CN106397107A - Purification system for carbon tetrafluoride - Google Patents
Purification system for carbon tetrafluoride Download PDFInfo
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- CN106397107A CN106397107A CN201610953559.5A CN201610953559A CN106397107A CN 106397107 A CN106397107 A CN 106397107A CN 201610953559 A CN201610953559 A CN 201610953559A CN 106397107 A CN106397107 A CN 106397107A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/007—Preparation of halogenated hydrocarbons from carbon or from carbides and halogens
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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Abstract
A purification system for carbon tetrafluoride comprises a fluorine source, a reaction device, a water scrubber, an alkaline tower and a rectifying tower, wherein the reaction device comprises a second dust remover; the second dust remover comprises a dust collecting pipe, a second blow-off pipe and a fourth gas inlet pipe; the fourth gas inlet pipe is arranged vertically; the bottom of the fourth gas inlet pipe is positioned in the dust collecting pipe; the top of the fourth gas inlet pipe penetrates through the top of the dust collecting pipe; a gas distributor is arranged at the bottom of the fourth gas inlet pipe; a gas interceptor is positioned above the gas distributor; the second blow-off pipe is arranged at the bottom of the dust collecting tube; and the fluorine source, the reaction device, the water scrubber, the alkaline tower and the rectifying tower are successively connected. According to the content, the purification system for the carbon tetrafluoride is provided, and is perfect in purification effect and good in dust removal effect.
Description
Technical field
The present invention relates to purification for gas field, more particularly, to a kind of purification system of carbon tetrafluoride.
Background technology
Carbon tetrafluoride is important plasma etching gas in current microelectronics industry, be widely used in silicon, silicon dioxide,
The etching of the thin-film materials such as silicon nitride, phosphorosilicate glass and tungsten, in electronic device surface clean, the production of solaode, laser
Technology, cryogenic refrigeration, gas-insulated, leak detectants, printed circuit produce in detergent, the aspect such as lubricant and brake fluid
Also there is extensive application.Carbon tetrafluoride synthetic method is a lot, include hydrofluorocarbons and fluorine gas, cfc in the presence of a catalyst with
Fluohydric acid gas and fluorine gas prepare carbon tetrafluoride etc. with carbon source directly contact reaction.Wherein, current maturation process adopt hydrofluorocarbons,
Cfc does carbon source and prepares carbon tetrafluoride, and the prices of raw materials are expensive, easily explode, and has in synthetic product and be difficult removal
Impurity；Fluorine carbon directly contact reaction method prepares carbon tetrafluoride, and the method, through continuous development and perfection, can prepare four
Perfluorocarbon.
But, the purification effect of existing carbon tetrafluoride purification system is not high, and dust removing effects are unsatisfactory, are unfavorable for tetrafluoro
Change the preparation of carbon.
Content of the invention
It is an object of the invention to proposing a kind of purification system of carbon tetrafluoride, good dedusting effect, the purification of carbon tetrafluoride
Effect is preferable.
For reaching this purpose, the present invention employs the following technical solutions：
A kind of purification system of carbon tetrafluoride, including fluorine source gas, reaction unit, water scrubber, caustic wash tower and rectifying column；
Described reaction unit includes the second cleaner unit；
Described second cleaner unit includes dust leg, the second blow-off pipe and the 4th air inlet pipe；
Described 4th air inlet pipe is vertically arranged, and its bottom is located in described dust leg, and its top is through described dust leg
Top；
The bottom of described 4th air inlet pipe is provided with gas distributor, is provided with gas positioned at the top of described gas distributor and disturbs
Stream plate；
Described second blow-off pipe is located at the bottom of described dust leg；
Described fluorine source gas, reaction unit, water scrubber, caustic wash tower and rectifying column are sequentially connected.
Further, described purification system also includes airbag, cooler, lower pressure adsorber, pressurized adsorbent device and fills
Device；
Described fluorine source gas, reaction unit, water scrubber, caustic wash tower, airbag, cooler, lower pressure adsorber, pressurized adsorbent
Device, rectifying column and filler are sequentially connected.
Further, described reaction unit includes the first reactor being sequentially connected and second reactor；
Described first reactor includes the first cleaner unit, and described second reactor includes the second cleaner unit；
Described first reactor also includes the first feed bin pipe, economizer bank and reaction tube；
The bottom of described first feed bin pipe is provided with trumpet-shaped dilatation pipe, and the opening of described dilatation Guan Youqi upper end is under it
The opening at end gradually inwardly narrows；
Described first feed bin pipe, dilatation pipe and economizer bank be vertically arranged, described reaction tube be horizontally set；
The upper end of described economizer bank is connected with the opening of described dilatation pipe lower end, and the lower end of described economizer bank is communicated in described
The outer wall of reaction tube；
The two ends of described reaction tube are provided with the first air inlet；
Described first feed bin pipe is provided with downtake pipe, and it is connected to described first cleaner unit；
Described second reactor also includes the second feed bin pipe, discharge, heating muff and the 3rd exhaustor；
Described discharge is located at the bottom of described second feed bin pipe；
The top of described discharge is provided with opening and is communicated to the inside of described second feed bin pipe；
The top open part of described discharge is provided with sieve plate；
Described discharge is provided with the 3rd air inlet pipe, and it is connected to described first cleaner unit；
Described 3rd exhaustor is connected to described 4th air inlet pipe of described second cleaner unit；
Described heating muff has multiple, and it is hollow, and it extends transversely through in described second feed bin pipe；
Setting heating tube in described heating muff.
Further, the top of the first feed bin pipe is provided with the first charge pipe and blow-down pipe；
Described one end of first charge pipe and one end of blow-down pipe are respectively communicated with the top of described first feed bin pipe；
The two ends of the other end of described first charge pipe and described reaction tube are equipped with flange and blind flange, described blind flange
It is installed on described flange
Further, described first reactor also includes cooler bin；
In described cooler bin, the two ends of described reaction tube protrude from the outside of described cooler bin to described reaction tube.
Described cooler bin is rectangular box, and its top is provided with opening；
The bottom outer wall of the wherein side wall of described cooler bin is at least provided with a water inlet pipe；
Outer wall at the top proximal of wherein side wall of described cooler bin is at least provided with an overflow pipe；
Described reaction tube is provided with least one thermometer boss；
The lower end closed of described thermometer boss and be located at described reaction tube in；
It is provided with temperature detector in described thermometer boss.
Further, described first cleaner unit includes dust removing tube and dividing plate；
Described dividing plate includes upper spacer and lower clapboard, the quantity all at least one of described upper spacer and lower clapboard；
Described upper spacer and lower clapboard are equally spacedly welded in described dust removing tube；
Adjacent described upper spacer and lower clapboard form dedusting gas circuit；
The outer wall of described dust removing tube is communicated with the second air inlet pipe and the second exhaust pipe within described dust removing tube, described
Downtake pipe is connected with described second air inlet pipe.
Further, the two ends of described dust removing tube are equipped with blind flange and flange, described blind flange be installed on described flange with
Seal described dust removing tube；
Fitted with the lower surface of the described blind flange on described dust removing tube top in the top of described upper spacer, described lower clapboard
Fitted with the upper surface of the described blind flange of described dust removing tube bottom in bottom；
Described first cleaner unit also includes baffle plate；
Described baffle plate is fixed on described blind flange, and be located at respectively described upper spacer or lower clapboard weld two
Side；
The bottom of described dust removing tube is provided with trumpet-shaped seal pipe；
The described blind flange of the bottom of described dust removing tube is communicated with the first blow-off pipe within described dust removing tube, described
First blow-off pipe is provided with valve.
Further, the top of described second feed bin pipe is provided with the second charge pipe, and one end of described second charge pipe is communicated in
The inside of described second feed bin pipe, its other end is provided with flange and blind flange, and described blind flange is installed on described flange；
Described 3rd exhaustor is located at the outer wall of described second charge pipe；
Described second reactor also includes temperature detector, its located at described second feed bin pipe, and close to described heating
Sleeve pipe.
Further, described gas distributor is horn-like；
Described gas distributor is gradually expanded outwardly from the opening of its upper end to the opening of its lower end；
Described gas distributor is fixed on the bottom of described 4th air inlet pipe thereon at end opening；Described gas distributor
Upper arrangement completely pore.
Further, described gas spoiler is horn-like；
Described gas spoiler is gradually inwardly narrowed from the opening of its upper end to the opening of its lower end, the opening of its upper end
Edge is fixed on the inwall of described dust leg；
Described second blow-off pipe is outward-dipping；
The top of described second blow-off pipe side is obtuse angle with the angle A of the base plane formation of described dust leg；
The top of described second blow-off pipe opposite side is acute angle with the angle B of the base plane formation of described dust leg；
The bottom of described second blow-off pipe is provided with sewage draining exit；
Described dust leg is provided with the 4th exhaustor, and it is located at the top of described gas spoiler, and close to described dust
The outer wall at pipe top；
It is provided with Semicircular baffle, it is located in described 4th air inlet pipe close to described 4th exhaustor in described dust leg
That side, and be located at described 4th exhaustor lower section；
Described Semicircular baffle is downward-sloping setting.
It is an object of the invention to proposing a kind of purification system of carbon tetrafluoride, its purification effect is preferable, good dedusting effect.
When being contaminated with the carbon tetrafluoride gas of carbon dust after described 4th air inlet pipe from the bottom of described 4th air inlet pipe
Discharge, described 4th air inlet pipe vertically arranged so as to easier for installation, described gas distributor can will be contaminated with carbon dust
Carbon tetrafluoride gas are uniformly distributed, and in the presence of described gas spoiler, the carbon tetrafluoride gas being contaminated with carbon dust can be in institute
State in dust leg and stop the longer time, be more favorable for carbon dust falls in described second blow-off pipe, described 4th exhaustor
Positioned at the top of described gas spoiler, make finally more to increase from the purity of the carbon tetrafluoride gas of wherein discharge, mix more
Few carbon dust.
Brief description
Fig. 1 is the part sectioned view in the front of first reactor of the one of embodiment of the present invention.
Fig. 2 is the part sectioned view of the side of first reactor of the one of embodiment of the present invention.
Fig. 3 is the part sectioned view in the front of the first cleaner unit of the one of embodiment of the present invention.
Fig. 4 is the partial enlarged drawing at the C of Fig. 3.
Fig. 5 is the positive structure schematic of the second reactor of the one of embodiment of the present invention.
Fig. 6 is the cross-sectional view of the discharge of the one of embodiment of the present invention.
Fig. 7 is the perspective view of the second cleaner unit of the one of embodiment of the present invention.
Fig. 8 is the theory diagram of the one of embodiment of the present invention.
Wherein：Fluorine source gas 1, first reactor 2, the first feed bin pipe 21, dilatation pipe 211, downtake pipe 212, first add
Expects pipe 213, blow-down pipe 214, support base 215, economizer bank 22, reaction tube 23, the first air inlet 231, thermometer boss 232, method
Blue 261, blind flange 262, cooler bin 24, water inlet pipe 241, overflow pipe 242, the first cleaner unit 25, dust removing tube 251, seal pipe
2511st, dividing plate 252, upper spacer 2521, lower clapboard 2522, dedusting gas circuit 253, the second air inlet pipe 254, second exhaust pipe 255, gear
Plate 256, the first blow-off pipe 257, second reactor 3, the second feed bin pipe 31, the 3rd exhaustor 311, the second charge pipe 312, second
Support feet 313, discharge 32, sieve plate 321, the 3rd air inlet pipe 322, support column 323, heating muff 33, temperature detector 34,
Two cleaner units 35, dust leg 351, the 4th exhaustor 3511, Semicircular baffle 3512, the second blow-off pipe 352, sewage draining exit 3521,
First support feet 3522, the 4th air inlet pipe 353, gas distributor 354, pore 3541, gas spoiler 355, water scrubber 4, alkali
Wash tower 5, airbag 6, cooler 7, lower pressure adsorber 81, pressurized adsorbent device 82, rectifying column 9, filler 10.
Specific embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by specific embodiment.
As shown in figure 8, a kind of purification system of carbon tetrafluoride, including the fluorine source gas 1 being sequentially connected, reaction unit, washing
Tower 4, caustic wash tower 5, airbag 6, cooler 7, lower pressure adsorber 81, pressurized adsorbent device 82, rectifying column 9 and filler 10；
Described reaction unit includes first reactor 2 and second reactor 3；
Be provided with booster pump between described caustic wash tower 5 and airbag 6, described lower pressure adsorber 81 and pressurized adsorbent device 82 it
Between be provided with booster pump, for a kind of described carbon tetrafluoride purification system provide power.
Described first reactor 2 includes the first cleaner unit 25, and described second reactor 3 includes the second cleaner unit 35；
The fluorine source gas 1 of the present embodiment prepare fluorine gas using the method for electrolysis, and fluorine gas is passed through to described the from described fluorine source gas 1
The carbon reaction interior with it of one reactor 2 generates carbon tetrafluoride gas, but, often the utilization rate of fluorine gas can not reach percent
Hundred, and can be mixed with the carbon dust of incomplete reaction, reacted gas becomes and mainly contains carbon tetrafluoride, perfluoroethane, octafluoro third
Alkane, carbon monoxide, carbon dioxide, carbon dust, fluorine gas, the mixed gas of fluohydric acid gas；Described first cleaner unit 25 being capable of filtration fraction
Carbon dust, prevents dust blocking follow-up system, improves the purity of carbon tetrafluoride gas.
After single filter, by described second reactor 3, the carbon in described second reactor can be fluorine for mixed gas
Gas thoroughly reacts, and can improve the utilization rate of fluorine gas, and the water being again avoided that in fluorine gas and follow-up water scrubber occurs violent anti-
Should, described second cleaner unit 25 can filter out the overwhelming majority and react incomplete in first reactor 2 and second reactor
Carbon dust, improves the purity of carbon tetrafluoride gas further.
Enter described water scrubber 4 from the second cleaner unit 35 mixed gas out, by the process of washing, can either remove
Fluohydric acid gas in mixed gas, the aqueous solution of fluohydric acid gas can store as side-product, and can save and need in follow-up alkali cleaning
Alkali liquor.From described water scrubber 4 mixed gas out through caustic wash tower 5, the fluorination failing to completely remove in water-washing process
Hydrogen removes, and improves the purity of the carbon tetrafluoride gas in mixed gas further, and the alkali liquor used by the present embodiment is potassium hydroxide
Solution.
Enter to described airbag 6 from described caustic wash tower 5 mixed gas out, mixed gas are gathered up temporarily
Come, ensure that follow-up technique has enough tolerance.During washing, gaseous mixture cognition carries substantial amounts of water, institute secretly
State cooler 7 and can remove substantial amounts of water in mixed gas, be easy to being further purified of follow-up carbon tetrafluoride gas；Described low pressure
Adsorber 81 removes the impurity such as moisture carbon dioxide in mixed gas, carbon monoxide, described pressurized adsorbent device 82 energy further
Enough carbon monoxides further removing in mixed gas, carbon dioxide and micro moisture, improve carbon tetrafluoride gas further
The purity of body；Again through the distillation operation of rectifying column, carbon tetrafluoride gas are separated, then described filler 10 is filled
Dress operation, the carbon tetrafluoride gas after purification are filled.
As shown in figure 1, described first reactor 2 also includes the first feed bin pipe 21, economizer bank 22 and reaction tube 23；
The bottom of described first feed bin pipe 21 is provided with trumpet-shaped dilatation pipe 211, described dilatation pipe 211 opening by its upper end
Mouth gradually inwardly narrows to the opening of its lower end；
Described first feed bin pipe 21, dilatation pipe 211 and economizer bank 22 be vertically arranged, described reaction tube 23 be laterally set
Put；
The upper end of described economizer bank 22 is connected with the opening of described dilatation pipe 211 lower end, and the lower end of described economizer bank 22 is even
Lead in the outer wall of described reaction tube 23；
The two ends of described reaction tube 23 are provided with the first air inlet 231；
Described first feed bin pipe 21 is provided with downtake pipe 212, and it is connected to described first cleaner unit 25；
As shown in figure 5, described second reactor 3 also includes the second feed bin pipe 31, discharge 32, heating muff 33 and the 3rd
Exhaustor 311；
Described discharge 32 is located at the bottom of described second feed bin pipe 31；
The top of described discharge 32 is provided with opening and is communicated to the inside of described second feed bin pipe 31；
The top open part of described discharge 32 is provided with sieve plate 321；
Described discharge 32 is provided with the 3rd air inlet pipe 322, and it is connected to described first cleaner unit 25；
Described 3rd exhaustor 311 is connected to described second cleaner unit 35；
Described heating muff 33 has multiple, and it is hollow, and it extends transversely through in described second feed bin pipe 31；
Setting heating tube in described heating muff 33.
The described first reactor 2 of the present embodiment is used for fluorine gas and carbon reaction generates carbon tetrafluoride, and carbon is placed on described the
In one feed bin pipe 21, economizer bank 22 and reaction tube 23, described first air inlet 231 is located at the two ends of reaction tube 23, one side energy
In enough increasing the unit interval, fluorine gas is passed through to the amount of described reaction tube 23, so that more fluorine gas and carbon is fully contacted, and increases reaction
Efficiency；Fluorine gas and carbon occur to release heat during chemical reaction, and the lower end due to described economizer bank 22 is communicated in described reaction tube
23 outer wall, substantial amounts of heat can be transferred to the carbon in described economizer bank 22 by product carbon tetrafluoride, and these carbon are carried out
Preheating, keeps reaction temperature stable, makes the reaction efficiency of follow-up carbon and fluorine gas higher.
With the carrying out of reaction, the carbon of described reaction tube 23 is gradually consumed, due to described first feed bin pipe 21, dilatation pipe
211 and economizer bank 22 be vertically arranged, under gravity, the carbon in described economizer bank 22 will fall to described reaction
Pipe 23 is persistently carried out with ensureing react, improves stability and the persistence of its work；Similarly, in described first feed bin pipe 21
Carbon can fall to and in described economizer bank 22, ensure that the carbon of question response is preheated, ready for follow-up reaction.
Trumpet-shaped described dilatation pipe 211 has the effect expanding described first feed bin pipe 21 volume, due to described dilatation
Pipe 211 is gradually inwardly narrowed from the opening of its upper end to the opening of its lower end, so being connected to described dilatation pipe 211 upper end open
The first feed bin pipe 21 cross-sectional area can more than be connected to described dilatation pipe 211 lower ending opening economizer bank 22 cross section
Amass it is assumed that described first feed bin pipe 21 and economizer bank 22 are under identical length, the volume of described first feed bin pipe 21 can be significantly
Increasing, thus reducing the addition number of times of carbon, improving the persistence of described first reactor 2 work.
Gaseous mixture cognition carries out dust removal process from described downtake pipe 212 row to described first cleaner unit 25, carries out just
After level dedusting, in mixed gas, the content of carbon dust reduces, and the purity of carbon tetrafluoride gas improves, and the mixing after primary dedusting
Gas enters described discharge 32 by described 3rd air inlet pipe 322, and described sieve plate 321 is to allow carbon dust in mixed gas
Fall in described discharge 32, in order to prevent from blocking；Fluorine gas and carbon tetrafluoride gas then enter to described second by sieve plate 321
Feed bin pipe 31, because described discharge 32 is located at the bottom of described second feed bin pipe 31, can be convenient during follow-up cleaning carbon dust
Fast.
Because described heating muff 33 is hollow, described heating tube is facilitated to put into the inside of described heating muff 33；
Because described heating muff 33 has multiple, it extends transversely through in described second feed bin pipe 31, can be effectively more carbon
It is carried in described second feed bin pipe 31；Heating tube heats, and so that the temperature of the carbon being supported by described heating muff 33 is raised, when
During the carbon haptoreaction that fluorine gas is raised with temperature, the efficiency of reaction can be higher, can quickly generate carbon tetrafluoride gas, then
It is expelled to described second cleaner unit 35 from described 3rd exhaustor 311 and carries out two-stage dust removal, the utilization rate of final fluorine gas reaches hundred
/ hundred, the content of carbon dust is also preferably minimized, and greatly promotes the purity of carbon tetrafluoride gas.
Further, the top of described first feed bin pipe 21 is provided with the first charge pipe 213 and blow-down pipe 214；
Described one end of first charge pipe 213 and one end of blow-down pipe 214 are respectively communicated with described first feed bin pipe 21
Top；
The described other end of the first charge pipe 213 and the two ends of described reaction tube 23 are equipped with flange 261 and blind flange
262, described blind flange 262 is installed on described flange 261.
Carbon in described first reactor 2 after reaction consumes, from located at the first of described first feed bin pipe 21 top
Charge pipe 213 adds carbon, operates simpler convenience directly, because one end of described first charge pipe 213 and blow-down pipe 214
One end is respectively communicated with the top of described first feed bin pipe 21, so carbon can fall to the first feed bin pipe under gravity
21st, dilatation pipe 211, economizer bank 22 and reaction tube 23, to ensure persistently carrying out of reaction；Because described first charge pipe 213
The two ends of the other end and described reaction tube 23 are equipped with flange 261 and blind flange 262, and described blind flange 262 is installed on described method
Blue 261, so described blind flange 262 only need to be dismantled in charging and during emptying gas, just described first reactor 2 can be carried out
Feeding operation.
The other end of described blow-down pipe 214 is communicated to exhaust gas treating tower, and only need to open emptying valve during operation can be to enter
The emptying of circulation of qi promoting body.
Further, described reaction tube 23 be respectively arranged at two ends with flange 261 and blind flange 262, described blind flange 262 is installed
In described flange 261 to seal described reaction tube 23；
Described first air inlet 231 is located at described blind flange 262.
By installing described flange 261 in described blind flange 262, can effectively seal described reaction tube 23, it is to avoid gas
Body leaks, the such as leakage of reactant fluorine gas and the leakage of product carbon tetrafluoride gas；By dismantling described blind flange 262, energy
Enough rapidly clear up the waste residue that the reaction in described reaction tube 23 stays, simple to operation；Described first air inlet 231 located at
Described blind flange 262 is it is ensured that fluorine gas is passed through effectively to described reaction tube.
Further, the described downtake pipe 212 laterally radial position at described first feed bin pipe 21 top proximal.
The described downtake pipe 212 laterally outer wall at described first feed bin pipe 21 top proximal, can make mixing
The distance that gas rises increases, and is conducive to the sedimentation under gravity of carbon dust, improves the purity of carbon tetrafluoride gas.
Further, described first reactor 2 also includes cooler bin 24；
In described cooler bin 24, the two ends of described reaction tube 23 protrude from described cooler bin 24 to described reaction tube 23
Outside.
Fluorine gas and carbon reaction when can release substantial amounts of heat, described cooler bin 24 built with cooling water, to reduce described reaction
The temperature of pipe 23, thus increase its service life.The two ends of described reaction tube 23 protrude from the outside of described cooler bin 24, convenient
It is arranged on the dismounting of the blind flange 262 at its two ends, it is to avoid cooling water enters in described reaction tube 23.
Further, described cooler bin 24 is rectangular box, and its top is provided with opening；
The bottom outer wall of the wherein side wall of described cooler bin 24 is at least provided with a water inlet pipe 241；
Outer wall at the top proximal of wherein side wall of described cooler bin 24 is at least provided with an overflow pipe 242；
Described reaction tube 23 is provided with least one thermometer boss 232；
The lower end closed of described thermometer boss 232 and be located at described reaction tube 23 in；
It is provided with temperature detector 34 in described thermometer boss 232.
The casing of rectangle easily produces, and the cooling water that can load is also more, the opening that its top is provided with play observation and
Check that described first reactor 2 acts on.As shown in Fig. 2 the quantity of the described water inlet pipe 241 of the present embodiment is one, described overflow
The quantity of pipe 242 is two, and described water inlet pipe 241 and overflow pipe 242, all located at the side wall of described cooler bin 24, are more convenient its peace
Dress；The bottom outer wall of the wherein side wall of described cooler bin 24, when cooling water covers the water inlet of described water inlet pipe 241, cold
But water is passed through and can more slowly stablize to during described cooler bin 24；Described overflow pipe 242 is located at wherein the one of described cooler bin 24
Outer wall at the top proximal of side wall it is ensured that the cooling water in described cooler bin 24 enough effectively to cool down described reaction tube
23, it is to avoid cooling water excess overflows.
As shown in figure 1, the quantity of the described thermometer boss 232 of the present embodiment is two, and it is symmetrically set in described economizer bank
On the described reaction tube 23 of 22 both sides, it is possible to increase described temperature detector 34 is accurate to the temperature detection in reaction tube 23
Degree, the lower end closed of described thermometer boss 232, described reaction tube 23 can be sealed and also can protect described temperature detector 34.
Further, as shown in figure 3, described first cleaner unit 25 includes dust removing tube 251 and dividing plate 252；
Described dividing plate 252 includes upper spacer 2521 and lower clapboard 2522, the number of described upper spacer 2521 and lower clapboard 2522
Amount all at least one；
Described upper spacer 2521 and lower clapboard 2522 are equally spacedly welded in described dust removing tube 251；
Adjacent described upper spacer 2521 and lower clapboard 2522 form dedusting gas circuit 253；
The outer wall of described dust removing tube 251 is communicated with the second air inlet pipe 254 and second row within described dust removing tube 251
Trachea 255, described downtake pipe 212 is connected with described second air inlet pipe 254.
Mixed gas when described second air inlet pipe 254 enters to the dedusting gas circuit 253 of described dust removing tube 251, in institute
In the presence of stating iris action and the gravity of upper spacer 2521 and lower clapboard 2522, carbon dust can be settled down to described dust removing tube 251
Bottom, is easy to follow-up cleaning, to improve the purity of carbon tetrafluoride gas, the carbon tetrafluoride gas being finally further purified from
Described second exhaust pipe 255 is expelled to described 3rd air inlet pipe 322.
The quantity of the described upper spacer 2521 of the present embodiment is two, and the quantity of described lower clapboard 2522 is one, by welding,
Make described upper spacer 2521 and lower clapboard 2522 more firmly in described dust removing tube 251.
Further, the two ends of described dust removing tube 251 are equipped with blind flange 262 and flange 261, and described blind flange 262 is installed
In described flange 261 to seal described dust removing tube 251；
Fitted with the lower surface of the described blind flange 262 on described dust removing tube 251 top in the top of described upper spacer 2521, institute
Fitted with the upper surface of the described blind flange 262 of described dust removing tube 251 bottom in the bottom stating lower clapboard 2522；
Described first cleaner unit 25 also includes baffle plate 256；
Described baffle plate 256 is fixed on described blind flange 262, and is located at described upper spacer 2521 or lower clapboard 2522 respectively
Weld both sides；
The bottom of described dust removing tube 251 is provided with trumpet-shaped seal pipe 2511；
The described blind flange 262 of the bottom of described dust removing tube 251 is communicated with the first row within described dust removing tube 251
Dirty pipe 257, described first blow-off pipe 257 is provided with valve.
As shown in Figure 3 and Figure 4, described dust removing tube 251 can rapidly be cleared up by dismounting described blind flange 262, described
Fitted with the lower surface of the described blind flange 262 on described dust removing tube 251 top in the top of upper spacer 2521, described lower clapboard 2522
Bottom fit with the upper surface of the described blind flange 262 of described dust removing tube 251 bottom, so that mixed gas is removed along described as far as possible
Moving in dust and gas road 253, rather than directly directly wears from the joint place of described blind flange 262 and upper spacer 2521 and lower clapboard 2522
Cross, improve and remove the quality of carbon dust and the purity of carbon tetrafluoride gas.
Described baffle plate 256 can stop mixed gas directly from described blind flange 262 and upper spacer 2521 and lower clapboard
2522 joint place is directly through raising further removes the quality of carbon dust and the purity of carbon tetrafluoride gas.
The described blind flange 262 of described dust removing tube 251 bottom need to periodically pull down discharge solid-state carbon dust, but described dust removing tube
The diameter of 251 bottoms is bigger, is more difficult to seal, so described seal pipe 2511 is set to from opening the opening to its lower end of its upper end
The trumpet-shaped pipe that mouth gradually inwardly narrows, improves its seal degree.
The fluorine gas of the present embodiment is produced by electrolysis, so can be contaminated with hydrogen fluoride gas in fluorine gas, when its temperature
Acid solution can be become after degree, in order to clear up safety during carbon dust, first open the valve on described first blow-off pipe 257, clear acid solution,
Dismantle the clear dust of blind flange 262 again.
Further, described first feed bin pipe 21 also includes at least two support bases 215；
Described support base 215 is equally spacedly arranged along the outer wall circumference of described first feed bin pipe 21.
The quantity of the described support base 215 of the present embodiment is two, and it is along between the outer wall circumference etc. of described first feed bin pipe 21
Away from ground setting, can preferably support described first feed bin pipe 21, stress when making described first feed bin pipe 21 be supported is more
Uniformly.
Further, the top of described second feed bin pipe 31 is provided with the second charge pipe 312, and the one of described second charge pipe 312
End is communicated in the inside of described second feed bin pipe 31, and its other end is provided with flange 261 and blind flange 262, and described blind flange 262 is pacified
It is loaded on described flange 261；
Described 3rd exhaustor 311 is located at the outer wall of described second charge pipe 312；
As shown in figure 5, described second reactor 3 also includes temperature detector 34, its located at described second feed bin pipe 31, and
Close to described heating muff 33.
Carbon in described second reactor 3 after reaction consumes, from located at the second of described second feed bin pipe 31 top
Charge pipe 312 adds carbon, operates simpler convenience directly, one end of described second charge pipe 312 is communicated in described second material
The inside of storekeeper 31, so carbon can fall in described second feed bin pipe 31 under gravity, only needs in charging to dismantle
Described blind flange 262, just can carry out feeding operation to described second reactor 3.
Carbon near described heating muff 33 is higher with the reaction efficiency of fluorine gas, and described temperature detector 34 can be effectively
Detect in described second feed bin pipe 31 close to the temperature at described heating muff 33, thus heating tube preferably described in control
Heating-up temperature, to ensure that carbon and fluorine gas is continuously in optimal reaction temperature.
Further, as shown in figure 5, the bottom of described discharge 32 is provided with blind flange 262 and flange 261；
Described blind flange 262 is installed on described flange 261 to seal described discharge 32.
By installing described blind flange 262, more enough can effectively seal described discharge 32, it is to avoid gas leaks；Logical
Cross and dismantle described blind flange 262, can rapidly clear up the dust that the reaction in described discharge 32 stays, mainly described
The carbon dust that sieve plate 321 filters.
Further, as shown in fig. 6, being provided with support column 323 in described discharge 32；
The two ends of described support column 323 are respectively held against the bottom of described sieve plate 321 and the top of described blind flange 262.
Described support column 323 has supporting role to described sieve plate 321, can effectively support described sieve plate 321 it is ensured that
The stability of its work is so as to carbon dust can stably be filtered.
Further, described heating muff 33 is located at the proximal end of described second feed bin pipe 31 bottom.
As far as possible many carbon can be made to be supported by described heating muff 33, on the one hand reduce the number of times subsequently adding carbon, another
Aspect also can make fluorine gas contact with more carbon, improves the efficiency of its reaction.
Described second reactor 3 also includes temperature detector 34, its located at described second feed bin pipe 31, and close to described
Heating muff 33.
Carbon near described heating muff 33 is higher with the reaction efficiency of fluorine gas, and described temperature detector 34 can be effectively
Detect in described second feed bin pipe 31 close to the temperature at described heating muff 33, thus heating tube preferably described in control
Heating-up temperature, to ensure that carbon and fluorine gas is continuously in optimal reaction temperature.
Further, described second cleaner unit 35 includes dust leg 351, the second blow-off pipe 352 and the 4th air inlet pipe 353；
Described 4th air inlet pipe 353 is communicated to described 3rd exhaustor 311；
Described 4th air inlet pipe 353 is vertically arranged, and its bottom is located in described dust leg 351, and its top is through described
The top of dust leg 351；
The bottom of described 4th air inlet pipe 353 is provided with gas distributor 354, positioned at the top of described gas distributor 354
It is provided with gas spoiler 355；
Described second blow-off pipe 352 is located at the bottom of described dust leg 351；
Described dust leg 351 is provided with the 4th exhaustor 3511, and it is located at the top of described gas spoiler 355.
Some reactions can be mixed not in the carbon tetrafluoride gas of the carbon in described second feed bin pipe 31 and fluorine gas reaction generation
Sufficiently carbon dust, when the carbon tetrafluoride gas being contaminated with carbon dust enter to described 4th air inlet pipe 353 through the 3rd exhaustor 311
Discharge from the bottom of described 4th air inlet pipe 353 afterwards, described 4th air inlet pipe 353 vertically arranged so as to easier for installation, institute
State the top of the 4th air inlet pipe 353 through the top of described dust leg 351 so as to connection with described 3rd exhaustor 311
Convenient.
The carbon tetrafluoride gas being contaminated with carbon dust can be uniformly distributed by described gas distributor 354, disturbs in described gas
In the presence of stream plate 355, the carbon tetrafluoride gas being contaminated with carbon dust can stop the longer time, more in described dust leg 351
Plus falling in described second blow-off pipe 352 beneficial to carbon dust, described 4th exhaustor 3511 is located at described gas spoiler 355
Top, make finally more to increase from the purity of the carbon tetrafluoride gas of wherein discharge, mix fewer carbon dust.
Further, described gas distributor 354 is horn-like；
Described gas distributor 354 is gradually expanded outwardly from the opening of its upper end to the opening of its lower end；
Described gas distributor 354 is fixed on the bottom of described 4th air inlet pipe 353 thereon at end opening；Described gas
Full pore 3541 is arranged on distributor 354.
Because the upper end open of described gas distributor 354 is less, it is possible to fourth air inlet pipe 353 less with aperture
Coupling is fixed, and trumpet-shaped described gas distributor 354 is gradually expanded outwardly from the opening of its upper end to the opening of its lower end, makes
The distribution obtaining mixed gas is more uniform, is more favorable for the sedimentation of carbon dust.Described pore 3541 further makes mixed gas
Distribution is more uniform, is more favorable for the sedimentation of carbon dust.
Further, described gas spoiler 355 is horn-like；
Described gas spoiler 355 is gradually inwardly narrowed from the opening of its upper end to the opening of its lower end, the opening of its upper end
The edge of mouth is fixed on the inwall of described dust leg 351；
Described second blow-off pipe 352 is outward-dipping；
The top of described second blow-off pipe 352 side is blunt with the angle A of the base plane formation of described dust leg 351
Angle；
The top of described second blow-off pipe 352 opposite side is sharp with the angle B of the base plane formation of described dust leg 351
Angle；
The bottom of described second blow-off pipe 352 is provided with sewage draining exit 3521；
Described 4th exhaustor 3511 located at described dust leg 351 close to top outer wall；
It is provided with Semicircular baffle 3512, it is located in described 4th air inlet pipe 353 close to described in described dust leg 351
That side of 4th exhaustor 3511, and it is located at the lower section of described 4th exhaustor 3511；
Described Semicircular baffle 3512 is downward-sloping setting.
The edge of the opening of described gas spoiler 355 upper end is fixed on the inwall of described dust leg 351, so being contaminated with
The carbon tetrafluoride gas of carbon dust can be hindered towards the outer wall of described dust leg 351 bottom by described gas spoiler 355 effectively
Gear, makes mixed gas have more times to rest in described dust leg 351, is conducive to the sedimentation of carbon dust；Described gas is disturbed
Stream plate 355 is gradually inwardly narrowed from the opening of its upper end to the opening of its lower end, even if carbon dust is from described gas spoiler 355
Top sedimentation, also will not be deposited on described gas spoiler 355, also can be along the opening of described gas spoiler 355 upper end
Fall to the opening of its lower end, eventually fall in described second blow-off pipe 352.
As shown in fig. 7, the described angle A of the present embodiment is 120 °, angle B is 30 °, and convenient safely cleaning is described
Carbon dust in second blow-off pipe 352, the described sewage draining exit 3521 of the present embodiment is provided with blind flange 262 and flange 261, by dismounting
The mode of blind flange 262, carbon dust is finally discharged from described sewage draining exit 3521.
Described 4th exhaustor 3511 makes mixed gas have more located at described dust leg 351 close to the outer wall at top
Time rest in described dust leg 351, be conducive to the sedimentation of carbon dust；It is provided with Semicircular baffle in described dust leg 351
3512, it can intercept the rising of mixed gas, and mixed gas are rushed for, away from described 4th exhaustor 3511 exit, entering one
Step ground allows mixed gas have more times to rest in described dust leg 351, is more conducive to be conducive to the sedimentation of carbon dust, described partly
Circular baffle plate 3512 is downward-sloping setting, and carbon dust is not easy to pile up thereon, whereabouts of taking advantage of a situation.
The outer wall of described second blow-off pipe 352 is at least vertically provided with three the first support feets 3522, can support described
Second blow-off pipe 352, facilitates its installation.The outer wall of described second feed bin pipe 31 is at least vertically provided with three the second support feets
313, described second feed bin pipe 31 can be supported, facilitate its installation.
Describe the know-why of the present invention above in association with specific embodiment.These descriptions are intended merely to explain the present invention's
Principle, and limiting the scope of the invention can not be construed to by any way.Based on explanation herein, the technology of this area
Personnel do not need to pay other specific embodiments that performing creative labour can associate the present invention, and these modes fall within
Within protection scope of the present invention.
Claims (10)
1. a kind of purification system of carbon tetrafluoride, including fluorine source gas, reaction unit, water scrubber, caustic wash tower and rectifying column；
It is characterized in that：Described reaction unit includes the second cleaner unit；
Described second cleaner unit includes dust leg, the second blow-off pipe and the 4th air inlet pipe；
Described 4th air inlet pipe is vertically arranged, and its bottom is located in described dust leg, and its top is through the top of described dust leg
Portion；
The bottom of described 4th air inlet pipe is provided with gas distributor, is provided with gas flow-disturbing positioned at the top of described gas distributor
Plate；
Described second blow-off pipe is located at the bottom of described dust leg；
Described fluorine source gas, reaction unit, water scrubber, caustic wash tower and rectifying column are sequentially connected.
2. a kind of carbon tetrafluoride according to claim 1 purification system it is characterised in that：Described purification system also includes
Airbag, cooler, lower pressure adsorber, pressurized adsorbent device and filler；
Described fluorine source gas, reaction unit, water scrubber, caustic wash tower, airbag, cooler, lower pressure adsorber, pressurized adsorbent device,
Rectifying column and filler are sequentially connected.
3. a kind of carbon tetrafluoride according to claim 1 purification system it is characterised in that：
Described reaction unit includes the first reactor being sequentially connected and second reactor；
Described first reactor includes the first cleaner unit, and described second reactor includes the second cleaner unit；
Described first reactor also includes the first feed bin pipe, economizer bank and reaction tube；
The bottom of described first feed bin pipe is provided with trumpet-shaped dilatation pipe, and the opening of described dilatation Guan Youqi upper end is to its lower end
Opening gradually inwardly narrows；
Described first feed bin pipe, dilatation pipe and economizer bank be vertically arranged, described reaction tube be horizontally set；
The upper end of described economizer bank is connected with the opening of described dilatation pipe lower end, and the lower end of described economizer bank is communicated in described reaction
The outer wall of pipe；
The two ends of described reaction tube are provided with the first air inlet；
Described first feed bin pipe is provided with downtake pipe, and it is connected to described first cleaner unit；
Described second reactor also includes the second feed bin pipe, discharge, heating muff and the 3rd exhaustor；
Described discharge is located at the bottom of described second feed bin pipe；
The top of described discharge is provided with opening and is communicated to the inside of described second feed bin pipe；
The top open part of described discharge is provided with sieve plate；
Described discharge is provided with the 3rd air inlet pipe, and it is connected to described first cleaner unit；
Described 3rd exhaustor is connected to described 4th air inlet pipe of described second cleaner unit；
Described heating muff has multiple, and it is hollow, and it extends transversely through in described second feed bin pipe；
Setting heating tube in described heating muff.
4. described a kind of purification system of carbon tetrafluoride according to claim 3 it is characterised in that：The top of the first feed bin pipe
Portion is provided with the first charge pipe and blow-down pipe；
Described one end of first charge pipe and one end of blow-down pipe are respectively communicated with the top of described first feed bin pipe；
The two ends of the other end of described first charge pipe and described reaction tube are equipped with flange and blind flange, and described blind flange is installed
In described flange.
5. a kind of carbon tetrafluoride according to claim 3 purification system it is characterised in that：Described first reactor is also wrapped
Include cooler bin；
In described cooler bin, the two ends of described reaction tube protrude from the outside of described cooler bin to described reaction tube.
Described cooler bin is rectangular box, and its top is provided with opening；
The bottom outer wall of the wherein side wall of described cooler bin is at least provided with a water inlet pipe；
Outer wall at the top proximal of wherein side wall of described cooler bin is at least provided with an overflow pipe；
Described reaction tube is provided with least one thermometer boss；
The lower end closed of described thermometer boss and be located at described reaction tube in；
It is provided with temperature detector in described thermometer boss.
6. a kind of carbon tetrafluoride according to claim 3 purification system it is characterised in that：Described first cleaner unit includes
Dust removing tube and dividing plate；
Described dividing plate includes upper spacer and lower clapboard, the quantity all at least one of described upper spacer and lower clapboard；
Described upper spacer and lower clapboard are equally spacedly welded in described dust removing tube；
Adjacent described upper spacer and lower clapboard form dedusting gas circuit；
The outer wall of described dust removing tube is communicated with the second air inlet pipe and the second exhaust pipe within described dust removing tube, and described first
Exhaustor is connected with described second air inlet pipe.
7. a kind of carbon tetrafluoride according to claim 6 purification system it is characterised in that：The two ends of described dust removing tube are equal
It is provided with blind flange and flange, described blind flange is installed on described flange to seal described dust removing tube；
Fitted with the lower surface of the described blind flange on described dust removing tube top in the top of described upper spacer, the bottom of described lower clapboard
Fit with the upper surface of the described blind flange of described dust removing tube bottom；
Described first cleaner unit also includes baffle plate；
Described baffle plate is fixed on described blind flange, and is located at the both sides of the weld of described upper spacer or lower clapboard respectively；
The bottom of described dust removing tube is provided with trumpet-shaped seal pipe；
The described blind flange of the bottom of described dust removing tube is communicated with the first blow-off pipe within described dust removing tube, and described first
Blow-off pipe is provided with valve.
8. a kind of carbon tetrafluoride according to claim 3 purification system it is characterised in that：The top of described second feed bin pipe
Portion is provided with the second charge pipe, and one end of described second charge pipe is communicated in the inside of described second feed bin pipe, and its other end is provided with
Flange and blind flange, described blind flange is installed on described flange；
Described 3rd exhaustor is located at the outer wall of described second charge pipe；
Described second reactor also includes temperature detector, its located at described second feed bin pipe, and close to described heating muff.
9. a kind of carbon tetrafluoride according to claim 1 purification system it is characterised in that：
Described gas distributor is horn-like；
Described gas distributor is gradually expanded outwardly from the opening of its upper end to the opening of its lower end；
Described gas distributor is fixed on the bottom of described 4th air inlet pipe thereon at end opening；Arrange on described gas distributor
The full pore of row.
10. a kind of carbon tetrafluoride according to claim 1 purification system it is characterised in that：Described gas spoiler is
Horn-like；
Described gas spoiler is gradually inwardly narrowed from the opening of its upper end to the opening of its lower end, the edge of the opening of its upper end
It is fixed on the inwall of described dust leg；
Described second blow-off pipe is outward-dipping；
The top of described second blow-off pipe side is obtuse angle with the angle A of the base plane formation of described dust leg；
The top of described second blow-off pipe opposite side is acute angle with the angle B of the base plane formation of described dust leg；
The bottom of described second blow-off pipe is provided with sewage draining exit；
Described dust leg is provided with the 4th exhaustor, and it is located at the top of described gas spoiler, and close to described dust leg top
The outer wall in portion；
Be provided with Semicircular baffle in described dust leg, its be located at the described 4th in air inlet pipe close to described 4th exhaustor that
Side, and it is located at the lower section of described 4th exhaustor；
Described Semicircular baffle is downward-sloping setting.
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