CN103922291A - Multi-chamber reactor for preparing sulfur hexafluoride and usage method of multi-chamber reactor - Google Patents

Multi-chamber reactor for preparing sulfur hexafluoride and usage method of multi-chamber reactor Download PDF

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Publication number
CN103922291A
CN103922291A CN201410167981.9A CN201410167981A CN103922291A CN 103922291 A CN103922291 A CN 103922291A CN 201410167981 A CN201410167981 A CN 201410167981A CN 103922291 A CN103922291 A CN 103922291A
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chamber
reaction
reactor
sulphur
sulfur hexafluoride
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CN201410167981.9A
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CN103922291B (en
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张怀
赵纪峥
赵冰
牛学坤
张景利
张志勇
徐洪涛
朱进京
苗凯
杨柠
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Haohua Gas Co Ltd
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Liming Research Institute of Chemical Industry Co Ltd
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Abstract

The invention discloses a multi-chamber reactor for preparing sulfur hexafluoride, and a usage method of the multi-chamber reactor. A reaction zone of the multi-chamber reactor is divided into an upper part and a lower part, the lower part is a liquid phase chamber, the upper part is divided into at least two reaction chambers by a partition, a channel is left between the partition and the bottom of the multi-chamber reactor, each reaction chamber is provided with a fluorine inlet and a sulfur hexafluoride outlet, a charging zone is communicated with all the reaction chambers through the channel between the partition and the bottom of the multi-chamber reactor, a temperature control device is arranged on the upper part of the multi-chamber reactor, and a sulfur heater is arranged at the bottom of the multi-chamber reactor. According to production or overhauling demand, any one or more reaction chambers can be closed or opened. The multi-chamber reactor is easy for the technology to control, the phenomenon of blocking an outlet of the reactor due to single reaction chamber can be reduced, the consumption is low, the production cost is low and the overhauling is convenient.

Description

A kind of multiple-chamber reactor and using method thereof of preparing sulfur hexafluoride
Technical field
The present invention relates to a kind of reactor of preparing sulfur hexafluoride, particularly a kind of fluorine gas and melting sulfur reaction and prepare the multiple-chamber reactor of sulfur hexafluoride.
Background technology
Sulfur hexafluoride is often produced in the mode of fluorine gas and sulphur direct reaction, and concrete grammar has three classes: 1) Gu gas-reaction: the direct and solid-state sulphur contact reacts of fluorine gas; 2) gas-liquid reaction: fluorine gas and molten sulfur reaction; 3) gas-solid/liquid/gas reactions: fluorine gas and gaseous state sulfur reaction.
Because fluorine, reaction of Salmon-Saxl are violent thermopositive reaction, when fluorine gas reacts with solid sulfur, temperature of reaction is wayward, and by product is many, and post-processing difficulty is large, is not suitable for suitability for industrialized production.Fluorine gas and gaseous state sulfur reaction, be sulphur is heated to 445 ℃ (boiling points) more than, make sulphur become gaseous state and send into reactor and react with fluorine, this method also exists the unmanageable defect of temperature of reaction, simultaneous reactions device must adopt special material, is also unsuitable for suitability for industrialized production.Fluorine gas and melting sulfur reaction, be that the sulphur in reactor is remained under molten state and reacted with the fluorine gas passing into, and this method temperature of reaction is more easy to control, is the industrial main method of current sulfur hexafluoride.
As Fig. 1, shown in 2, be device schematic diagram and the vertical view of preparing sulfur hexafluoride of prior art, the reaction unit that prior art is prepared sulfur hexafluoride comprises molten sulphur device 1, inside at molten sulphur device 1 is provided with liquid baffle plate 2 and gas baffle 3, one end at molten sulphur device 1, one side of liquid baffle plate 2 is provided with sulphur and adds entrance 4, opposite side at liquid baffle plate 2 is provided with fluorine gas import 5, the other end at reaction unit is provided with thick gas sulfur hexafluoride outlet 6, bottom at molten sulphur device is provided with electric heater unit 7, bottom liquid phase region at reaction unit is provided with thermometer 8, on the top of reaction unit, cooling water jecket 9 is set, between the bottom of molten sulphur device 1 and liquid baffle plate 2, there is a path 10.
The reaction process that prior art is prepared sulfur hexafluoride is: solid sulfur adds entrance 4 by sulphur and adds in the C of charging zone, Molten sulphur after thawing enters reaction zone D by path 10, by electric heater unit, maintain sulphur again and melt vaporization, and control by thermometer 8, fluorine gas enters in the D of reaction zone and sulphur steam reaction by fluorine gas import 5, the heat that wherein reaction produces is undertaken cooling by cooling water jecket 9, the sulfur hexafluoride gas of generation enters next process from exporting 6.
CN201089722Y discloses a kind of device of preparing sulfur hexafluoride, comprise molten sulphur device and reactor, upper end at molten sulphur device is provided with sulphur entrance, lower end at molten sulphur device is provided with relief outlet, molten sulphur device and reactor divide and are arranged and communicate by pipeline, in reactor shell, be respectively arranged with fluorine gas entrance, sulfur hexafluoride outlet, at inside reactor, be provided with two dividing plates.
CN203440075U discloses a kind of device of preparing sulfur hexafluoride gas, comprises molten sulphur device and reactor, and molten sulphur device communicates by Molten sulphur outlet conduit with reactor.
In current sulfur hexafluoride industrial production, a reactor only has a reaction compartment, has following shortcoming:
1) reactor quantity is many, and it is more loaded down with trivial details that the sulphur of reactor such as adds at the operation;
2) system leak source is corresponding more, fluorine gas low conversion rate, and in thick gas, foreign matter content is also many;
3) in reasons such as electrolyzer maintenance, cause under the temporary transient dead status of reactor, need heating to maintain sulphur in molten state, product energy consumption is high.
Summary of the invention
First technical problem that the present invention will solve is to provide a kind of multiple-chamber reactor of preparing sulfur hexafluoride.
Second technical problem that the present invention will solve is to provide a kind of using method of this multiple-chamber reactor.
The multiple-chamber reactor of preparing sulfur hexafluoride of the present invention, be included as charging zone and reaction zone, its reaction zone is divided at least two reaction chambers by dividing plate, and each reaction chamber is a unit that fluorine gas reacts with liquid-state sulfur, between dividing plate and multiple-chamber reactor bottom, leaves passage.
The detailed technical scheme of the present invention is: a kind of multiple-chamber reactor of preparing sulfur hexafluoride, be included as charging zone and reaction zone, reaction zone is divided into upper and lower two portions, bottom is liquid-phase chamber, top is divided at least two reaction chambers by dividing plate, between dividing plate and multiple-chamber reactor bottom, leave passage, each reaction chamber is established fluorine gas import and sulfur hexafluoride outlet, charging zone communicates with each reaction chamber with the passage between multiple-chamber reactor bottom by dividing plate, multiple-chamber reactor top is provided with temperature regulating device, and multiple-chamber reactor bottom is provided with sulphur well heater.Its material is soft steel, stainless steel, nickel or Monel metal etc.
The sulphur well heater of described multiple-chamber reactor bottom setting can be electric heater, for sulphur heating, sulphur is heated to fusing point more than 120 ℃, becomes molten state; Multiple-chamber reactor top is provided with cooling water jecket, the heat of fluorine gas and the generation of sulfur reaction process is shifted, and be provided with reaction chamber temperature point for measuring temperature on reactor top.
According to producing or maintenance needs, can close or open wherein arbitrary or several reaction chamber.
The use procedure that the present invention prepares the multiple-chamber reactor of sulfur hexafluoride is:
Solid sulphur joins charging zone C by sulphur charging opening 11, and by sulphur well heater 19, by solid sulphur heat fused, temperature is controlled at 120~180 ℃, and optimum temps is at 125~140 ℃, and the liquid-state sulfur of melting is distributed in the B of liquid-phase chamber region; Fluorine gas is parallel to liquid phase sulphur metal line 20 by fluorine gas import 12 and enters in reaction chamber a-quadrant, by temperature-measuring casing 13 thermometrics, sulphur and fluorine gas carry out chemical reaction, in cooling water jecket 18, pass into water coolant simultaneously, multiple-chamber reactor is carried out to temperature control, and the sulfur hexafluoride of generation enters into hypomere operation from sulfur hexafluoride outlet 14.In reaction process, according to the height of liquid level, sulphur is added in charging zone in good time.
The present invention is that during sulfur hexafluoride is produced, a conventional reactor only has a reaction compartment, an and corresponding liquid Space of reaction compartment, change a reactor into and have a plurality of reaction compartments, and the corresponding liquid Space of a plurality of reaction compartments, solved in sulfur hexafluoride industrial production and prepared the problems such as sulfur hexafluoride reactor quantity is many, reduced the energy consumption of sulfur hexafluoride.
The present invention joins together to form a whole liquid-phase chamber by Molten sulphur by the liquid phase part of reaction zone, has reduced work fussy degree, and technique is easy to control.Simultaneously, because a plurality of reaction chambers are connected, make the volume of liquid-phase chamber relatively large, when system pressure fluctuation is larger, the fluctuation range of sulphur liquid level greatly reduces than the fluctuation range of the conventional single reaction compartment of single reactor, reduce Molten sulphur and overflowed in SF6 outlet conduit, caused the probability of sulphur frozen plug pipeline, reduced the phenomenon that reactor outlet that single chamber reactor causes stops up.
When the single chamber reactor of prior art is temporarily stopped using, in order to keep sulfur melting state, need to heat sulphur and maintain the above temperature of fusing point, will to sulphur, heat in advance the electric energy that need consumption is a large amount of while again enabling reactor.And the liquid phase of multiple-chamber reactor communicates, even if one of them even a plurality of reaction chamber is stopped using, because the heat release of fluorine, reaction of Salmon-Saxl is larger, in reaction chamber in normal use, the reaction heat of fluorine, reaction of Salmon-Saxl will make sulphur temperature in molten state, or by regulating the flow velocity of temperature lowering water just can make sulphur keep molten state, without sulphur heater is heated.Like this, multiple-chamber reactor can make sulphur always in molten state, heats the energy consumption of sulphur while having avoided reactor again to drive after parking because maintenance or other reason cause, and has greatly reduced production cost; Can improve simultaneously fluorine gas transformation efficiency, reduced the foreign matter content in thick gas.
Accompanying drawing explanation
Fig. 1 is the device schematic diagram of preparing sulfur hexafluoride of prior art
Fig. 2 is the vertical view of preparing sulfur hexafluoride of prior art
Fig. 3 is multiple-chamber reactor schematic diagram of the present invention
Fig. 4 is multiple-chamber reactor vertical view of the present invention
Fig. 5 is multiple-chamber reactor fluorine gas of the present invention ingress sectional view
1 molten sulphur device, 2 liquid baffle plates, 3 gas barriers, 4 sulphur add entrance, 5 fluorine gas entrances, 6 sulfur hexafluoride outlets, 7 electric heaters, 8 thermometers, 9 cooling water jeckets, 10 passage 11 sulphur charging openings, 12 fluorine gas imports, 13 temperature-measuring casings, 14 sulfur hexafluorides export 15 entrance of cooling water, 16 cooling water outlets, 17 dividing plates, 18 cooling water jecket 19 sulphur well heaters, 20 sulphur metal lines, 21 gas baffles, 22 sulphur passage A reaction chambers, B liquid-phase chamber, C charging zone, D reaction zone
Embodiment
Below in conjunction with embodiment, the invention will be further described.
As Fig. 3, 4, shown in 5, a kind of multiple-chamber reactor of preparing sulfur hexafluoride of the present invention, be divided into charging zone C and reaction zone D, multiple-chamber reactor top is provided with cooling water jecket 18, on cooling water jecket, be provided with cooling water inlet 15 and cooling water outlet 16, molten state sulphur liquid level 20 is divided into upper and lower two portions by reaction zone, top is divided at least two reaction chamber A by dividing plate 17, bottom is the B of liquid-phase chamber, the length of dividing plate should be able to reach molten state sulphur liquid level following and and multiple-chamber reactor bottom between leave Molten sulphur passage 22, each reaction chamber A is provided with fluorine gas import 12, temperature-measuring casing 13, sulfur hexafluoride outlet 14 and gas baffle 21, the B of liquid-phase chamber communicates with each reaction chamber A by liquid-state sulfur, reactor bottom is provided with sulphur well heater 19.Multiple-chamber reactor of the present invention adopts plain carbon stool to make.
Embodiment 1
Multiple-chamber reactor reaction chamber is wherein more than 2.
Solid sulphur joins charging zone by sulphur charging opening 11, and by sulphur well heater 19, by solid sulphur heat fused, temperature is controlled at 120~180 ℃, and optimum temps is at 125~140 ℃, and the liquid-state sulfur of melting is distributed in the B of liquid-phase chamber territory; Fluorine gas is parallel to liquid phase sulphur metal line 20 by fluorine gas import 11 and enters in reaction chamber a-quadrant, by temperature-measuring casing 13 monitoring reaction chamber temperatures, sulphur and fluorine gas carry out chemical reaction, in cooling water jecket 18, pass into water coolant simultaneously, multiple-chamber reactor is lowered the temperature, and the sulfur hexafluoride of generation enters into hypomere operation from sulfur hexafluoride outlet 16.In reaction is carried out, according to the height of liquid level, sulphur is added in charging zone in good time.Gained sulfur hexafluoride (SF 6) content of each component of gas is in Table 1.
Table 1 sulfur hexafluoride (SF 6) each component concentration of gas
Component SF 6 CF 4 C 2F 6 C 3F 8 HF F 2 O 2 N 2 SOF 2 SO 2F 2
Content >95% <0.5% <0.05% <500ppm <0.5% <0.5% <1% <2% <200ppm <100ppm
Embodiment 2
The fluorine gas of multiple-chamber reactor in embodiment 1 one of them or several reaction chambers is closed, and this reaction chamber quits work, and the work such as can overhaul.Other reaction chambers are working properly.
The multiple-chamber reactor of preparing sulfur hexafluoride provided by the invention can obviously reduce the energy consumption in sulfur hexafluoride production, has reduced the production cost of product.

Claims (6)

1. a multiple-chamber reactor of preparing sulfur hexafluoride, comprises charging zone and reaction zone, and its reaction zone is divided at least two reaction chambers by dividing plate, and each reaction chamber is a unit that fluorine gas reacts with liquid-state sulfur, between dividing plate and multiple-chamber reactor bottom, leaves passage.
2. the multiple-chamber reactor of preparing sulfur hexafluoride according to claim 1, it is characterized in that reaction zone is divided into upper and lower two portions, bottom is liquid-phase chamber, top is divided at least two reaction chambers by dividing plate, between dividing plate and multiple-chamber reactor bottom, leave passage, each reaction chamber is provided with fluorine gas import and sulfur hexafluoride outlet, and charging zone communicates with each reaction chamber with the passage between multiple-chamber reactor bottom by dividing plate, multiple-chamber reactor top is provided with temperature regulating device, and bottom is provided with sulphur well heater.
3. the multiple-chamber reactor of preparing sulfur hexafluoride according to claim 2, is characterized in that the bottom of multiple-chamber reactor is provided with electric heater, and the top of multiple-chamber reactor is provided with cooling water jecket.
4. the multiple-chamber reactor of preparing sulfur hexafluoride according to claim 3, is characterized in that cutting out or opening wherein arbitrary or several reaction chamber.
5. according to the multiple-chamber reactor of preparing sulfur hexafluoride one of claim 1~4 Suo Shu, it is characterized in that adopting plain carbon stool to make.
6. the using method of the described multiple-chamber reactor of preparing sulfur hexafluoride of one of claim 1~4, solid sulphur joins charging zone (C) by sulphur charging opening (11), by sulphur well heater (19) by solid sulphur heat fused, temperature is controlled at 120~180 ℃, and the liquid-state sulfur of melting is distributed in liquid-phase chamber (B) region; Fluorine gas is parallel to liquid phase sulphur metal line (20) by fluorine gas import (12) and enters in reaction chamber (A) region, by temperature-measuring casing (13) thermometric, sulphur and fluorine gas carry out chemical reaction, in cooling water jecket (18), pass into water coolant simultaneously, multiple-chamber reactor is carried out to temperature control, the sulfur hexafluoride generating enters into hypomere operation from sulfur hexafluoride outlet (14), in reaction is carried out, according to the height of liquid level, sulphur is added in charging zone in good time.
CN201410167981.9A 2014-04-18 2014-04-18 A kind of multiple hearth reactor preparing sulfur hexafluoride and using method thereof Active CN103922291B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105926003A (en) * 2016-07-07 2016-09-07 洛阳高昌机电科技有限公司 Multi-chamber reactor for preparing sulfur hexafluoride
CN109455673A (en) * 2018-11-07 2019-03-12 华能(天津)煤气化发电有限公司 A kind of sulphur purification apparatus system
CN115121211A (en) * 2022-06-23 2022-09-30 中船(邯郸)派瑞特种气体股份有限公司 Equipment for preparing sulfur tetrafluoride

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030070606A1 (en) * 2001-10-05 2003-04-17 Leblond Nicolas Preparation of feedstock of alkaline earth and alkali metal fluorides
CN101955165A (en) * 2010-10-18 2011-01-26 天津市泰旭物流有限公司 Technology for producing sulfur hexafluoride by utilizing fluorine and molten sulfur surface contact reaction method
CN203144104U (en) * 2013-03-29 2013-08-21 四川众力氟业有限责任公司 Pyrolyzing furnace applicable to sulfur hexafluoride production
CN203440075U (en) * 2013-07-18 2014-02-19 苏州金宏气体股份有限公司 Novel reactor device for preparing sulfur hexafluoride gas
CN203807168U (en) * 2014-04-18 2014-09-03 黎明化工研究设计院有限责任公司 Multi-hearth reactor for preparing sulfur hexafluoride

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030070606A1 (en) * 2001-10-05 2003-04-17 Leblond Nicolas Preparation of feedstock of alkaline earth and alkali metal fluorides
CN101955165A (en) * 2010-10-18 2011-01-26 天津市泰旭物流有限公司 Technology for producing sulfur hexafluoride by utilizing fluorine and molten sulfur surface contact reaction method
CN203144104U (en) * 2013-03-29 2013-08-21 四川众力氟业有限责任公司 Pyrolyzing furnace applicable to sulfur hexafluoride production
CN203440075U (en) * 2013-07-18 2014-02-19 苏州金宏气体股份有限公司 Novel reactor device for preparing sulfur hexafluoride gas
CN203807168U (en) * 2014-04-18 2014-09-03 黎明化工研究设计院有限责任公司 Multi-hearth reactor for preparing sulfur hexafluoride

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105926003A (en) * 2016-07-07 2016-09-07 洛阳高昌机电科技有限公司 Multi-chamber reactor for preparing sulfur hexafluoride
CN105926003B (en) * 2016-07-07 2018-06-01 泉州市君贤网络科技有限公司 A kind of multiple hearth reactor for preparing sulfur hexafluoride
CN109455673A (en) * 2018-11-07 2019-03-12 华能(天津)煤气化发电有限公司 A kind of sulphur purification apparatus system
CN115121211A (en) * 2022-06-23 2022-09-30 中船(邯郸)派瑞特种气体股份有限公司 Equipment for preparing sulfur tetrafluoride
CN115121211B (en) * 2022-06-23 2023-05-02 中船(邯郸)派瑞特种气体股份有限公司 Equipment for preparing sulfur tetrafluoride

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Effective date of registration: 20210521

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Patentee before: LIMING Research Institute OF CHEMICAL INDUSTRY

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