 connected to the first dust collector 25;

the second reactor 3 comprises a second bin pipe 31, a gas collecting pipe 32, a heating sleeve 33 and a third exhaust pipe 311;

the gas collecting pipe 32 is arranged at the bottom of the second material bin pipe 31;

the top of the gas collecting tube 32 is provided with an opening and is communicated with the inside of the second material bin tube 31;

a sieve plate 321 is arranged at the top opening of the gas collecting tube 32;

the gas collecting pipe 32 is provided with a third gas inlet pipe 322 which is connected to the first dust collector 25;

the third exhaust pipe 311 is connected to the second dust collector 35;

the heating sleeve 33 has a plurality of hollow parts which transversely penetrate through the second material chamber tube 31;

a heating pipe is arranged in the heating sleeve 33.

The first reactor 2 of this embodiment is configured to react fluorine gas with carbon to generate carbon tetrafluoride, the carbon is placed in the first bin tube 21, the preheating tube 22 and the reaction tube 23, and the first air inlet 231 is disposed at two ends of the reaction tube 23, so that on one hand, the amount of fluorine gas introduced into the reaction tube 23 in unit time can be increased, more fluorine gas is fully contacted with carbon, and the reaction efficiency is increased; the fluorine gas and the carbon generate heat during chemical reaction, and as the lower end of the preheating pipe 22 is communicated with the reaction pipe 23, a large amount of heat is transferred from the carbon tetrafluoride as a reaction product to the carbon in the preheating pipe 22, the carbon is preheated, the reaction temperature is kept stable, and the reaction efficiency of the subsequent carbon and fluorine gas is higher.

As the reaction proceeds, the carbon in the reaction tube 23 is gradually consumed, and as the first bin tube 21, the expansion tube 211 and the preheating tube 22 are all vertically arranged, the carbon in the preheating tube 22 will drop to the reaction tube 23 under the action of gravity to ensure the continuous progress of the reaction, and improve the stability and the persistence of the operation thereof; likewise, the carbon in the first hopper tube 21 will drop into the preheating tube 22 to ensure that the carbon to be reacted is preheated and ready for subsequent reactions.

The flared expansion pipe 211 has the function of expanding the volume of the first bin pipe 21, and since the expansion pipe 211 gradually narrows inwardly from the opening at the upper end to the opening at the lower end, the cross-sectional area of the first bin pipe 21 connected to the opening at the upper end of the expansion pipe 211 is larger than the cross-sectional area of the preheating pipe 22 connected to the opening at the lower end of the expansion pipe 211, and the volume of the first bin pipe 21 is greatly increased under the condition that the first bin pipe 21 and the preheating pipe 22 are in the same length, so that the addition times of carbon are reduced, and the operation duration of the first reactor 2 is improved.

The fluorine gas and the carbon react to generate carbon tetrafluoride gas, however, the utilization rate of the fluorine gas cannot reach hundred percent, and the incompletely reacted carbon powder is mixed, the reacted gas becomes a mixed gas mainly containing carbon tetrafluoride, hexafluoroethane, octafluoropropane, carbon monoxide, carbon dioxide, carbon powder, fluorine gas and hydrogen fluoride, the mixed gas is discharged from the first exhaust pipe 212 to the first dust remover 25 for dust removal treatment, after primary dust removal, the carbon powder content in the mixed gas is reduced, the purity of the carbon tetrafluoride gas is improved, and the mixed gas after primary dust removal enters the gas collecting pipe 32 through the third gas inlet pipe 322, and the fluorine gas and the carbon tetrafluoride gas enter the second material bin pipe 31 through the sieve 321, and because the gas collecting pipe 32 is arranged at the bottom of the second material bin pipe 31, the carbon powder can be cleaned more conveniently and quickly.

Since the heating sleeve 33 is hollow, it is convenient for the heating pipe to be put into the inside of the heating sleeve 33; since the heating sleeve 33 has a plurality of heating sleeves which transversely penetrate the second hopper tube 31, more carbon can be effectively carried in the second hopper tube 31; the heating pipe heats up the carbon supported by the heating sleeve 33, when the fluorine gas contacts the carbon reaching the temperature for reaction, the reaction efficiency is higher, carbon tetrafluoride gas can be generated more quickly, then the carbon tetrafluoride gas is discharged from the third exhaust pipe 311 to the second dust collector 35 for secondary dust removal, finally the utilization rate of the fluorine gas reaches one hundred percent, the content of carbon powder is reduced to the minimum, the purity of the carbon tetrafluoride gas is greatly improved, and the occurrence of blocking of subsequent pipelines and equipment is reduced.

Further, a first feeding pipe 213 and a blow-down pipe 214 are arranged at the top of the first bin pipe 21;

one end of the first feeding pipe 213 and one end of the blow-down pipe 214 are respectively connected to the top of the first bin pipe 21;

the other end of the first feeding pipe 213 and the two ends of the reaction pipe 23 are respectively provided with a flange 261 and a flange cover 262, and the flange cover 262 is mounted on the flange 261.

After the carbon in the first reactor 2 is consumed by the reaction, the carbon is added from the first feeding tube 213 arranged at the top of the first bin tube 21, so that the operation is simpler, more convenient and more direct, and because one end of the first feeding tube 213 and one end of the blow-down tube 214 are respectively communicated with the top of the first bin tube 21, the carbon can fall to the first bin tube 21, the expansion tube 211, the preheating tube 22 and the reaction tube 23 under the action of gravity so as to ensure the continuous progress of the reaction; since the other end of the first feeding pipe 213 is provided with a flange 261 and a flange cover 262 at both ends of the reaction pipe 23, the flange cover 262 is mounted on the flange 261, the feeding operation of the first reactor 2 can be performed by only disassembling the flange cover 262 during the feeding.

The other end of the blow-down pipe 214 is connected to the exhaust gas treatment tower, and the gas can be blown down only by opening the blow-down valve during operation.

Further, the two ends of the reaction tube 23 are respectively provided with a flange 261 and a flange cover 262, and the flange cover 262 is mounted on the flange 261 to seal the reaction tube 23;

the first air inlet 231 is provided to the flange cover 262.

By mounting the flange 261 to the flange cover 262, the reaction tube 23 can be effectively sealed from gas leakage, such as leakage of reactant fluorine gas and leakage of product carbon tetrafluoride gas; by disassembling the flange cover 262, the waste residue left by the reaction in the reaction tube 23 can be quickly cleaned, and the operation is simple and convenient; the first gas inlet 231 is provided in the flange cover 262, so as to ensure that fluorine gas is effectively introduced into the reaction tube.

Further, the first exhaust pipe 212 is disposed laterally at a radial position at a top proximal end of the first bin pipe 21.

The first exhaust pipe 212 is transversely arranged on the outer wall of the top proximal end of the first bin pipe 21, so that the rising path of the mixed gas can be increased, the sedimentation of carbon powder under the action of gravity is facilitated, and the purity of the carbon tetrafluoride gas is improved.

Further, the first reactor 2 further comprises a cooling tank 24;

the reaction tube 23 is disposed in the cooling tank 24, and both ends of the reaction tube 23 protrude outside the cooling tank 24.

A large amount of heat is released when the fluorine gas reacts with the carbon, and the cooling water is contained in the cooling tank 24 to lower the temperature of the reaction tube 23, thereby increasing the service life thereof. The two ends of the reaction tube 23 protrude outside the cooling box 24, so that the flange covers 262 mounted at the two ends of the reaction tube are convenient to mount and dismount, and cooling water is prevented from entering the reaction tube 23.

Further, the cooling box 24 is a rectangular box body, and an opening is formed in the top of the cooling box;

at least one water inlet pipe 241 is arranged on the outer wall of the bottom of one side wall of the cooling box 24;

the outer wall of one of the side walls of the cooling box 24 at the top proximal end thereof is provided with at least one overflow pipe 242;

the reaction tube 23 is provided with at least one thermo-well tube 232;

the lower end of the thermo-well tube 232 is closed and located in the reaction tube 23;

a temperature detector 34 is provided in the thermo-well tube 232.

The rectangular box is easy to produce, more cooling water can be loaded, and the opening arranged at the top of the rectangular box plays a role in observing and checking the use condition of the first reactor 2. As shown in fig. 2, in this embodiment, the number of the water inlet pipes 241 is one, the number of the overflow pipes 242 is two, and the water inlet pipes 241 and the overflow pipes 242 are both arranged on the side wall of the cooling tank 24, so that the installation is more convenient; the outer wall of the bottom of one side wall of the cooling tank 24 is slower and more stable when cooling water enters the water inlet of the water inlet pipe 241 and is introduced into the cooling tank 24; the overflow pipe 242 is provided on the outer wall of the cooling tank 24 at the top proximal end of one of the side walls, so as to ensure that the cooling water in the cooling tank 24 is sufficient to effectively cool the reaction tube 23, thereby avoiding excessive overflow of the cooling water.

As shown in fig. 1, the number of the thermo-well tubes 232 in the present embodiment is two, and the thermo-well tubes 232 are symmetrically disposed on the reaction tubes 23 on both sides of the preheating tube 22, so that the accuracy of the temperature detection in the reaction tubes 23 by the temperature detector 34 can be improved, and the lower ends of the thermo-well tubes 232 are closed, so that the reaction tubes 23 can be sealed and the temperature detector 34 can be protected.

Further, as shown in fig. 3, the first dust collector 25 includes a dust collecting pipe 251 and a partition 252;

the partition 252 includes an upper partition 2521 and a lower partition 2522, and the number of the upper partition 2521 and the lower partition 2522 is at least one;

the upper partition 2521 and the lower partition 2522 are welded in the dust removing pipe 251 at equal intervals;

adjacent upper and lower baffles 2521 and 2522 form a dust removal air path 253;

the outer side of the dust removing pipe 251 is provided with a second air inlet pipe 254 and a second air outlet pipe 255 which are communicated with the inside of the dust removing pipe 251, and the first air outlet pipe 212 is connected with the second air inlet pipe 254.

When the mixed gas enters the dust removing air path 253 of the dust removing tube 251 through the second air inlet tube 254, carbon powder will settle to the bottom of the dust removing tube 251 under the barrier action and gravity action of the upper partition 2521 and the lower partition 2522, so as to facilitate the subsequent cleaning, thereby improving the purity of the carbon tetrafluoride gas, and finally the carbon tetrafluoride gas which is further purified is discharged from the second air outlet tube 255 to the third air inlet tube 322.

The number of the upper partition plates 2521 is two, and the number of the lower partition plates 2522 is one, so that the upper partition plates 2521 and the lower partition plates 2522 are more firmly disposed in the dust removing pipe 251 by welding.

Further, both ends of the dust removing pipe 251 are provided with a flange cover 262 and a flange 261, and the flange cover 262 is mounted on the flange 261 to seal the dust removing pipe 251;

the top of the upper partition 2521 is attached to the lower surface of the flange cover 262 at the top end of the dust removing tube 251, and the bottom of the lower partition 2522 is attached to the upper surface of the flange cover 262 at the bottom end of the dust removing tube 251;

the first dust collector 25 further includes a baffle 256;

the baffle 256 is fixed to the flange cover 262 and is located at both sides of the welding portion of the upper or lower partition 2521, 2522, respectively;

a horn-shaped sealing tube 2511 is arranged at the bottom end of the dust removing tube 251;

the flange cover 262 at the bottom end of the dust removing pipe 251 is provided with a first drain pipe 257 communicated with the inside of the dust removing pipe 251, and the first drain pipe 257 is provided with a valve.

As shown in fig. 3 and 4, the dust removal pipe 251 can be cleaned quickly by assembling and disassembling the flange cover 262, the top of the upper partition plate 2521 is attached to the lower surface of the flange cover 262 at the top end of the dust removal pipe 251, the bottom of the lower partition plate 2522 is attached to the upper surface of the flange cover 262 at the bottom end of the dust removal pipe 251, so that the mixed gas moves along the dust removal gas path 253 as much as possible, and the mixed gas does not directly pass through the attachment position of the flange cover 262 with the upper partition plate 2521 and the lower partition plate 2522, thereby improving the quality of carbon dust removal and the purity of carbon tetrafluoride gas.

The baffle 256 can prevent the mixed gas from directly passing through the joint between the flange cover 262 and the upper partition 2521 and the lower partition 2522, so as to further improve the quality of carbon powder removal and the purity of carbon tetrafluoride gas.

The flange cover 262 at the bottom end of the dust removing tube 251 is required to be removed periodically, but the larger the diameter of the bottom end of the dust removing tube 251 is, the more difficult it is to seal, so the sealing tube 2511 is configured as a trumpet-shaped tube gradually narrowed inwards from the opening at the upper end to the opening at the lower end thereof, and the sealing degree is improved.

The fluorine gas in this embodiment is produced by an electrolytic method, so that the fluorine gas is mixed with hydrogen fluoride gas, and becomes acid liquid after the temperature of the fluorine gas is reduced, and for the safety of cleaning carbon powder, the valve on the first drain pipe 257 is opened to remove the acid liquid, and then the flange cover 262 dust is removed.

Further, the first bin pipe 21 further includes at least two support seats 215;

the support seats 215 are disposed at equal intervals along the circumference of the outer wall of the first hopper tube 21.

The number of the supporting seats 215 in this embodiment is two, and the supporting seats are disposed at equal intervals along the circumference of the outer wall of the first bin pipe 21, so that the first bin pipe 21 can be better supported, and the stress when the first bin pipe 21 is supported is more uniform.

Further, a second feeding pipe 312 is arranged at the top of the second bin pipe 31, one end of the second feeding pipe 312 is communicated with the inside of the second bin pipe 31, a flange 261 and a flange cover 262 are arranged at the other end of the second feeding pipe, and the flange cover 262 is mounted on the flange 261;

the third exhaust pipe 311 is arranged outside the second feeding pipe 312;

as shown in fig. 5, the second reactor 3 further includes a temperature detector 34 provided in the second hopper tube 31.

After the carbon in the second reactor 3 is consumed by reaction, the carbon is added from the second feeding pipe 312 arranged at the top of the second material bin pipe 31, the operation is simpler, more convenient and direct, one end of the second feeding pipe 312 is communicated with the inside of the second material bin pipe 31, so that the carbon can fall into the second material bin pipe 31 under the action of gravity, and the feeding operation can be performed on the second reactor 3 only by disassembling the flange cover 262 during feeding.

The reaction efficiency of the carbon and the fluorine gas near the heating sleeve 33 is higher, and the temperature detector 34 can effectively detect the temperature of the second bin tube 31 close to the heating sleeve 33, so that the heating temperature of the heating tube can be better controlled, and the carbon and the fluorine gas can be ensured to be continuously at the optimal reaction temperature.

Further, as shown in fig. 5, a flange cover 262 and a flange 261 are provided at the bottom of the gas collecting tube 32;

the flange cover 262 is mounted to the flange 261 to seal the header 32.

By installing the flange cover 262, the gas collecting pipe 32 can be effectively sealed, and gas leakage is avoided; by removing the flange cover 262, dust left by the reaction in the gas collecting tube 32 can be quickly cleaned.

Further, as shown in fig. 6, a supporting column 323 is disposed in the gas collecting tube 32;

both ends of the support column 323 respectively support against the bottom of the screen plate 321 and the top of the flange cover 262.

The support column 323 has a supporting function on the screen plate 321, and can effectively support the screen plate 321, so that the stability of the operation of the screen plate 321 is ensured, and carbon powder can be stably filtered.

Further, the heating jacket 33 is provided at the proximal end of the bottom of the second magazine tube 31.

The heating jacket 33 can support as much carbon as possible, so that the number of subsequent carbon additions is reduced, and the fluorine gas can be brought into contact with more carbon to improve the reaction efficiency.

The second reactor 3 further comprises a temperature detector 34, which is arranged in the second cartridge tube 31 and is close to the heating jacket 33.

The reaction efficiency of the carbon and the fluorine gas near the heating sleeve 33 is higher, and the temperature detector 34 can effectively detect the reaction temperature of the second bin tube 31, so that the heating temperature of the heating tube can be better controlled to ensure that the carbon and the fluorine gas are continuously at the optimal reaction temperature.

Further, the second dust collector 35 includes a dust collecting pipe 351, a second drain pipe 352, and a fourth air inlet pipe 353;

the fourth intake pipe 353 is connected to the third exhaust pipe 311;

the fourth air inlet pipe 353 is vertically arranged, the bottom of the fourth air inlet pipe is positioned in the dust collecting pipe 351, and the top of the fourth air inlet pipe penetrates through the top of the dust collecting pipe 351;

a gas distributor 354 is arranged at the bottom of the fourth air inlet pipe 353, and a gas spoiler 355 is arranged above the gas distributor 354;

the second blow-down pipe 352 is arranged at the bottom of the dust collecting pipe 351;

the dust collecting pipe 351 is provided with a fourth exhaust pipe 3511 which is located above the gas spoiler 355.

Carbon powder with insufficient reaction can be mixed in the carbon tetrafluoride gas generated by the reaction of carbon and fluorine gas in the second bin tube 31, when the carbon tetrafluoride gas mixed with carbon powder enters the fourth air inlet tube 353 through the third air outlet tube 311 and then is discharged from the bottom of the fourth air inlet tube 353, the fourth air inlet tube 353 is vertically arranged, so that the installation is more convenient, and the top of the fourth air inlet tube 353 penetrates through the top of the dust collecting tube 351, so that the connection of the fourth air inlet tube 353 and the third air outlet tube 311 is more convenient.

The gas distributor 354 can uniformly distribute the carbon tetrafluoride gas mixed with carbon powder, under the action of the gas spoiler 355, the carbon tetrafluoride gas mixed with carbon powder can stay in the dust collecting pipe 351 for a longer time, so that the carbon powder is more beneficial to settling in the second sewage draining pipe 352, and the fourth exhaust pipe 3511 is positioned above the gas spoiler 355, so that the purity of the carbon tetrafluoride gas finally discharged from the gas spoiler is higher, and less carbon powder is mixed.

Further, the gas distributor 354 is horn-shaped;

the gas distributor 354 gradually expands outwardly from an opening at an upper end thereof to an opening at a lower end thereof;

the gas distributor 354 is fixed to the bottom of the fourth gas inlet pipe 353 at an upper end opening thereof; the gas distributor 354 is provided with gas holes 3541.

Because the upper end opening of the gas distributor 354 is smaller, the gas distributor 354 can be matched and fixed with the fourth air inlet pipe 353 with smaller aperture, and the horn-shaped gas distributor 354 gradually expands outwards from the opening at the upper end to the opening at the lower end, so that the mixed gas is distributed more uniformly, and the sedimentation of carbon powder is facilitated. The air holes 3541 further make the distribution of the mixed gas more uniform, and are more beneficial to the sedimentation of carbon powder.

Further, the gas spoiler 355 has a horn shape;

the gas spoiler 355 is gradually narrowed inwards from the opening at the upper end to the opening at the lower end, and the edge of the opening at the upper end is fixed on the inner wall of the dust collecting tube 351;

the second drain pipe 352 is inclined outward;

an angle A formed by the top of one side of the second blow-down pipe 352 and the bottom plane of the dust collecting pipe 351 is an obtuse angle;

an angle B formed by the top of the other side of the second blow-down pipe 352 and the bottom plane of the dust collecting pipe 351 is an acute angle;

a drain outlet 3521 is arranged at the bottom of the second drain pipe 352;

the fourth exhaust pipe 3511 is arranged on the outer wall of the dust collecting pipe 351 close to the top;

a semicircular baffle plate 3512 is disposed in the dust collecting pipe 351, and is located on a side of the fourth air inlet pipe 353, which is close to the fourth air outlet pipe 3511, and below the fourth air outlet pipe 3511;

the semicircular baffle 3512 is arranged in a downward inclined manner.

The edge of the opening at the upper end of the gas spoiler 355 is fixed on the inner wall of the dust collecting pipe 351, so that carbon tetrafluoride gas mixed with carbon powder can be effectively blocked by the gas spoiler 355 towards the outer wall of the bottom of the dust collecting pipe 351, so that the mixed gas stays in the dust collecting pipe 351 for more time, and the sedimentation of the carbon powder is facilitated; the gas spoiler 355 gradually narrows from the opening at the upper end to the opening at the lower end, and even if carbon powder is settled from above the gas spoiler 355, the carbon powder will not be accumulated on the gas spoiler 355, and will fall down to the opening at the lower end along the opening at the upper end of the gas spoiler 355, and finally falls into the second drain pipe 352.

As shown in fig. 7, in this embodiment, the angle a is 120 ° and the angle B is 30 °, so that the carbon powder in the second drain 352 can be cleaned more conveniently and safely, the drain 3521 of this embodiment is provided with a flange cover 262 and a flange 261, and the carbon powder is finally discharged from the drain 3521 by detaching the flange cover 262.

The fourth exhaust pipe 3511 is arranged on the outer wall of the dust collecting pipe 351 close to the top, so that the mixed gas stays in the dust collecting pipe 351 for more time, and the sedimentation of carbon powder is facilitated; the semicircular baffle 3512 is arranged in the dust collecting pipe 351 and can prevent the mixed gas from rising, the mixed gas is driven to be far away from the outlet of the fourth exhaust pipe 3511, further the mixed gas is enabled to stay in the dust collecting pipe 351 for more time, sedimentation of carbon powder is facilitated, the semicircular baffle 3512 is arranged in a downward inclined mode, carbon powder is not easy to accumulate on the semicircular baffle 3512, and the mixed gas falls down in a following mode.

The outer wall of the second drain pipe 352 is vertically provided with three first supporting legs 3522, which can support the second drain pipe 352, so that the installation is convenient. The outer wall of the second bin pipe 31 is at least vertically provided with three second supporting legs 313, which can support the second bin pipe 31, so that the installation is convenient.

The technical principle of the present invention is described above in connection with the specific embodiments. The description is made for the purpose of illustrating the general principles of the invention and should not be taken in any way as limiting the scope of the invention. Other embodiments of the invention will be apparent to those skilled in the art from consideration of this specification without undue burden.

Claims (7)

1. A reaction device with a secondary reactor comprises a first reactor, a first dust remover, a second reactor and a second dust remover which are connected in sequence;

the method is characterized in that: the first reactor comprises a first material bin pipe, a preheating pipe and a reaction pipe;

the bottom of the first bin pipe is provided with a horn-shaped expansion pipe, and the expansion pipe gradually narrows inwards from an opening at the upper end of the expansion pipe to an opening at the lower end of the expansion pipe;

the first bin pipe, the dilatation pipe and the preheating pipe are all arranged vertically, and the reaction pipe is arranged transversely;

the upper end of the preheating pipe is connected with the opening at the lower end of the dilatation pipe, and the lower end of the preheating pipe is communicated with the reaction pipe;

the two ends of the reaction tube are provided with first air inlets;

the first bin pipe is provided with a first exhaust pipe which is connected with the first dust remover;

the first reactor further comprises a cooling tank;

the reaction tube is arranged in the cooling box, and two ends of the reaction tube protrude out of the cooling box;

the first dust remover comprises a dust removing pipe and a partition plate;

the partition board comprises an upper partition board and a lower partition board, and the number of the upper partition board and the number of the lower partition board are at least one;

the upper partition plate and the lower partition plate are welded in the dust removing pipe at equal intervals;

the upper partition plate and the lower partition plate which are adjacent to each other form a dust removing air passage;

the outer wall of the dust removal pipe is provided with a second air inlet pipe and a second air outlet pipe which are communicated with the inside of the dust removal pipe, and the first air outlet pipe is connected with the second air inlet pipe;

the second reactor comprises a second material bin pipe, a gas collecting pipe, a heating sleeve and a third exhaust pipe;

the gas collecting pipe is arranged at the bottom of the second material bin pipe;

the top of the gas collecting tube is provided with an opening and is communicated with the inside of the second material bin tube;

a sieve plate is arranged at the top opening of the gas collecting tube;

the gas collecting tube is provided with a third gas inlet tube which is connected with the first dust remover;

the third exhaust pipe is connected to the second dust remover;

the heating sleeve is hollow and transversely penetrates through the second bin pipe;

a heating pipe is arranged in the heating sleeve;

the cooling box is a rectangular box body, and an opening is formed in the top of the cooling box;

at least one water inlet pipe is arranged on the outer wall of the bottom of one side wall of the cooling box;

the outer wall of the top proximal end of one side wall of the cooling box is provided with at least one overflow pipe;

the reaction tube is provided with at least one thermometer sleeve;

the lower end of the thermometer sleeve is closed and positioned in the reaction tube;

a temperature detector is arranged in the thermo-well tube.

2. A reaction apparatus having a secondary reactor according to claim 1, wherein: a first feeding pipe and a blow-down pipe are arranged at the top of the first bin pipe;

one end of the first feeding pipe and one end of the blow-down pipe are respectively communicated with the top of the first material bin pipe;

the other end of the first feeding pipe and two ends of the reaction pipe are both provided with a flange and a flange cover, and the flange cover is installed on the flange.

3. A reaction apparatus having a secondary reactor according to claim 1, wherein: the two ends of the dust removal pipe are respectively provided with a flange cover and a flange, and the flange covers are arranged on the flanges so as to seal the dust removal pipe;

the top of the upper partition plate is attached to the lower surface of the flange cover at the top end of the dust removal pipe, and the bottom of the lower partition plate is attached to the upper surface of the flange cover at the bottom end of the dust removal pipe;

the first dust remover also comprises a baffle;

the baffle is fixed on the flange cover and is respectively positioned at two sides of the welding part of the upper baffle plate or the lower baffle plate;

the bottom end of the dust removing pipe is provided with a horn-shaped sealing pipe;

the flange cover at the bottom end of the dust removal pipe is provided with a first blow-down pipe communicated with the inside of the dust removal pipe, and the first blow-down pipe is provided with a valve.

4. A reaction apparatus having a secondary reactor according to claim 1, wherein: the top of the second bin pipe is provided with a second feeding pipe, one end of the second feeding pipe is communicated with the inside of the second bin pipe, the other end of the second feeding pipe is provided with a flange and a flange cover, and the flange cover is arranged on the flange;

the third exhaust pipe is arranged on the outer wall of the second feeding pipe;

the second reactor also comprises a temperature detector which is arranged on the second material bin pipe.

5. A reaction apparatus having a secondary reactor according to claim 1, wherein: the second dust remover comprises a dust collecting pipe, a second blow-down pipe and a fourth air inlet pipe;

the fourth air inlet pipe is communicated with the third air outlet pipe;

the bottom of the fourth air inlet pipe is positioned in the dust collecting pipe, and the top of the fourth air inlet pipe penetrates through the top of the dust collecting pipe;

the bottom of the fourth air inlet pipe is provided with a gas distributor, and a gas spoiler is arranged above the gas distributor;

the second blow-down pipe is arranged at the bottom of the dust collecting pipe;

the dust collecting pipe is provided with a fourth exhaust pipe which is positioned above the gas spoiler.

6. A reaction apparatus having a secondary reactor as claimed in claim 5, wherein: the gas distributor is horn-shaped;

the gas distributor gradually expands outwards from an opening at the upper end of the gas distributor to an opening at the lower end of the gas distributor;

the gas distributor is fixed at the bottom of the fourth gas inlet pipe at the opening of the upper end of the gas distributor; and the gas distributor is provided with full air holes.

7. A reaction apparatus having a secondary reactor as claimed in claim 5, wherein: the gas spoiler is in a horn shape;

the gas spoiler gradually narrows inwards from an opening at the upper end of the gas spoiler to an opening at the lower end of the gas spoiler, and the edge of the opening at the upper end of the gas spoiler is fixed on the inner wall of the dust collecting pipe;

the second blow-down pipe is inclined outwards;

an angle A formed by the top of one side of the second blow-down pipe and the bottom plane of the dust collecting pipe is an obtuse angle;

an angle B formed by the top of the other side of the second blow-down pipe and the bottom plane of the dust collecting pipe is an acute angle;

a drain outlet is arranged at the bottom of the second drain pipe;

the fourth exhaust pipe is arranged on the outer wall of the dust collecting pipe close to the top;

a semicircular baffle plate is arranged in the dust collecting pipe, is positioned on the side, close to the fourth exhaust pipe, of the fourth air inlet pipe, and is positioned below the fourth exhaust pipe;

the semicircular baffle is arranged in a downward inclined mode.