CN108553933A - A kind of thionyl chloride distillation system continuously adds sulphur device and technique - Google Patents
A kind of thionyl chloride distillation system continuously adds sulphur device and technique Download PDFInfo
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- CN108553933A CN108553933A CN201810570162.7A CN201810570162A CN108553933A CN 108553933 A CN108553933 A CN 108553933A CN 201810570162 A CN201810570162 A CN 201810570162A CN 108553933 A CN108553933 A CN 108553933A
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- sulphur
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- molten sulfur
- sulfur
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
- B01J10/005—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor carried out at high temperatures in the presence of a molten material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/45—Compounds containing sulfur and halogen, with or without oxygen
- C01B17/4561—Compounds containing sulfur, halogen and oxygen only
- C01B17/4584—Thionyl chloride (SOCl2)
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a kind of thionyl chloride distillation system and continuously adds sulphur device and technique, including:Molten sulphur and molten sulfur transport system, distillation system and molten sulfur mix return-flow system, wherein:The molten sulphur and molten sulfur transport system include interconnected molten sulphur tank and molten sulfur surge tank;The distillation system includes first rectifying column;It includes return tank that the molten sulfur, which mixes return-flow system,;The molten sulfur surge tank is connected to the return tank, and the return tank is connected to the tower top of the first rectifying column.The invention technology controlling and process is simple, and equipment investment is small, easy to popularize, effectively increases the conversion ratio of sulfur dichloride and chlorine, enhances rectifying separating effect, while significantly reducing the operational risk and workload of staff.
Description
Technical field
The invention belongs to chemical engineering process technical fields, continuously add sulphur more particularly, to a kind of thionyl chloride distillation system
Device and technique.
Background technology
First rectifying column is de-heavy oil column in thionyl chloride distillation system, and main separation task is that removing thionyl chloride is thick
Heavy constituent sulfur monochloride in product.Meanwhile need to over cure device (or over cure section) be set in tower top, solid sulfur is added in over cure device,
It is the heavy constituent sulfur monochloride being easily isolated by light component sulfur dichloride and chlorine conversion.With in over cure device, solid sulfur is not
The conversion ratio of disconnected consumption, sulfur dichloride and chlorine can gradually reduce, and sulphur occur and be unevenly distributed phenomenon, and top gaseous phase is caused to exist
Bias current in over cure device, problem above can lead to impurity content exceeding index in overhead fraction, influence separating effect, therefore need regular replenishment solid
Body sulphur.
Above-mentioned interval adds sulphur system, and there are the following problems:(1) distillation system pressure can be destroyed when regular replenishment solid sulfur,
Rectifying column need to seriously affect production efficiency through re-establishing vapor liquid equilibrium after a period of time;(2) sulphur dispensing port is located at the first essence
Tower top is evaporated, need to manually lift and be transported to dispensing port position, operating personnel are in high-rise working environment, there is grievous hurt and height
The potential risk that place falls;(3) it needs sulfur consumption in periodic observation over cure device and is replenished in time, the work of worker's inspection and operation
Amount is big.It is above-mentioned to solve the problems, such as, it would be highly desirable to which that research and development are a kind of continuously to add sulphur technique, is suitable for chlorination sulfone distillation system.
Invention content
In view of this, the purpose of the present invention is being directed to current thionyl chloride rectifying production process, provides one kind and continuously add
Sulphur device and technique.The technology controlling and process is simple, and equipment investment is small, easy to popularize, effectively increases sulfur dichloride and chlorine
Conversion ratio, enhance rectifying separating effect, while significantly reducing the operational risk and workload of staff.
In order to achieve the above objectives, the technical solution of the invention is realized in:
A kind of thionyl chloride distillation system continuously adds sulphur device, including:Molten sulphur and molten sulfur transport system, distillation system and liquid
Sulphur mixes return-flow system, wherein:
The molten sulphur and molten sulfur transport system include interconnected molten sulphur tank and molten sulfur surge tank;
The distillation system includes first rectifying column;
It includes return tank that the molten sulfur, which mixes return-flow system,;
The molten sulfur surge tank is connected to the return tank, and the return tank is connected to the tower top of the first rectifying column.
Further, the molten sulphur and molten sulfur transport system include sulphur lower hopper, sulphur baiting valve, molten sulphur tank, molten sulfur
Surge tank, submerged pump, molten sulfur feed-line, steam and condensate liquid feed-line.
Further, the sulphur lower hopper material is stainless steel, and bottom cone angle is 60 °, ensures that Cosan can enter
Molten sulphur tank.
Further, the sulphur baiting valve is stainless steel pneumatic ball valve, while easily operated position by lower hopper
Equipped with operation post, the switch of baiting valve is controlled.
Further, the molten sulphur tank material is stainless steel, while being equipped with external jacket, and low-pressure steam is passed through in chuck
Heating fusing is carried out to solid sulfur powder, steam condensate is back to lime set tank.Temperature maintains 120~140 DEG C in molten sulphur tank,
Centrifugally glass-wool insulating layer is equipped with outside chuck, it is adiabatic to molten sulphur tank heat preservation.Molten sulphur tank top is switched equipped with high charge level, and lower part is set
There is low level switch, it can be achieved that high and low material position is alarmed, prompt operating personnel stop charging or sulphur is replenished in time.
Further, the molten sulfur surge tank material is stainless steel, while being equipped with external jacket, and low pressure is passed through in chuck
It is 120~140 DEG C that steam, which maintains temperature in tank, is equipped with centrifugally glass-wool insulating layer outside chuck, is kept the temperature to molten sulfur surge tank exhausted
Heat.Tank deck is equipped with submerged pump, molten sulfur can be delivered to return tank, the seal form of submerged pump is double mechanical seal.
Further, the molten sulfur feed-line is jacketed pipe, and low-pressure steam is passed through in chuck and is carried out entirely to molten sulfur
Journey heat tracing maintains molten sulfur temperature, keeps its good mobile performance.Flow is set on submerged pump outlet molten sulfur feed-line
Meter can adjust molten sulfur addition according to thionyl chloride crude product feed rate.
Further, the distillation system includes first rectifying column, condenser, reboiler, rectifying surge tank, rectifying buffering
Pump and corresponding Location Detection of Medium Transportation Pipeline.
Further, the first rectifying column is packed tower, and filler pattern is corrugated plate regular packing, and filler is divided into three
Section, every section of packed height is 5m.Overhead condenser is dual-tubesheet tubular heat exchanger;Tower reactor thermosyphon reboiler is two-tube
Board-like tubular heat exchanger.Tower top is additionally provided with tank type liquid distributor, and the molten sulfur for being conducive to phegma and wherein dissolving is steamed with rising
Vapour uniformly contacts.
Further, the rectifying surge tank is stainless steel horizontal vessel, and external container is equipped with centrifugally glass-wool insulating layer,
Material is got by tower top discharging pump, is sent respectively to return tank and Second distillation column.On going to the pipeline of Second distillation column
Automatic regulating valve is set, the liquid level of rectifying surge tank is controlled.
Further, it is stainless steel horizontal vessel that the molten sulfur, which mixes return tank in return-flow system, external container be equipped with from
Heart mineral wool insulating layer.Molten sulfur inside extending tube is equipped in the molten sulfur feed inlet of the return tank, extended in the molten sulfur inside extending tube away from
Tank bottom 150-300mm, while molten sulfur inside extending tube bottom sets blind plate, it is Φ 8mm apertures that 4 row's sizes are opened in side, often arranges 10 holes, hole
Spacing is 20mm, and 4 row's apertures are uniformly distributed in 360 °, this, which is provided with, is sufficiently mixed and dissolves in phegma conducive to molten sulfur.It dissolves
The phegma of molten sulfur is pumped to the first rectifying column tower top through reflux, and molten sulfur is made to react with sulfur dichloride and chlorine, controls
Impurity content in overhead fraction processed.
Further, it is provided with automatic regulating valve on the feeding line of the return tank, can control the liquid level of return tank.
The phegma pipeline is provided with autocontrol valve, and the tower top temperature of first rectifying column can be controlled by adjusting regurgitant volume.
The present invention has following advantage:
1. realizing the production technology for continuously adding sulphur into thionyl chloride distillation system, ensure the continuous of distillation operation
Property, improve production efficiency;
2. Molten sulphur is added into distillation system, instead of the solid sulfur in former technique, to make sulphur in tower top point
Cloth is more uniform, improves the conversion ratio of sulfur dichloride, chlorine and sulfur reaction, enhances separating effect;
3. avoiding the potential risk of worker's high-rise working, the labor intensity of worker is greatly reduced.
The another object of the invention is to propose that a kind of thionyl chloride distillation system continuously adds sulphur technique, including as follows
Step:
Step 1, in the molten sulphur tank to solid sulfur powder carry out heating fusing obtain Molten sulphur;
Step 2, the Molten sulphur enter the molten sulfur surge tank and enter the reflux by the molten sulfur surge tank
It is mixed with thionyl chloride in tank;
Step 3, Molten sulphur and thionyl chloride mixture, which pass back into, carries out rectifying in the first rectifying column.
Further, operating pressure is 1-10kPaG in the first rectifying column, and tower top operation temperature is 70~80 DEG C, tower
Kettle operation temperature is 120~130 DEG C, and sulphur addition is 1~4 times of reactive chemistry metering.
In above-mentioned steps, sulphur tank is melted if being only arranged, cannot achieve the requirement sent out immediately after sulphur fusing.Therefore it must be arranged
One molten sulfur surge tank, could realize continuous operation.
Description of the drawings
A part of attached drawing for constituting the present invention is used to provide further understanding of the present invention, schematic implementation of the invention
Example and its explanation are not constituted improper limitations of the present invention for explaining the present invention.In the accompanying drawings:
Fig. 1 is according to embodiment disclosed by the invention, and a kind of thionyl chloride distillation system continuously adds the flow of sulphur technique
Schematic diagram.
Fig. 2 is the side for continuously adding return tank molten sulfur inside extending tube described in sulphur technique in order to illustrate a kind of thionyl chloride distillation system
View.
Fig. 3 is the vertical view for continuously adding tank type liquid distributor described in sulphur technique in order to illustrate a kind of thionyl chloride distillation system
Figure.
Fig. 4 is the side view for continuously adding tank type liquid distributor described in sulphur technique in order to illustrate a kind of thionyl chloride distillation system
Figure.
In figure:(01) sulphur lower hopper;(011) sulphur baiting valve;(02) sulphur tank is melted;(03) molten sulfur surge tank;(031) liquid
Sulphur transport Stream gauge;(04) submerged pump;(05) return tank;(051) return tank fluid level transmitter;(052) return tank liquid level is adjusted
Valve;(053) molten sulfur inside extending tube;(054) molten sulfur inside extending tube side opening;(055) molten sulfur inside extending tube bottom blind flange;(06) reflux pump;
(07) first rectifying column;(071) tower top temperature transmitter;(072) tower top temperature regulating valve;(073) tank type liquid distributor;
(08) condenser;(09) rectifying surge tank;(091) rectifying surge tank fluid level transmitter;(092) rectifying surge tank liquid level is adjusted
Valve;(10) tower top discharging pump;(11) reboiler;(12) molten sulfur conveys jacketed pipe.
It is logistics code name in box in figure, wherein:(21,22) molten sulfur;(23) phegma;(24) thionyl chloride crude product into
Material;(25) top gaseous phase;(26) overhead condensation liquid;(27) return tank is fed;(28) tower top discharges;(29) tower reactor discharges;(31,
33) steam is heated;(32,34) steam condensate.
Specific implementation mode
In addition to being defined, technical term used in following embodiment has and the invention one of ordinary skill in the art
The identical meanings being commonly understood by.Test reagent used in following embodiment is unless otherwise specified conventional biochemical reagent;
The experimental method is unless otherwise specified conventional method.
All Digital IDs, such as temperature, pressure, length, quality, flow, including range are all approximations.It has wanted
Solution, although all adding term " about " before always not describing all Digital IDs explicitly.While it will also be understood that, although not total
It is explicitly to describe, reagent described herein is only example, and equivalent is known in the art.
With reference to embodiment come the present invention will be described in detail create.
Embodiment 1
Solid sulfur used in the present embodiment is Cosan, and packaging bag specification is 25kg/ bags.First, by the artificial broken bag of sulphur
After be put into sulphur lower hopper, sulphur automatic blanking valve is then opened by Operation switch, Cosan, which enters, to be melted in sulphur tank.In repetition
Operation is stated, Cosan is added in molten sulphur tank, the frequency is operated to reduce, according to knowhow, makes in molten sulphur tank sulphur amount extremely
Meet one day production requirement less.
0.5MPaG low-pressure steams are passed through in the external jacket of molten sulphur tank, heating fusing is carried out to solid sulfur.Pass through temperature
Spending instrument, temperature in sulphur tank is melted in monitoring in real time, to ensure that Molten sulphur is in optimal flow performance, maintains to melt temperature in sulphur tank and exists
120~140 DEG C.The molten sulfur of fusing enters molten sulfur surge tank by gravity stream, and molten sulfur feed-line is jacketed pipe, is led in chuck
It is molten sulfur pipeline heat tracing to enter low-pressure steam.To maintain molten sulfur temperature, it is low in the external jacket of molten sulfur surge tank to be passed through 0.5MPaG
Press steam.Buffered molten sulfur is delivered to return tank by submerged pump, and molten sulfur flowmeter is arranged on pump discharge pipeline, controls and supervises
Survey molten sulfur flow.Molten sulfur is solved homogeneously in return tank in thionyl chloride phegma.The phegma for having dissolved Molten sulphur is logical
The tank type liquid distributor that reflux is pumped into the tower top of first rectifying column is crossed, molten sulfur is uniformly distributed with phegma in distributor
Afterwards, it is come into full contact with tower top upflowing vapor.It is to be easy to point by light component sulfur dichloride and chlorine conversion by chemically reacting
From heavy constituent sulfur monochloride.
Thionyl chloride crude product feed composition (mass fraction) is as follows in the present embodiment:Thionyl chloride 75.7%;Sulfur monochloride
18.3%;Sulfur dioxide 4.4%;Sulfur dichloride 1.2%;Chlorine 0.4%.After first rectifying column is detached, kettle material
Main composition is heavy constituent sulfur monochloride, excessive sulphur, thionyl chloride, and kettle liquid enters sulfur monochloride dashpot and carries out recycling profit
With;Overhead fraction mainly organize as concentrate after thionyl chloride, light component sulfur dioxide, tower top discharging enter Second distillation column after
Continuous removing light component.
First rectifying column operating pressure described in the present embodiment is 5kPaG, and tower top operation temperature is 70~80 DEG C, tower reactor behaviour
It is 120~130 DEG C to make temperature, operating reflux ratio 1.2.Sulphur addition is 2 times of reactive chemistry metering, keeps sulphur excessive,
Ensure that sulfur dichloride and chlorine are fully converted.
Tower top discharging composition (mass fraction) is after rectifying separation:Thionyl chloride 93.9%;Sulfur dioxide 6.0%;Dichloro
Change sulphur, chlorine content is respectively less than 500ppm;Sulfur monochloride and sulphur is not detected.By continuous into thionyl chloride distillation system
Add sulphur to operate, so that first rectifying column is stripped of the heavy constituent sulfur monochloride in charging, while sulfur dichloride and chlorine being carried out
Effectively conversion, finally makes impurity composition in overhead product meet index request.
In theory, reflux ratio is bigger, sulphur addition is bigger, and separating effect is better.But the present invention considers
Tower top impurity content and process energy consumption, therefore, in the present embodiment use reflux ratio 1.2, and sulphur addition is the 2 of stoichiometry
Times, final to ensure that tower top impurity content is less than 500pp and realizes best energy-saving effect, this is theoretical calculation and limited number of time examination
Test the effect being unable to reach.
Embodiment 2
Sulphur technique, the operation of embodiment 2 and embodiment 1 are continuously added for thionyl chloride distillation system of the present invention
Journey and thionyl chloride crude product feed composition are identical.Embodiment 2 difference from example 1 is that:The operation of distillation system is returned
Stream is than being 1.8;Sulphur addition is 3 times of reactive chemistry metering.
Sulfur dichloride, chlorine content are less than 100ppm, impurity composition in the first rectifying column ejection material composition of the present embodiment
Content it is lower.Embodiment 2 is obviously improved compared with the separating effect of embodiment 1, but since reflux ratio increases, and sulphur input amount
More, therefore operating cost is improved.The present embodiment is suitable for the downstream user occasion more demanding to target product impurity content.
The foregoing is merely the preferred embodiments of the invention, are not intended to limit the invention creation, all at this
Within the spirit and principle of innovation and creation, any modification, equivalent replacement, improvement and so on should be included in the invention
Protection domain within.
Claims (10)
1. a kind of thionyl chloride distillation system continuously adds sulphur device, it is characterised in that:Including:Molten sulphur and molten sulfur transport system, essence
It evaporates system and molten sulfur mixes return-flow system, wherein:
The molten sulphur and molten sulfur transport system include interconnected molten sulphur tank and molten sulfur surge tank;
The distillation system includes first rectifying column;
It includes return tank that the molten sulfur, which mixes return-flow system,;
The molten sulfur surge tank is connected to the return tank, and the return tank is connected to the tower top of the first rectifying column.
2. a kind of thionyl chloride distillation system according to claim 1 continuously adds sulphur device, it is characterised in that:The molten sulphur
And molten sulfur transport system includes sulphur lower hopper, sulphur baiting valve, molten sulphur tank, molten sulfur surge tank, submerged pump, molten sulfur delivery pipe
Line, steam and condensate liquid feed-line.
3. a kind of thionyl chloride distillation system according to claim 1 continuously adds sulphur device, it is characterised in that:The sulphur
Lower hopper material is stainless steel, and bottom cone angle is 60 °, ensures that Cosan can enter molten sulphur tank, the sulphur baiting valve is not
Become rusty steel pneumatic ball valve, while easily operated position by lower hopper is equipped with operation post, controls the switch of baiting valve.
4. a kind of thionyl chloride distillation system according to claim 1 continuously adds sulphur device, it is characterised in that:The molten sulphur
Tank material is stainless steel, while being equipped with external jacket, and low-pressure steam is passed through in chuck and carries out heating fusing to solid sulfur powder,
Steam condensate is back to lime set tank, and temperature maintains 120~140 DEG C in the molten sulphur tank, and rotary glass is equipped with outside chuck
Cotton insulating layer, it is adiabatic to molten sulphur tank heat preservation.
5. a kind of thionyl chloride distillation system according to claim 1 continuously adds sulphur device, it is characterised in that:The molten sulfur
Surge tank material be stainless steel, while be equipped with external jacket, be passed through in chuck low-pressure steam maintain tank in temperature be 120~
140 DEG C, chuck outside is equipped with centrifugally glass-wool insulating layer, is kept the temperature to molten sulfur surge tank adiabatic.Tank deck is equipped with submerged pump, can be by liquid
Sulphur is delivered to return tank, and the seal form of submerged pump is double mechanical seal.
6. a kind of thionyl chloride distillation system according to claim 1 continuously adds sulphur device, it is characterised in that:Its feature exists
In:The molten sulfur feed-line is jacketed pipe, and low-pressure steam is passed through in chuck and carries out whole heat tracing to molten sulfur, maintains molten sulfur
Temperature keeps its good mobile performance.Flowmeter is set on submerged pump outlet molten sulfur feed-line, it can be according to thionyl chloride
Crude product feed rate adjusts molten sulfur addition.
7. a kind of thionyl chloride distillation system according to claim 1 continuously adds sulphur device, it is characterised in that:The rectifying
System includes first rectifying column, condenser, reboiler, rectifying surge tank, rectifying buffering pump and corresponding Location Detection of Medium Transportation Pipeline.
8. a kind of thionyl chloride distillation system according to claim 1 continuously adds sulphur device, it is characterised in that:The reflux
It is equipped with molten sulfur inside extending tube in the molten sulfur feed inlet of tank, is extended to away from tank bottom 200mm, while molten sulfur inside extending tube in the molten sulfur inside extending tube
Bottom sets blind plate, and it is Φ 8mm apertures that 4 row's sizes are opened in side, often arranges 10 holes, pitch of holes 20mm, and 4 row's apertures are in 360 ° equal
Cloth.
9. a kind of thionyl chloride distillation system continuously adds sulphur technique, it is characterised in that:Include the following steps:
Step 1, in the molten sulphur tank to solid sulfur powder carry out heating fusing obtain Molten sulphur;
Step 2, the Molten sulphur enter the molten sulfur surge tank and are entered in the return tank by the molten sulfur surge tank
It is mixed with thionyl chloride;
Step 3, Molten sulphur and thionyl chloride mixture flow back into the first rectifying column.
10. a kind of thionyl chloride distillation system according to claim 9 continuously adds sulphur technique, it is characterised in that:Described
Operating pressure is 1~10kPaG in one rectifying column, and tower top operation temperature is 70~80 DEG C, and tower reactor operation temperature is 120~130
DEG C, sulphur addition is 1~4 times of reactive chemistry metering.
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Cited By (1)
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CN112169711A (en) * | 2020-09-26 | 2021-01-05 | 安徽金禾实业股份有限公司 | Continuous vulcanizing device and method for thionyl chloride sulfur distribution system |
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CN112169711B (en) * | 2020-09-26 | 2021-08-27 | 安徽金轩科技有限公司 | Continuous vulcanizing device and method for thionyl chloride sulfur distribution system |
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Application publication date: 20180921 |