CN106187676B - The recovery method of distillation residual liquid in a kind of production of tetrachloro-ethylene - Google Patents
The recovery method of distillation residual liquid in a kind of production of tetrachloro-ethylene Download PDFInfo
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- CN106187676B CN106187676B CN201610696192.3A CN201610696192A CN106187676B CN 106187676 B CN106187676 B CN 106187676B CN 201610696192 A CN201610696192 A CN 201610696192A CN 106187676 B CN106187676 B CN 106187676B
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Abstract
The present invention proposes the recovery method of distillation residual liquid in a kind of production of tetrachloro-ethylene, includes the following steps：The heavy constituent of chilling tower reactor sequentially enters lightness-removing column and tetrachloro-ethylene rectifying column in tetrachloro-ethylene production, and tower bottoms is again introduced into de- tetrachloro-ethylene tower and carries out secondary rectifying, further separation and recycling tetrachloro-ethylene；Tower bottoms after de- tetrachloro-ethylene enters pentachloroethane rectifying column, and tower bottoms enters carbon trichloride rectifying column, obtains carbon trichloride product.It can effectively solve the problems, such as that useful constituent emission loss is big in conventional heavy constituent concentration and recovery method, raffinate treating capacity is big, can effectively recycle the tetrachloro-ethylene in heavy constituent, be sufficiently separated out carbon trichloride product, to reduce loss, reduce cost, additional income.
Description
Technical field
The invention belongs to chemical waste liquid processing technology fields, and in particular to distillation residual liquid returns in a kind of production of tetrachloro-ethylene
Receiving method.
Background technology
Tetrachloro-ethylene production in heavy constituent, that is, hexachloride, main component be tetrachloro-ethylene and carbon trichloride, it is also few
Pentachloroethane, hexachlorobutadiene and the hexachloro-benzene of amount, yield are about the 10% of tetrachloro-ethylene product volume.Current tetrachloro-ethylene
Process units, generally from chilling tower and the place of tetrachloro-ethylene tower bottom of rectifying tower two be pumped into heavy constituent system for concentrating and recycling into
Row is concentrated by evaporation recycling, in order to allow process units steady and continuous to run, is concentrated by evaporation temperature and all controls at 200 DEG C or less.It is super
A large amount of hexachlorides will be circulated back to reaction system together with carbon tetrachloride, tetrachloro-ethylene light component after crossing 200 DEG C, cause to react
System hexachloride concentration over-standard, so as to cause material Crystallization Plugging equipment and pipeline, reaction system can not continuous and steady operation.
Current tetrachloro-ethylene heavy constituent concentration and recovery method, since concentration can only be evaporated in lower temperature range
Recycling carbon tetrachloride and tetrachloro-ethylene light component, therefore the still tetrachloro-ethylene containing 30-40%, various chlordenes in the raffinate discharged
Object can not be kept completely separate；And at solid after raffinate barrelling crystallisation by cooling, without much practical values, only a few handles producer and carries out
Simple separating treatment, treating capacity is little, and most of qualified processing producers are all to carry out burning disposal, and processing cost is expensive,
Generally at 4000-8000 yuan/ton；There is also larger safety and environmentally friendly risk, years in transport and processing procedure for raffinate simultaneously
Millions of heavy constituent processing costs will be taken out every year by producing 10,000 tons of tetrachloro-ethylene manufacturing enterprise, this intangibly increases enterprise
Production cost, reduce the competitiveness of enterprise.
Invention content
The present invention is in order to solve the susceptible to plugging technical problem of tetrachloro-ethylene kettle liquid perchloride rectifying separation equipment, it is proposed that
The recovery method of distillation residual liquid in a kind of production of tetrachloro-ethylene.Useful group can be effectively solved in conventional heavy constituent concentration and recovery method
Divide the problem that emission loss is big, raffinate treating capacity is big, can effectively recycle the tetrachloro-ethylene in heavy constituent, be sufficiently separated out chlordene
Ethane product reduces cost, additional income to reduce loss.
In order to achieve the above-mentioned object of the invention, the present invention adopts the following technical scheme that：
The recovery method of distillation residual liquid, includes the following steps in a kind of production of tetrachloro-ethylene：
A, the heavy constituent of chilling tower reactor sequentially enters lightness-removing column and tetrachloro-ethylene rectifying column, tower bottoms in tetrachloro-ethylene production
It is again introduced into de- tetrachloro-ethylene tower and carries out secondary rectifying, further separation and recycling tetrachloro-ethylene；
Preferably, the tower top temperature of the lightness-removing column is 76-80 DEG C, pressure 8-10kpa；Bottom temperature is 145-155
DEG C, pressure 105-125kpa.Energy consumption can be reduced using compression rectification, be sufficiently separated out light component.
Preferably, the light component that the lightness-removing column obtains is added in the carbon tetrachloride raw material in tetrachloro-ethylene production, into
Enter reaction system and participates in reaction.
Preferably, the tower top temperature of the tetrachloro-ethylene rectifying column is 118-124 DEG C, pressure 2-5kpa；Bottom temperature
It is 130-140 DEG C, pressure 40-50kpa.The quality of tetrachloro-ethylene product is improved while reducing energy consumption, product purity reaches
99.99% or more.
Preferably, the tower top temperature of the de- tetrachloro-ethylene tower is 115-125 DEG C, pressure 15-25kpa；Bottom temperature
It is 195-205 DEG C, pressure 45-55kpa.Energy consumption is reduced, while further increasing the rate of recovery of tetrachloro-ethylene.
B, it takes off the tower bottoms after tetrachloro-ethylene and enters pentachloroethane rectifying column, tower bottoms enters carbon trichloride rectifying column, obtains
To carbon trichloride product.
Preferably, the pentachloroethane is added to after separating in the carbon tetrachloride raw material in tetrachloro-ethylene production, into
Enter reaction system and participates in reaction.
Preferably, the tower top temperature of the de- pentachloroethane tower is 155-165 DEG C, pressure 15-25kpa；Bottom temperature
It is 205-220 DEG C, pressure 45-55kpa.Energy consumption is reduced, pentachloroethane component is fully removed.
Preferably, the tower top temperature of the carbon trichloride rectifying column is 185-195 DEG C, pressure 15-25kpa；Tower reactor temperature
Degree is 220-240 DEG C, pressure 45-55kpa.Energy consumption is reduced, the carbon trichloride rate of recovery is improved, reduces the final residual liquid discharge of device
Amount.
Preferably, the tetrachloro-ethylene product obtained using recycling rinses tower top to dissolve the crystal in tower, avoids blocking.
The distillate of secondary rectifying of the present invention returns to the rectifying again of tetrachloro-ethylene rectifying column, in order to fully recycle tower reactor
Tetrachloro-ethylene in liquid needs to improve the secondary rectifying of bottom temperature progress, and tower top tetrachloro-ethylene product heavy constituent content also can
It increases, therefore the distillate of secondary rectifying again returns to tetrachloro-ethylene rectifying column and be refining to obtain tetrachloro-ethylene product, four
The vinyl chloride rate of recovery can reach 99.5%.
The beneficial effects of the present invention are：
1, carbon trichloride and a small amount of hexachloro-benzene boiling point are high in tetrachloro-ethylene rectifying column kettle liquid, and fusing point is also high, and carbon trichloride exists
184.5 DEG C begin to distil, if control bad separation temperature and material composition, material will Crystallization Plugging equipment and pipeline, be
System cannot continuous and steady operation.The present invention solves the problems, such as that the high chlorine object rectifying separation equipment of tetrachloro-ethylene kettle liquid is easily stifled.
2, the heavy constituent of chilling tower reactor is introduced into lightness-removing column and tetrachloro-ethylene rectifying column during the present invention produces tetrachloro-ethylene,
Deviate from hydrogen chloride, chlorine, carbon tetrachloride and part tetrachloro-ethylene therein；Into the tetrachloro-ethylene rectifying column of raffinate recovery system
Without hydrogen chloride and chlorine in kettle liquid, the corrosion to raffinate reclaimer is alleviated, reduces equipment, pipeline and the electrical throwing of instrument
Money.
3, tetrachloro-ethylene rectifying column kettle liquid is introduced into de- tetrachloro-ethylene tower, and tetrachloro-ethylene is further separated out to come, recycling
Using tetrachloro-ethylene, the yield of tetrachloro-ethylene is increased；De- tetrachloro-ethylene tower bottoms, which enters, takes off pentachloroethane tower, because of pentachloroethane
Amount deficiency rectifying tower reactor liquid measure 1% (wt%), therefore be added to after pentachloroethane is separated tetrachloro-ethylene production in
It inside carbon tetrachloride raw material, enters back into reaction system and participates in reaction, the discharge of raffinate is reduced while increasing utilization rate.Effectively solution
The problem that useful constituent emission loss is big, raffinate treating capacity is big in certainly conventional heavy constituent system for concentrating and recycling.
4, since tetrachloro-ethylene tower reactor heavy constituent is relatively more, boiling point difference is big, and amount is also bigger, if rectifying is not recycled again
Useful constituent, for residual liquid discharge amount with regard to big, processing cost is expensive.The present invention has carried out secondary rectifying to tetrachloro-ethylene, be in order into
One step recycles the component of tetrachloro-ethylene in kettle liquid, reduces discharge, and processing cost is low.
5, it takes off pentachloroethane tower bottoms and enters carbon trichloride rectifying column, carbon trichloride is separated, work is used as after pack
Industry product is sold, and carbon trichloride product can reach the index request in industrial carbon trichloride HG/T 3261-2002 standards, and six
Chloroethanes tower reactor liquid measure is seldom, send qualified unit to be handled after longer cooling, greatly reduces tetrachloro-ethylene production dress
Set residual liquid discharge amount.The present invention can not only fully recycle tetrachloro-ethylene, and can separate and recover 90% or so carbon trichloride work
For product, emission loss is greatly reduced, reduces production cost, additional income.
Specific embodiment
In order to facilitate the understanding of those skilled in the art, below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
The recovery method of distillation residual liquid, includes the following steps in a kind of production of tetrachloro-ethylene：
A, the heavy constituent of chilling tower reactor sequentially enters lightness-removing column and tetrachloro-ethylene rectifying column, tower bottoms in tetrachloro-ethylene production
It is again introduced into de- tetrachloro-ethylene tower and carries out secondary rectifying, further separation and recycling tetrachloro-ethylene；
B, it takes off the tower bottoms after tetrachloro-ethylene and enters pentachloroethane rectifying column, tower bottoms enters carbon trichloride rectifying column, obtains
To carbon trichloride product.
Embodiment 2
The recovery method of distillation residual liquid, includes the following steps in a kind of production of tetrachloro-ethylene：
A, the heavy constituent of chilling tower reactor sequentially enters lightness-removing column and tetrachloro-ethylene rectifying column, tower bottoms in tetrachloro-ethylene production
It is again introduced into de- tetrachloro-ethylene tower and carries out secondary rectifying, further separation and recycling tetrachloro-ethylene；
B, it takes off the tower bottoms after tetrachloro-ethylene and enters pentachloroethane rectifying column, tower bottoms enters carbon trichloride rectifying column, obtains
To carbon trichloride product.
The tower top temperature of the lightness-removing column is 76 DEG C, pressure 8kpa；Bottom temperature is 145 DEG C, pressure 105kpa.
Embodiment 3
The recovery method of distillation residual liquid, includes the following steps in a kind of production of tetrachloro-ethylene：
A, the heavy constituent of chilling tower reactor sequentially enters lightness-removing column and tetrachloro-ethylene rectifying column, tower bottoms in tetrachloro-ethylene production
It is again introduced into de- tetrachloro-ethylene tower and carries out secondary rectifying, further separation and recycling tetrachloro-ethylene；
B, it takes off the tower bottoms after tetrachloro-ethylene and enters pentachloroethane rectifying column, tower bottoms enters carbon trichloride rectifying column, obtains
To carbon trichloride product.
The tower top temperature of the lightness-removing column is 80 DEG C, pressure 10kpa；Bottom temperature is 155 DEG C, pressure 125kpa.
The tower top temperature of the tetrachloro-ethylene rectifying column is 124 DEG C, pressure 5kpa；Bottom temperature is 140 DEG C, and pressure is
50kpa。
Embodiment 4
The recovery method of distillation residual liquid, includes the following steps in a kind of production of tetrachloro-ethylene：
A, the heavy constituent of chilling tower reactor sequentially enters lightness-removing column and tetrachloro-ethylene rectifying column, tower bottoms in tetrachloro-ethylene production
It is again introduced into de- tetrachloro-ethylene tower and carries out secondary rectifying, further separation and recycling tetrachloro-ethylene；
B, it takes off the tower bottoms after tetrachloro-ethylene and enters pentachloroethane rectifying column, tower bottoms enters carbon trichloride rectifying column, obtains
To carbon trichloride product.
The tower top temperature of the lightness-removing column is 78 DEG C, pressure 8kpa；Bottom temperature is 146 DEG C, pressure 115kpa.
The tower top temperature of the tetrachloro-ethylene rectifying column is 118 DEG C, pressure 2kpa；Bottom temperature is 130 DEG C, and pressure is
40kpa。
The tower top temperature of the de- tetrachloro-ethylene tower is 115 DEG C, pressure 15kpa；Bottom temperature is 195 DEG C, and pressure is
45kpa。
The pentachloroethane that the light component and the pentachloroethane rectifying column that the lightness-removing column obtains are isolated is added to four
In carbon tetrachloride raw material in vinyl chloride production, participate in reacting into reaction system.
The distillate of the secondary rectifying returns to the rectifying again of tetrachloro-ethylene rectifying column.
Embodiment 5
The recovery method of distillation residual liquid, includes the following steps in a kind of production of tetrachloro-ethylene：
A, the heavy constituent of chilling tower reactor sequentially enters lightness-removing column and tetrachloro-ethylene rectifying column, tower bottoms in tetrachloro-ethylene production
It is again introduced into de- tetrachloro-ethylene tower and carries out secondary rectifying, further separation and recycling tetrachloro-ethylene；
B, it takes off the tower bottoms after tetrachloro-ethylene and enters pentachloroethane rectifying column, tower bottoms enters carbon trichloride rectifying column, obtains
To carbon trichloride product.
The tower top temperature of the lightness-removing column is 79 DEG C, pressure 10kpa；Bottom temperature is 150 DEG C, pressure 120kpa.
The tower top temperature of the tetrachloro-ethylene rectifying column is 120 DEG C, pressure 3kpa；Bottom temperature is 132 DEG C, and pressure is
45kpa。
The tower top temperature of the de- tetrachloro-ethylene tower is 125 DEG C, pressure 25kpa；Bottom temperature is 205 DEG C, and pressure is
55kpa。
The tower top temperature of the pentachloroethane rectifying column is 165 DEG C, pressure 25kpa；Bottom temperature is 220 DEG C, pressure
For 55kpa.
The tower top temperature of the carbon trichloride rectifying column is 190 DEG C, pressure 20kpa；Bottom temperature is 225 DEG C, pressure
For 50kpa.
The pentachloroethane that the light component and the pentachloroethane rectifying column that the lightness-removing column obtains are isolated is added to four
In carbon tetrachloride raw material in vinyl chloride production, participate in reacting into reaction system.
The tetrachloro-ethylene product obtained using recycling rinses tower top to dissolve the crystal in tower.
Embodiment 6
The recovery method of distillation residual liquid, includes the following steps in a kind of production of tetrachloro-ethylene：
A, the heavy constituent of chilling tower reactor sequentially enters lightness-removing column and tetrachloro-ethylene rectifying column, tower bottoms in tetrachloro-ethylene production
It is again introduced into de- tetrachloro-ethylene tower and carries out secondary rectifying, further separation and recycling tetrachloro-ethylene；
B, it takes off the tower bottoms after tetrachloro-ethylene and enters pentachloroethane rectifying column, tower bottoms enters carbon trichloride rectifying column, obtains
To carbon trichloride product.
The tower top temperature of the lightness-removing column is 78 DEG C, pressure 9kpa；Bottom temperature is 152 DEG C, pressure 112kpa.
The tower top temperature of the tetrachloro-ethylene rectifying column is 122 DEG C, pressure 3kpa；Bottom temperature is 136 DEG C, and pressure is
42kpa。
The tower top temperature of the de- tetrachloro-ethylene tower is 120 DEG C, pressure 16kpa；Bottom temperature is 198 DEG C, and pressure is
46kpa。
The tower top temperature of the pentachloroethane rectifying column is 160 DEG C, pressure 18kpa；Bottom temperature is 210 DEG C, pressure
For 48kpa.
The tower top temperature of the carbon trichloride rectifying column is 195 DEG C, pressure 25kpa；Bottom temperature is 240 DEG C, pressure
For 55kpa.
The pentachloroethane that the light component and the pentachloroethane rectifying column that the lightness-removing column obtains are isolated is added to four
In carbon tetrachloride raw material in vinyl chloride production, participate in reacting into reaction system.
The tetrachloro-ethylene product obtained using recycling rinses tower top to dissolve the crystal in tower.
The distillate of the secondary rectifying returns to the rectifying again of tetrachloro-ethylene rectifying column.
Embodiment 7
The recovery method of distillation residual liquid, includes the following steps in a kind of production of tetrachloro-ethylene：
A, the heavy constituent of chilling tower reactor sequentially enters lightness-removing column and tetrachloro-ethylene rectifying column, tower bottoms in tetrachloro-ethylene production
It is again introduced into de- tetrachloro-ethylene tower and carries out secondary rectifying, further separation and recycling tetrachloro-ethylene；
B, it takes off the tower bottoms after tetrachloro-ethylene and enters pentachloroethane rectifying column, tower bottoms enters carbon trichloride rectifying column, obtains
To carbon trichloride product.
The tower top temperature of the lightness-removing column is 77 DEG C, pressure 8kpa；Bottom temperature is 152 DEG C, pressure 120kpa.
The tower top temperature of the tetrachloro-ethylene rectifying column is 122 DEG C, pressure 4kpa；Bottom temperature is 132 DEG C, and pressure is
45kpa。
The tower top temperature of the de- tetrachloro-ethylene tower is 118 DEG C, pressure 16kpa；Bottom temperature is 202 DEG C, and pressure is
48kpa。
The tower top temperature of the pentachloroethane rectifying column is 155 DEG C, pressure 15kpa；Bottom temperature is 205 DEG C, pressure
For 45kpa.
The tower top temperature of the carbon trichloride rectifying column is 185 DEG C, pressure 15kpa；Bottom temperature is 220 DEG C, pressure
For 45kpa.
The pentachloroethane that the light component and the pentachloroethane rectifying column that the lightness-removing column obtains are isolated is added to four
In carbon tetrachloride raw material in vinyl chloride production, participate in reacting into reaction system.
The tetrachloro-ethylene product obtained using recycling rinses tower top to dissolve the crystal in tower.
The distillate of the secondary rectifying returns to the rectifying again of tetrachloro-ethylene rectifying column.
The recovery system used in recovery method of the present invention, including lightness-removing column, first rectifying column, Second distillation column, third
Rectifying column and the 4th rectifying column；The feed inlet of the bottom liquid outlet connection first rectifying column of the lightness-removing column, first rectifying
The feed inlet of the bottom liquid outlet connection Second distillation column of tower, the bottom liquid outlet of the Second distillation column connect third distillation column
Feed inlet, the bottom liquid outlet of the third distillation column connects the feed inlet of the 4th rectifying column；The 4th smart gold-plating tower it is cold
It is provided with collecting tank below condenser, the inside of the condenser is communicated with collecting tank, and the bottom surface of collecting tank by bottom surface and is higher than
The upper bottom surface of bottom surface forms, and the bottom surface is provided with discharge port, and the upper bottom surface is provided with connection descending trays
Leakage fluid dram, riser is additionally provided in collecting tank, and the lower end air inlet of riser is connected to descending trays, the top setting of riser
There is exhaust outlet.
Condenser is arranged in the top of collecting tank this system, after the condensate liquid of overhead condenser is fallen, just collects and exists
In collecting tank, a part is produced as product from the bottom surface discharge port of sump bottom, and produced quantity is controlled by regulating valve, cold
The more liquid levels of lime set accumulation slowly rise, and have been more than that the height of leakage fluid dram is just flowed to automatically in following one layer of column plate.Phegma is logical
Crossing collecting tank itself can overflow in tower, be not required in addition design return tank, and existing return tank is all arranged outside tower, and
And also phegma is squeezed into reflux pump and realizes forced refluence in tower.The collecting tank of this system is a part for tower body, entirely
The temperature at tower each position in the process of running is metastable, avoid the occurrence of be arranged outside tower return tank temperature change compared with
Big situation, will not be elongated because of flow, and surface area becomes larger, and thermal loss is big, and temperature change is big and material crystallization is caused to generate
The case where blocking.
Preferably, system can also be provided with the liter gas cap of closing nozzle on the top of riser, and the tube wall of riser is circumferential
Annular spread has multiple exhaust outlets.Liter gas cap can block the liquid that overhead condenser cools down and not fall in riser.Tube wall is set
Set exhaust outlet for the uprising gas in tower by and enter condenser, extend the time of contact of gas and liquid, ensure sufficient
Vapor liquid equilibrium is better achieved in mass transport process.
Specific implementation mode of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.
Claims (6)
1. the recovery method of distillation residual liquid in a kind of tetrachloro-ethylene production, which is characterized in that include the following steps：
A, the heavy constituent of chilling tower reactor sequentially enters lightness-removing column and tetrachloro-ethylene rectifying column in tetrachloro-ethylene production, and tower bottoms is again
Into carrying out secondary rectifying in de- tetrachloro-ethylene tower, it is smart again that the distillate of the secondary rectifying returns to tetrachloro-ethylene rectifying column
It evaporates, further separation and recycling tetrachloro-ethylene；
B, it takes off the tower bottoms after tetrachloro-ethylene and enters pentachloroethane rectifying column, tower bottoms enters carbon trichloride rectifying column, obtains six
Chloroethanes product；
The tower top temperature of the tetrachloro-ethylene rectifying column is 118-124 DEG C, pressure 2-5kpa；Bottom temperature is 130-140 DEG C,
Pressure is 40-50kpa；
The tower top temperature of the de- tetrachloro-ethylene tower is 115-125 DEG C, pressure 15-25kpa；Bottom temperature is 195-205 DEG C,
Pressure is 45-55kpa.
2. the recovery method of distillation residual liquid in a kind of tetrachloro-ethylene production according to claim 1, which is characterized in that described
The tower top temperature of lightness-removing column is 76-80 DEG C, pressure 8-10kpa；Bottom temperature is 145-155 DEG C, pressure 105-125kpa.
3. the recovery method of distillation residual liquid in a kind of tetrachloro-ethylene production according to claim 1, which is characterized in that described
The tower top temperature of pentachloroethane rectifying column is 155-165 DEG C, pressure 15-25kpa；Bottom temperature is 205-220 DEG C, and pressure is
45-55kpa。
4. the recovery method of distillation residual liquid in a kind of tetrachloro-ethylene production according to claim 1, which is characterized in that described
The tower top temperature of carbon trichloride rectifying column is 185-195 DEG C, pressure 15-25kpa；Bottom temperature is 220-240 DEG C, and pressure is
45-55kpa。
5. according to the recovery method of distillation residual liquid in a kind of tetrachloro-ethylene production described in claim 1, which is characterized in that use back
It receives obtained tetrachloro-ethylene product and rinses tower top to dissolve the crystal in tower.
6. the recovery method of distillation residual liquid in a kind of tetrachloro-ethylene production according to any one of claim 1-5,
It is characterized in that, the pentachloroethane that the light component and the pentachloroethane rectifying column that the lightness-removing column obtains are isolated is added to four
In carbon tetrachloride raw material in vinyl chloride production, participate in reacting into reaction system.
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| RU2560773C2 (en) * | 2013-04-29 | 2015-08-20 | Федеральное государственное унитарное предприятие "Российский научный центр "Прикладная химия" | Method of recycling chlororganic wastes |
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