CN110479124A - A kind of tetrachloroethanes process units and its method - Google Patents
A kind of tetrachloroethanes process units and its method Download PDFInfo
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- CN110479124A CN110479124A CN201910733406.3A CN201910733406A CN110479124A CN 110479124 A CN110479124 A CN 110479124A CN 201910733406 A CN201910733406 A CN 201910733406A CN 110479124 A CN110479124 A CN 110479124A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/20—Mixing gases with liquids
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- 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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/013—Preparation of halogenated hydrocarbons by addition of halogens
- C07C17/02—Preparation of halogenated hydrocarbons by addition of halogens to unsaturated hydrocarbons
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- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00026—Controlling or regulating the heat exchange system
- B01J2208/00035—Controlling or regulating the heat exchange system involving measured parameters
- B01J2208/00044—Temperature measurement
Abstract
The invention discloses a kind of tetrachloroethanes process units, including reactor, forced circulation heat exchanger, circulating pump, complete condenser, tail condenser, level-one dehydrater and second level dehydrater, the gas phase import of the gaseous phase outlet and complete condenser of reactor connects, the liquid-phase outlet of complete condenser is connected with the import of level-one dehydrater, the outlet of level-one dehydrater and the liquid-phase outlet of second level dehydrater are connected in parallel, the gaseous phase outlet of complete condenser is connect with the import of tail condenser, the liquid-phase outlet of tail condenser is connect with the import of second level dehydrater, the phegma outlet of second level dehydrater is connected with the phegma import of reactor, reactor bottom is provided with circulation fluid outlet, circulation fluid outlet is connect with the import of circulating pump, the outlet of circulating pump is connected with the import of forced circulation heat exchanger, the outlet of forced circulation heat exchanger and the circulation fluid import of reactor connect.The present invention also provides the methods for using device production tetrachloroethanes.The advantages of present invention has structure simple, and operating flexibility is big, safety and environmental protection.
Description
Technical field
The present invention relates to chloralkane technical fields, specifically, being related to a kind of tetrachloroethanes process units and its method.
Background technique
Tetrachloroethanes is a kind of solvent, is slightly soluble in water, since its toxicity is big, dissolving power is strong, therefore removes and makees the molten of specific use
Outside agent, it is mainly used as the manufacture raw material of trichloro ethylene, tetrachloro-ethylene.It is also used to the system of Insecticides (tech) & Herbicides (tech) and film etc.
It makes.
In tetrachloroethanes production, the production capacity of reaction unit directly determines the yield of tetrachloroethanes.It is domestic at present raw
The enterprise for producing tetrachloroethanes, is all made of conventional carbon steel enamel reactor, and internal diameter is generally 1200~4000mm, heat dissipation effect
Difference, gasket are easy leakage, and vacuum degree is difficult to ensure, separate unit reaction unit produces yield≤4500t/a of tetrachloroethanes, serious to make
The about yield of tetrachloroethanes.Restrict tetrachloroethanes list set reaction unit yield principal element be in reaction process acetylene gas and
The heat that chlorine reaction generates is more difficult to be taken away, the more difficult band of heat that reaction generates in the middle part of the reactor being especially relatively large in diameter
It walks, acetylene and chlorine flowrate is caused to be difficult to be promoted, to constrain the yield of single set reaction unit production tetrachloroethanes.Meanwhile
Temperature is affected to the selectivity of reaction, and temperature is higher, and side reaction is more, so as to cause product purity reduction, reaction choosing
Select rate and yield decline.And conventional carbon steel enamel reactor gas-liquid mass transfer heat-transfer effect is poor, and acetylene and chlorine is easily caused to match
Unstable, temperature distribution is non-uniform, and side reaction increases, and declines selecting response rate and yield.In addition, if being pressed in operational process
Power control is bad, and rupture disk is easy detonation, and material can spray, and security risk is high.
If Chinese patent notification number CN203507980U discloses a kind of trichloro ethylene production chlorination tower, including tower body,
Tower body is divided into the first tower section, the second tower section, third tower section and the 4th tower section from bottom to top；First tower section be equipped with acetylene gas entrance and
Chlorine inlet, acetylene entrance is interior inserted with acetylene distributor pipe, and chlorine inlet is interior inserted with chlorine distributor pipe；Acetylene distributor pipe and chlorine
The bottom of gas distributor pipe is respectively equipped with venthole；First tower section is set there are two first circulation mouth, more domestic currently used enamel
The tetrachloroethanes quality of chlorination tower production is high, and ceramic packing is loaded in tower, keeps two kinds of gases of chlorine and acetylene equal in chlorination tower
Even distribution avoids local detonation, can quickly be carried out continuously charging production, and specific yield energy consumption is low, and utilization rate of equipment and installations is high.Deficiency
Place is that each tower section temperature difference is big in the chlorination tower, and control is difficult, and product recovery rate is lower.
If China Patent Publication No. CN102267868A discloses a kind of industrial production apparatus for trichloroethylene, it has acetylene
Admission line and chlorine admission line are connected with chlorination tower input end respectively, thick tetrachloroethanes tank outlet end and tetrachloroethanes tower into
Mouth end is connected, and another outlet end of dehydrochlorination reaction device feed preheater is connected with desorber input end, the outlet of extraction-container flow container
End be connected with low boiling tower input end, low boiling tower lower part outlet end respectively with low boiling tower reboiler input end and trichloro ethylene tower import
End be connected, trichloro ethylene kettle liquid tank outlet end is connected with midbarrel tower input end, midbarrel tower lower part outlet end respectively with
Midbarrel tower reboiler input end and tetrachloro-ethylene tower input end are connected, the heat exchanger of each complete condenser, each tail cooler
Part uses the graphite piece of phenol-formaldehyde resin modified dipping.This industrial production apparatus for trichloroethylene, structurally reasonable, production capacity
It greatly, being capable of safe and stable long-term operation.Trichloro ethylene product quality produced is high.Shortcoming is heat in reaction tower
Using poor, thick tetrachloroethanes purity is not high, and energy consumption is higher.
If Chinese patent notification number CN201912928U is related to a kind of chlorination tower, including four tower sections, from tower bottom to tower top
Section, main reaction section, secondary response section and gaseous phase section are respectively fed, the outside of main reaction section is equipped with collet, and collet is equipped with collet
Entrance and jacket outlet, secondary response section are equipped with circulation tube inlet, and charging section is equipped with circulation pipe outlet, chlorine inlet and acetylene
Gas entrance, gaseous phase section is equipped with feed inlet and gas vent, and when work, tetrachloroethanes is full of chlorination tower, acetylene by feed inlet
Gas enters chlorination tower by acetylene gas entrance, and chlorine enters chlorination tower by chlorine inlet, and acetylene gas and chlorine are in tetrachloroethanes
Negative reaction in liquid phase reacts the heat a part released and provides reaction temperature, and a part of heat is by recirculated water in collet
Interior circulation removes, some removes heat by circulation tube inlet and circulation pipe outlet by tetrachloroethanes, heat dissipation effect
Fruit is good, to improve the purity of product, ensure that the quality of product, improves the yield of tetrachloroethanes.Shortcoming is anti-
Answer temperature difficult to control, fluctuation is big, is not suitable for APC transformation (Advanced process control).
Summary of the invention
The problem to be solved in the present invention is against the above deficiency, to provide that a kind of structure is simple, and operating flexibility is big, heat dissipation effect
It is good, the tetrachloroethanes process units and its method of safety and environmental protection.
In order to solve the above problem, the technical solution adopted by the present invention are as follows: a kind of tetrachloroethanes process units, including reaction
Device, forced circulation heat exchanger, circulating pump, complete condenser, tail condenser, level-one dehydrater and second level dehydrater, the reactor is by certainly
Skirt, first segment cylinder, the second section cylinder, third section cylinder, Section of four cylinder, Section of five cylinder and the 6th of lower and upper arrangement
Cylinder composition is saved, the third section cylinder is provided with the first temperature-measuring port, and Section of four cylinder is provided with the second temperature-measuring port and the
One circulation fluid import, Section of five cylinder are provided with third temperature-measuring port and second circulation liquid import, the gas phase of the reactor
Outlet is connect with the gas phase import of the complete condenser, the import phase of the liquid-phase outlet of the complete condenser and the level-one dehydrater
Even, the outlet of the level-one dehydrater and the liquid-phase outlet of the second level dehydrater are connected in parallel, and the gas phase of the complete condenser goes out
Mouth is connect with the import of the tail condenser, and the liquid-phase outlet of the tail condenser is connect with the import of the second level dehydrater, described
The phegma outlet of second level dehydrater is connected with the phegma import of the reactor, and the reactor bottom is provided with circulation fluid
Outlet, the circulation fluid outlet are connect with the import of the circulating pump, and the outlet of the circulating pump and the forced circulation exchange heat
The import of device is connected, the outlet of the forced circulation heat exchanger and the first circulation liquid import and the second circulation liquid import
Connection.
As the preferred embodiment of the present invention, the internal diameter of the reactor is 1600~2000mm.
As the preferred embodiment of the present invention, the tail condenser is additionally provided with offgas outlet.
As the preferred embodiment of the present invention, it is provided with acetylene air inlet distributor in the first segment cylinder, described
It is provided with chlorine air inlet distributor in two section cylinders, the first screen and the first pressing plate are provided in the third section cylinder, it is described
Section four, it is provided with the second screen and the second pressing plate in cylinder, is provided with third screen and third pressure in Section of five cylinder
Plate, the third section cylinder is provided with the first half-pipe jacket outside, is provided with the second half-pipe jacket outside Section of four cylinder, described
Section five, third half-pipe jacket is provided with outside cylinder.
As the preferred embodiment of the present invention, the air inlet of the acetylene air inlet distributor and chlorine air inlet distribution
The air inlet of device is distributed in the two sides of the reactor, the air inlet of the acetylene air inlet distributor and chlorine air inlet distribution
The vertical drop of the air inlet of device is 500~550mm.
As the preferred embodiment of the present invention, the outlet of the acetylene air inlet distributor and the chlorine air inlet distributor
The quantity in hole is 600~800, and aperture is 3~6mm.
As the preferred embodiment of the present invention, the acetylene air inlet distributor and the chlorine air inlet distributor are coil pipe
Shape.
The present invention also provides the methods for using process units production tetrachloroethanes, comprising the following steps:
(1) acetylene and chlorine are passed through into acetylene air inlet distributor simultaneously respectively and chlorine air inlet distributor is continuously added to react
Device is reacted, and controls reactor upper section by third temperature-measuring port, the second temperature-measuring port and the first temperature-measuring port respectively in reaction process
Reaction temperature is 90~107 DEG C, and middle section reaction temperature is 92~110 DEG C, and lower section reaction temperature is 100~120 DEG C, the second
Alkynes and chlorine molar ratio are 1:1.9-2.1, and acetylene flow is 160-250m3/ h, vacuum degree is 70~90kPa, anti-by what is obtained
Liquid is answered to return to the import of first circulation liquid and second circulation liquid import through circulation fluid outlet, circulating pump, forced circulation heat exchanger, successively
Circulation；
(2) gas-phase product that reaction obtains is entered in complete condenser by the gaseous phase outlet of reactor, is obtained through condensation liquefaction
To liquid phase enter the water removal of level-one dehydrater after obtain product, uncooled gas-phase product is entered by the gaseous phase outlet of complete condenser
Tail condenser；
(3) from complete condenser come uncooled gas-phase product in tail condenser further condensation liquefaction, obtained liquid phase into
Enter after further being removed water in second level dehydrater, a part of liquid phase exports the reflux of reacted device by the phegma of second level dehydrater
Liquid circumfluence enters reactor, and a part of liquid phase continuously produces from the liquid-phase outlet of second level dehydrater and obtains product.
The temperature of the complete condenser is preferably controlled to 20-35 DEG C, and the temperature of the tail condenser is preferably controlled to 15-30 DEG C.
Temperature is affected to the selectivity of reaction, and temperature is higher, and side reaction is more, so as to cause product purity drop
It is low, selecting response rate and yield decline.And conventional carbon steel enamel reactor gas-liquid mass transfer heat-transfer effect is poor, easily cause acetylene and
Chlorine proportion is unstable, and temperature distribution is non-uniform, and side reaction increases, and declines selecting response rate and yield.Tetrachloro of the invention
The third section cylinder of ethane process units is provided with the first temperature-measuring port, and Section of four cylinder is provided with the second temperature-measuring port, Section of five cylinder
Body is provided with third temperature-measuring port, for monitoring each section of reaction temperature of reactor, reaction temperature can be effectively controlled, thus effectively
Reduce the generation of side reaction.Therefore, the temperature difference of reactor upper, middle and lower section is smaller, and reacting balance control ability significantly increases, instead
Answer process more complete, conversion ratio, product purity significantly improve.According to needs of production, tetrachloroethanes of the invention is raw
Produce device can also mating APC control system and SIS system, piecewise acquisition can be carried out to reaction temperature data in production process, can
Each section of reaction temperature of real-time monitoring reactor；Acetylene gas and chlorine are automatically cut off when reaction unit vacuum degree is lower than control amount
Air inlet, and reaction unit cooling system and evacuation system at this time still operate normally, so that it is guaranteed that total system will not superpressure, explosion
Piece will not act, and further increase the gentle self-control of Automated water, and the safely controllable degree of package unit is high.
The reactor bottom of tetrachloroethanes process units of the invention is provided with circulation fluid outlet, and it is strong both to have can be used for mother liquor
System circulation, and can be used for emptying raffinate.Section four, cylinder is additionally provided with first circulation liquid import, and Section of five cylinder is additionally provided with
Second circulation liquid import, the import of first circulation liquid and the import of second circulation liquid are connect with the outlet of forced circulation heat exchanger, so as to
Reaction solution forced circulation is carried out, the cooling effect of reaction solution is improved.
Acetylene air inlet is respectively arranged in the first segment cylinder of tetrachloroethanes process units of the invention and the second section cylinder
Distributor and chlorine air inlet distributor, are sprayed to acetylene gas and chlorine uniformly in reactor with regime flow, in reactor
It is uniformly distributed, acetylene gas and chlorine proportion are stablized, and reacting balance carries out, and improves reacting balance control ability, conversion ratio, product
Purity significantly improves.The quantity of the venthole of acetylene air inlet distributor and chlorine air inlet distributor is both preferably 600~800
A, aperture is both preferably 3~6mm.
The density ratio chlorine of acetylene is small, and the flow velocity of the velocity ratio chlorine of acetylene in the reactor is fast, therefore in the present invention,
Acetylene air inlet distributor is arranged under chlorine air inlet distributor, the air inlet of acetylene air inlet distributor and chlorine air inlet distribution
The vertical height of the air inlet of device is 500~550mm, acetylene gas and chlorine can be made to be uniformly mixed, reaction sufficiently, makes reacting balance
It carries out, further improves the conversion ratio and product purity of reaction.In the present invention, the air inlet and chlorine of acetylene air inlet distributor
The air inlet of air inlet distributor is distributed in the two sides of reactor, convenient to replace in the future.
Grid are provided in the third section cylinder of tetrachloroethanes process units of the invention, Section of four cylinder and Section of five cylinder
Plate and pressing plate, in order to load carbon steel material structured packing between screen and pressing plate, generation when preventing reaction solution forced circulation
It is mobile.Meanwhile it is uniformly distributed acetylene gas and chlorine in reactor, reacting balance control ability is further improved, is converted
Rate, product purity significantly improve.
Half is provided with outside the third section cylinder of tetrachloroethanes process units of the invention, Section of four cylinder and Section of five cylinder
Pipe clamp set, half-pipe jacket are passed through steam heating adjusting to reaction temperature for reacting the incipient stage, and the stage of reaction is passed through recirculated water
Temperature adjusting is carried out, heat in reactor is taken away, temperature needed for maintaining reaction.
The tail condenser of tetrachloroethanes process units of the invention is additionally provided with offgas outlet, and offgas outlet can be with suction unit
Connection extracts out the on-condensible gas in reactor in the HCl gas and raw material of side reaction generation to form negative pressure by suction unit,
Tail gas passes through alkaline calcium carbide clear liquid and absorbs.Suction unit makes reactor be in negative pressure state, can effectively reduce the boiling of tetrachloroethanes
Point reduces reactor and integrally controls temperature, and negative pressure is higher more advantageous to reaction.
Compared with prior art, the present invention having the advantage that
1, structure is simple, and operating flexibility is big, and tetrachloroethanes process units reactor shell diameter of the invention can be according to production
It can be carried out adjustment, design reasonable reactor size and and forced circulation pipeline, pressure by calculating in actual production
Circulation heat exchanger and circulating pump reach optimal reaction effect；Each cylinder of reactor uses flanged joint, is convenient for ordinary maintenance.
2, gas-liquid mass transfer heat-transfer effect is good, and tetrachloroethanes process units of the invention can carry out mother liquor forced circulation, makes anti-
The circulation of liquid is answered to become forced circulation from temperature difference promotion, internal circulating load increases exponentially, and significantly enhances mass-and heat-transfer effect, reactor
Upper, middle and lower section uniformity of temperature profile, reacting balance is controllable, further reduces the generation of side reaction, improves selecting response rate
And yield, product selectivity are 98% or more, reaction yield is 96% or more.
3, reaction process is safely controllable, and the third section cylinder of tetrachloroethanes process units of the invention is additionally provided with the first survey
Warm mouth, Section of four cylinder are additionally provided with the second temperature-measuring port, and Section of five cylinder is additionally provided with third temperature-measuring port, for monitoring reactor
Each section of reaction temperature, reaction temperature can be effectively controlled, to efficiently reduce the generation of side reaction, reactor upper, middle and lower section
The temperature difference fluctuation it is smaller, within ± 3 DEG C, reacting balance control ability significantly increases the temperature difference.
4, it is set respectively in good product quality, the first segment cylinder of tetrachloroethanes process units of the invention and the second section cylinder
It is equipped with acetylene air inlet distributor and chlorine air inlet distributor, acetylene gas and chlorine is made uniformly to be sprayed to reactor with regime flow
It is interior, it is uniformly distributed in reactor, acetylene gas and chlorine proportion are stablized, and reacting balance carries out；Acetylene air inlet distributor is arranged
Under chlorine air inlet distributor, the vertical height of the air inlet of the air inlet and chlorine air inlet distributor of acetylene air inlet distributor
For 500~550mm, acetylene gas and chlorine can be made to be uniformly mixed, reaction sufficiently, carries out reacting balance, further improves anti-
The conversion ratio and product purity answered；It is provided with screen and pressing plate in third section cylinder, Section of four cylinder and Section of five cylinder, so as to
In loading carbon steel material structured packing between screen and pressing plate, prevent from moving when mother liquor forced circulation, and make acetylene gas
It is uniformly distributed in reactor with chlorine, further improves reacting balance control ability, conversion ratio, product purity obviously mention
Height, product purity is 98% or more.
5, the tail condenser of safety and environmental protection, tetrachloroethanes process units of the invention is additionally provided with offgas outlet, offgas outlet
It can be connect with suction unit, the on-condensible gas in HCl gas and raw material for being generated side reaction in reactor by suction unit
Extraction forms negative pressure, and tail gas passes through alkaline calcium carbide clear liquid and absorbs, and suction unit makes reactor be in negative pressure state, can effectively reduce
The boiling point of tetrachloroethanes reduces reactor and integrally controls temperature, improves the security reliability of reaction process；Tetrachloro of the invention
Ethane process units can also mating SIS system and APC control system, chlorine and acetylene gas can be automatically cut off by encountering abnormal conditions
Intake valve, the use of APC control system can reduce the parking of system interlock caused by artificial maloperation factor, greatly improve reaction
The essential safety of device operation, further improves tail gas recycling and reusing after the stability and reaction manipulated in reaction process, saves
Energy, water-saving effect are obvious.
Detailed description of the invention
Fig. 1 is the schematic diagram of tetrachloroethanes process units of the invention；
Fig. 2 is the reactor schematic diagram of tetrachloroethanes process units of the invention.
In figure, 1 is skirt, and 2 be first segment cylinder, and 3 be acetylene air inlet distributor, and 4 be the second section cylinder, 5 for chlorine into
Gas distributor, 6 be third section cylinder, and 7 be Section of four cylinder, and 8 be the import of first circulation liquid, and 9 be Section of five cylinder, and 10 be the
Two circulation fluid imports, 11 be Section of six cylinder, and 12-1 is the first half-pipe jacket, and 12-2 is the second half-pipe jacket, and 12-3 is third
Half-pipe jacket, 13 be third pressing plate, and 14 export for circulation fluid, and 15 be forced circulation heat exchanger, and 16 be circulating pump, and 17 be Quan Ning
Device, 18 be tail condenser, and 19 be level-one dehydrater, and 20 be offgas outlet, and 21 be second level dehydrater, and 22 be the first temperature-measuring port, and 23 are
Second temperature-measuring port, 24 be third temperature-measuring port, and 25 be reactor, and 26 be the first screen, and 27 be the first pressing plate, and 28 be the second screen,
29 be the second pressing plate, and 30 be third screen.
Specific embodiment
As shown, tetrachloroethanes process units of the invention, including reactor 25, forced circulation heat exchanger 15, circulation
Pump 16, complete condenser 17, tail condenser 18, level-one dehydrater 19 and second level dehydrater 21, reactor 25 is by the skirt that arranges from bottom to top
Seat 1, first segment cylinder 2, the second section cylinder 4,6, the 4th sections of cylinders 7 of third section cylinder, Section of five cylinder 9 and Section of six cylinder
11 compositions, third section cylinder are provided with the first temperature-measuring port 22, and Section of four cylinder is provided with the second temperature-measuring port 23 and first circulation liquid
Import 8, Section of five cylinder are provided with third temperature-measuring port 24 and second circulation liquid import 10, the gaseous phase outlet and Quan Ning of reactor 25
The gas phase import of device 17 connects, and the liquid-phase outlet of complete condenser 17 is connected with the import of level-one dehydrater 19, level-one dehydrater 19
Outlet is connect with the liquid-phase outlet of second level dehydrater 21, and the gaseous phase outlet of complete condenser 17 is connect with the import of tail condenser 18, and tail is solidifying
The liquid-phase outlet of device 18 is connect with the import of second level dehydrater 21, the phegma outlet of second level dehydrater 21 and returning for reactor 25
Flow liquid import is connected, and 25 bottom of reactor is provided with circulation fluid outlet 14, and circulation fluid outlet 14 and the import of circulating pump 16 connect
It connects, the outlet of circulating pump 16 is connected with the import of forced circulation heat exchanger 15, and the outlet of forced circulation heat exchanger 15 is followed with first
Ring liquid import 8 and second circulation liquid import 10 connect.Acetylene air inlet distributor 3, the second section cylinder are provided in first segment cylinder 2
It is provided with chlorine air inlet distributor 5 in 4, the first screen 26 and the first pressing plate 27, Section of four cylinder are provided in third section cylinder 6
It is provided with the second screen 28 and the second pressing plate 29 in 7, is provided with third screen 30 and third pressing plate 13 in Section of five cylinder 9, the
Three section cylinders 6 are provided with the first half-pipe jacket 12-1 outside, Section of four cylinder 7 is provided with the second half-pipe jacket 12-2 outside, and Section five
Third half-pipe jacket 12-3 is provided with outside cylinder 9.
Use the process of device production tetrachloroethanes are as follows:
First tetrachloroethanes mother liquor is added in reactor 25 before driving for device；And the first screen 26 and the first pressing plate 27 it
Between, between the second screen 28 and the second pressing plate 29, carbon steel material is regular fills out for filling between third screen 30 and third pressing plate 13
Material, prevents from moving when mother liquor forced circulation.On the one hand carbon steel material structured packing provides phase for gas-liquid two-phase contact mass transfer
Interface, another aspect chlorine react the catalysis that the ferric trichloride generated is chlorine and acetylene reaction with carbon steel material structured packing
Agent.Acetylene is continuously uniformly sprayed in reactor 25 with regime flow by regulating valve control by acetylene air inlet distributor 3, simultaneously
Chlorine is continuously uniformly sprayed in reactor 25 with regime flow by regulating valve control by chlorine air inlet distributor 5, acetylene, chlorine
Gas dissolution, which enters to react under the action of ferric chloride catalyst in tetrachloroethanes mother liquor, generates tetrachloroethanes, reacts main and occurs
At 6 tower section of third section cylinder and acetylene air inlet distributor 3,5 sections of chlorine air inlet distributor, pass through third thermometric in reaction process
Mouthful the 24, second temperature-measuring port 23, the first temperature-measuring port 22 monitors the temperature of 25 upper, middle and lower of reactor section in setting value respectively, can be effective
Reaction temperature is controlled, to reduce the generation of side reaction, the temperature difference fluctuation between the section of reactor upper, middle and lower is small, and Temperature Distribution is equal
Even, reacting balance control ability significantly increases.The heat that reaction generates mainly is shifted by three kinds of modes: tetrachloroethanes vaporization,
First half-pipe jacket 12-1, the second half-pipe jacket 12-2 and third half-pipe jacket 12-3 cooling water temperature force outer circulation cooling.
Obtained gas-phase product is reacted to enter in complete condenser 17 by the gaseous phase outlet of reactor 25, the liquid phase obtained through condensation liquefaction into
Entering level-one dehydrater 19, uncooled gas phase enters the further condensation liquefaction of tail condenser 18 by the gaseous phase outlet of complete condenser 17,
The liquid phase that tail condenser 18 obtains enters in second level dehydrater 21 further remove water after, removed from outlet and the second level of level-one dehydrater 19
The liquid-phase outlet of hydrophone 21 continuously produces and obtains product；Partial Liquid Phase returning by second level dehydrater 21 in second level dehydrater 21
The phegma circumfluence that flow liquid exports reacted device 25 enters in reactor 25, maintains reactor mother liquor amount to play simultaneously certain
Cooling effect；A part of reaction solution is by circulation fluid outlet 14, after circulating pump 16,15 forced heat-exchanging of forced circulation heat exchanger,
Reactor 25, forced circulation and cooling is circulated back to by first circulation liquid import 8 and second circulation liquid import 10 to drop in auxiliary
It is uniformly distributed mother liquor effective flowing catalyst in reactor 25 while warm；By adjusting the first half-pipe jacket 12-1, second
Half-pipe jacket 12-2 and third half-pipe jacket 12-3 water circulation control reactor 25 respectively save the temperature of cylinder.Offgas outlet 20 can
It is connect with suction unit, the on-condensible gas in HCl gas and raw material for being generated side reaction in reactor 25 by suction unit
Negative pressure is formed through the extraction of offgas outlet 20, and is absorbed by alkaline calcium carbide clear liquid, suction unit makes reactor 25 be in negative pressure shape
State can effectively reduce the boiling point of tetrachloroethanes, reduce the whole control temperature of reactor 25, and negative pressure is higher to reacting more advantageous, has
Effect improves the security reliability of reaction process.
The present invention is explained in further detail by the following examples, it should be understood that embodiment described herein
Only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1
A kind of tetrachloroethanes process units, including reactor 25 (internal diameter 1600mm), forced circulation heat exchanger 15, circulation
Pump 16, complete condenser 17, tail condenser 18, level-one dehydrater 19 and second level dehydrater 21, the gaseous phase outlet and complete condenser of reactor 25
17 gas phase import connection, the liquid-phase outlet of complete condenser 17 are connected with the import of level-one dehydrater 19, and level-one dehydrater 19 goes out
Mouth is connect with the liquid-phase outlet of second level dehydrater 21, and the gaseous phase outlet of complete condenser 17 is connect with the import of tail condenser 18, tail condenser
18 liquid-phase outlet is connect with the import of second level dehydrater 21, the reflux of the phegma outlet and reactor 25 of second level dehydrater 21
Liquid import is connected, and 25 bottom of reactor is provided with circulation fluid outlet 14, and circulation fluid outlet 14 connect with the import of circulating pump 16, follows
The outlet of ring pump 16 is connected with the import of forced circulation heat exchanger 15, the outlet of forced circulation heat exchanger 15 and following for reactor 25
Ring liquid import connection.Reactor 25 is by the skirt 1, first segment cylinder 2, the second section cylinder 4, the third section cylinder that arrange from bottom to top
6, Section of four cylinder 7, Section of five cylinder 9 and Section of six cylinder 11 form, and are provided with spirally coiled acetylene air inlet in first segment cylinder 2
Distributor 3 (quantity of venthole is 600, aperture 6mm)；Spirally coiled chlorine air inlet distribution is provided in second section cylinder 4
Device 5 (quantity of venthole is 600, aperture 6mm)；The air inlet of acetylene air inlet distributor 3 and chlorine air inlet distributor 5
Air inlet is distributed in the two sides of reactor 25, the air inlet of the air inlet and chlorine air inlet distributor 5 of acetylene air inlet distributor 3
Vertical drop is 550mm；The first screen 26 and the first pressing plate 27 are provided in third section cylinder 6, third section cylinder 6 is additionally provided with
First temperature-measuring port 22；Section four, the second screen 28 and the second pressing plate 29 are provided in cylinder 7, Section of four cylinder 7 is additionally provided with
One circulation fluid import 8 and the second temperature-measuring port 23；Section five, it is provided with third screen 30 and third pressing plate 13 in cylinder 9, Section five
Cylinder 9 is additionally provided with second circulation liquid import 10 and third temperature-measuring port 24；First circulation liquid import 8 and second circulation liquid import 10
It is connect with the outlet of forced circulation heat exchanger 15；The first half-pipe jacket 12-1, Section of four cylinder 7 are provided with outside third section cylinder 6
It is provided with the second half-pipe jacket 12-2 outside, third half-pipe jacket 12-3 is provided with outside Section of five cylinder 9.Tail condenser 18 is additionally provided with
Offgas outlet 20.
State modulator when producing tetrachloroethanes using the device are as follows: acetylene is 1:2 with chlorine molar ratio, and acetylene flow is
200m3/ h, top reaction temperature are 101 DEG C, and middle part reaction temperature is 105 DEG C, and lower part reaction temperature is 110 DEG C, and vacuum degree is
The temperature control of 76kPa, complete condenser are 25 DEG C, and the temperature control of tail condenser is 20 DEG C.
As a result: reactor upper, middle and lower section temperature is respectively as follows: 100.2-102.4 DEG C, 104.1-106.6 DEG C, 108.5-
111.5 DEG C, uniformity of temperature profile, temperature difference fluctuation is small, and reaction process is steadily controllable, product purity 98.6%, tetrachloroethanes choosing
Selecting property is 99%, reaction yield 97.2%.
Embodiment 2
A kind of tetrachloroethanes process units, including reactor 25 (internal diameter 1800mm), forced circulation heat exchanger 15, circulation
Pump 16, complete condenser 17, tail condenser 18, level-one dehydrater 19 and second level dehydrater 21, the gaseous phase outlet and complete condenser of reactor 25
17 gas phase import connection, the liquid-phase outlet of complete condenser 17 are connected with the import of level-one dehydrater 19, and level-one dehydrater 19 goes out
Mouth is connect with the liquid-phase outlet of second level dehydrater 21, and the gaseous phase outlet of complete condenser 17 is connect with the import of tail condenser 18, tail condenser
18 liquid-phase outlet is connect with the import of second level dehydrater 21, the reflux of the phegma outlet and reactor 25 of second level dehydrater 21
Liquid import is connected, and 25 bottom of reactor is provided with circulation fluid outlet 14, and circulation fluid outlet 14 connect with the import of circulating pump 16, follows
The outlet of ring pump 16 is connected with the import of forced circulation heat exchanger 15, the outlet of forced circulation heat exchanger 15 and following for reactor 25
Ring liquid import connection.Reactor 25 is by the skirt 1, first segment cylinder 2, the second section cylinder 4, the third section cylinder that arrange from bottom to top
6, Section of four cylinder 7, Section of five cylinder 9 and Section of six cylinder 11 form, and are provided with spirally coiled acetylene air inlet in first segment cylinder 2
Distributor 3 (quantity of venthole is 700, aperture 5mm)；Spirally coiled chlorine air inlet distribution is provided in second section cylinder 4
Device 5 (quantity of venthole is 700, aperture 5mm)；The air inlet of acetylene air inlet distributor 3 and chlorine air inlet distributor 5
Air inlet is distributed in the two sides of reactor 25, the air inlet of the air inlet and chlorine air inlet distributor 5 of acetylene air inlet distributor 3
Vertical drop is 530mm；The first screen 26 and the first pressing plate 27 are provided in third section cylinder 6, third section cylinder 6 is additionally provided with
First temperature-measuring port 22；Section four, the second screen 28 and the second pressing plate 29 are provided in cylinder 7, Section of four cylinder 7 is additionally provided with
One circulation fluid import 8 and the second temperature-measuring port 23；Section five, it is provided with third screen 30 and third pressing plate 13 in cylinder 9, Section five
Cylinder 9 is additionally provided with second circulation liquid import 10 and third temperature-measuring port 24；First circulation liquid import 8 and second circulation liquid import 10
It is connect with the outlet of forced circulation heat exchanger 15；The first half-pipe jacket 12-1, Section of four cylinder 7 are provided with outside third section cylinder 6
It is provided with the second half-pipe jacket 12-2 outside, third half-pipe jacket 12-3 is provided with outside Section of five cylinder 9.Tail condenser 18 is additionally provided with
Offgas outlet 20.
State modulator when producing tetrachloroethanes using the device are as follows: acetylene is 1:1.99, acetylene flow with chlorine molar ratio
For 160m3/ h, top reaction temperature are 92 DEG C, and middle part reaction temperature is 95 DEG C, and lower part reaction temperature is 105 DEG C, and vacuum degree is
The temperature control of 90kPa, complete condenser are 35 DEG C, and the temperature control of tail condenser is 30 DEG C.
As a result: reactor upper, middle and lower section temperature is respectively as follows: 90.7-93.4 DEG C, 94.4-96.9 DEG C, 104.8-106.5
DEG C, uniformity of temperature profile, temperature difference fluctuation is small, and reaction process is steadily controllable, product purity 98.6%, and tetrachloroethanes is selectively
99.5%, reaction yield 97.5%.
Embodiment 3
A kind of tetrachloroethanes process units, including reactor 25 (internal diameter 1900mm), forced circulation heat exchanger 15, circulation
Pump 16, complete condenser 17, tail condenser 18, level-one dehydrater 19 and second level dehydrater 21, the gaseous phase outlet and complete condenser of reactor 25
17 gas phase import connection, the liquid-phase outlet of complete condenser 17 are connected with the import of level-one dehydrater 19, and level-one dehydrater 19 goes out
Mouth is connect with the liquid-phase outlet of second level dehydrater 21, and the gaseous phase outlet of complete condenser 17 is connect with the import of tail condenser 18, tail condenser
18 liquid-phase outlet is connect with the import of second level dehydrater 21, the reflux of the phegma outlet and reactor 25 of second level dehydrater 21
Liquid import is connected, and 25 bottom of reactor is provided with circulation fluid outlet 14, and circulation fluid outlet 14 connect with the import of circulating pump 16, follows
The outlet of ring pump 16 is connected with the import of forced circulation heat exchanger 15, the outlet of forced circulation heat exchanger 15 and following for reactor 25
Ring liquid import connection.Reactor 25 is by the skirt 1, first segment cylinder 2, the second section cylinder 4, the third section cylinder that arrange from bottom to top
6, Section of four cylinder 7, Section of five cylinder 9 and Section of six cylinder 11 form, and are provided with spirally coiled acetylene air inlet in first segment cylinder 2
Distributor 3 (quantity of venthole is 750, aperture 4mm)；Spirally coiled chlorine air inlet distribution is provided in second section cylinder 4
Device 5 (quantity of venthole is 750, aperture 4mm)；The air inlet of acetylene air inlet distributor 3 and chlorine air inlet distributor 5
Air inlet is distributed in the two sides of reactor 25, the air inlet of the air inlet and chlorine air inlet distributor 5 of acetylene air inlet distributor 3
Vertical drop is 510mm；The first screen 26 and the first pressing plate 27 are provided in third section cylinder 6, third section cylinder 6 is additionally provided with
First temperature-measuring port 22；Section four, the second screen 28 and the second pressing plate 29 are provided in cylinder 7, Section of four cylinder 7 is additionally provided with
One circulation fluid import 8 and the second temperature-measuring port 23；Section five, it is provided with third screen 30 and third pressing plate 13 in cylinder 9, Section five
Cylinder 9 is additionally provided with second circulation liquid import 10 and third temperature-measuring port 24；First circulation liquid import 8 and second circulation liquid import 10
It is connect with the outlet of forced circulation heat exchanger 15；The first half-pipe jacket 12-1, Section of four cylinder 7 are provided with outside third section cylinder 6
It is provided with the second half-pipe jacket 12-2 outside, third half-pipe jacket 12-3 is provided with outside Section of five cylinder 9.Tail condenser 18 is additionally provided with
Offgas outlet 20.
State modulator when producing tetrachloroethanes using the device are as follows: acetylene is 1:2.01, acetylene flow with chlorine molar ratio
For 250m3/ h, top reaction temperature are 107 DEG C, and middle part reaction temperature is 109 DEG C, and lower part reaction temperature is 118 DEG C, vacuum degree
Temperature control for 88kPa, complete condenser is 20 DEG C, and the temperature control of tail condenser is 15 DEG C.
As a result: reactor upper, middle and lower section temperature is respectively as follows: 106.7-109.3 DEG C, 108.4-111.3 DEG C, 117.1-120
DEG C, uniformity of temperature profile, the temperature difference is small, and reaction process is steadily controllable, product purity 98.2%, and tetrachloroethanes is selectively
98.6%, reaction yield 96.3%.
Embodiment 4
A kind of tetrachloroethanes process units, including reactor 25 (internal diameter 2000mm), forced circulation heat exchanger 15, circulation
Pump 16, complete condenser 17, tail condenser 18, level-one dehydrater 19 and second level dehydrater 21, the gaseous phase outlet and complete condenser of reactor 25
17 gas phase import connection, the liquid-phase outlet of complete condenser 17 are connected with the import of level-one dehydrater 19, and level-one dehydrater 19 goes out
Mouth is connect with the liquid-phase outlet of second level dehydrater 21, and the gaseous phase outlet of complete condenser 17 is connect with the import of tail condenser 18, tail condenser
18 liquid-phase outlet is connect with the import of second level dehydrater 21, the reflux of the phegma outlet and reactor 25 of second level dehydrater 21
Liquid import is connected, and 25 bottom of reactor is provided with circulation fluid outlet 14, and circulation fluid outlet 14 connect with the import of circulating pump 16, follows
The outlet of ring pump 16 is connected with the import of forced circulation heat exchanger 15, the outlet of forced circulation heat exchanger 15 and following for reactor 25
Ring liquid import connection.Reactor 25 is by the skirt 1, first segment cylinder 2, the second section cylinder 4, the third section cylinder that arrange from bottom to top
6, Section of four cylinder 7, Section of five cylinder 9 and Section of six cylinder 11 form, and are provided with spirally coiled acetylene air inlet in first segment cylinder 2
Distributor 3 (quantity of venthole is 800, aperture 3mm)；Spirally coiled chlorine air inlet distribution is provided in second section cylinder 4
Device 5 (quantity of venthole is 800, aperture 3mm)；The air inlet of acetylene air inlet distributor 3 and chlorine air inlet distributor 5
Air inlet is distributed in the two sides of reactor 25, the air inlet of the air inlet and chlorine air inlet distributor 5 of acetylene air inlet distributor 3
Vertical drop is 500mm；The first screen 26 and the first pressing plate 27 are provided in third section cylinder 6, third section cylinder 6 is additionally provided with
First temperature-measuring port 22；Section four, the second screen 28 and the second pressing plate 29 are provided in cylinder 7, Section of four cylinder 7 is additionally provided with
One circulation fluid import 8 and the second temperature-measuring port 23；Section five, it is provided with third screen 30 and third pressing plate 13 in cylinder 9, Section five
Cylinder 9 is additionally provided with second circulation liquid import 10 and third temperature-measuring port 24；First circulation liquid import 8 and second circulation liquid import 10
It is connect with the outlet of forced circulation heat exchanger 15；The first half-pipe jacket 12-1, Section of four cylinder 7 are provided with outside third section cylinder 6
It is provided with the second half-pipe jacket 12-2 outside, third half-pipe jacket 12-3 is provided with outside Section of five cylinder 9.Tail condenser 18 is additionally provided with
Offgas outlet 20.
State modulator when producing tetrachloroethanes using the device are as follows: acetylene is 1:2.03, acetylene flow with chlorine molar ratio
For 180m3/ h, top reaction temperature are 91 DEG C, and middle part reaction temperature is 92 DEG C, and lower part reaction temperature is 100 DEG C, and vacuum degree is
The temperature control of 70kPa, complete condenser are 30 DEG C, and the temperature control of tail condenser is 25 DEG C.
As a result: reactor upper, middle and lower section temperature is respectively as follows: 90-92.8 DEG C, 91.5-94.2 DEG C, 98.6-101.3 DEG C, temperature
Degree is evenly distributed, and the temperature difference is small, and reaction process is steadily controllable, and product purity 98%, tetrachloroethanes is selectively 98.2%, reaction
Yield is 96.1%.
Claims (9)
1. a kind of tetrachloroethanes process units, which is characterized in that including reactor, forced circulation heat exchanger, circulating pump, Quan Ning
Device, tail condenser, level-one dehydrater and second level dehydrater, the reactor is by the skirt, the first segment cylinder, that arrange from bottom to top
Two section cylinders, third section cylinder, Section of four cylinder, Section of five cylinder and Section of six cylinder composition, the third section cylinder setting
There is the first temperature-measuring port, Section of four cylinder is provided with the second temperature-measuring port and first circulation liquid import, and Section of five cylinder is set
It is equipped with third temperature-measuring port and second circulation liquid import, the gas phase import of the gaseous phase outlet of the reactor and the complete condenser connects
Connect, the liquid-phase outlet of the complete condenser is connected with the import of the level-one dehydrater, the outlet of the level-one dehydrater with it is described
The liquid-phase outlet of second level dehydrater is connected in parallel, and the gaseous phase outlet of the complete condenser is connect with the import of the tail condenser, described
The liquid-phase outlet of tail condenser is connect with the import of the second level dehydrater, the outlet of the phegma of the second level dehydrater with it is described anti-
The phegma import of device is answered to be connected, the reactor bottom is provided with circulation fluid outlet, the circulation fluid outlet and the circulation
The import of pump connects, and the outlet of the circulating pump is connected with the import of the forced circulation heat exchanger, the forced circulation heat exchange
The outlet of device is connect with the first circulation liquid import and the second circulation liquid import.
2. tetrachloroethanes process units according to claim 1, which is characterized in that the internal diameter of the reactor be 1600~
2000mm。
3. tetrachloroethanes process units according to claim 1, which is characterized in that the tail condenser is additionally provided with tail gas and goes out
Mouthful.
4. tetrachloroethanes process units according to claim 1, which is characterized in that be provided with second in the first segment cylinder
Alkynes air inlet distributor is provided with chlorine air inlet distributor in the second section cylinder, is provided with first in the third section cylinder
Screen and the first pressing plate are provided with the second screen and the second pressing plate, setting in Section of five cylinder in Section of four cylinder
There are third screen and third pressing plate, the first half-pipe jacket is provided with outside the third section cylinder, is arranged outside Section of four cylinder
There is the second half-pipe jacket, third half-pipe jacket is provided with outside Section of five cylinder.
5. tetrachloroethanes process units according to claim 4, which is characterized in that the air inlet of the acetylene air inlet distributor
The air inlet of mouth and the chlorine air inlet distributor is distributed in the two sides of the reactor, the air inlet of the acetylene air inlet distributor
The vertical drop of the air inlet of mouth and the chlorine air inlet distributor is 500~550mm.
6. tetrachloroethanes process units according to claim 4, which is characterized in that the acetylene air inlet distributor and chlorine
The quantity of the venthole of air inlet distributor is 600~800, and aperture is 3~6mm.
7. tetrachloroethanes process units according to claim 4, which is characterized in that the acetylene air inlet distributor and described
Chlorine air inlet distributor is spirally coiled.
8. using the method for process units production tetrachloroethanes described in claim 1, which comprises the following steps:
(1) simultaneously by acetylene and chlorine pass through acetylene air inlet distributor respectively and chlorine air inlet distributor be continuously added to reactor into
Row reacts, and controls the reaction of reactor upper section by third temperature-measuring port, the second temperature-measuring port and the first temperature-measuring port respectively in reaction process
Temperature is 90~107 DEG C, and middle section reaction temperature is 92~110 DEG C, and lower section reaction temperature is 100~120 DEG C, the acetylene and chlorine
Gas molar ratio is 1:1.9-2.1, and acetylene flow is 160-250m3/ h, vacuum degree are 70~90kPa, and obtained reaction solution is passed through
Circulation fluid outlet, circulating pump, forced circulation heat exchanger return to the import of first circulation liquid and second circulation liquid import, circuit sequentially；
(2) gas-phase product that reaction obtains is entered in complete condenser by the gaseous phase outlet of reactor, is obtained through condensation liquefaction
Liquid phase obtains product after entering the water removal of level-one dehydrater, and uncooled gas-phase product enters tail by the gaseous phase outlet of complete condenser and coagulates
Device；
(3) the uncooled gas-phase product come from complete condenser further condensation liquefaction in tail condenser, obtained liquid phase enter two
After further being removed water in grade dehydrater, a part of liquid phase by the phegma of second level dehydrater export the phegma of reacted device into
Mouth flows back into reactor, and a part of liquid phase continuously produces from the liquid-phase outlet of second level dehydrater and obtains product.
9. the method for production tetrachloroethanes according to claim 8, which is characterized in that the temperature of the complete condenser, which controls, is
20-35 DEG C, the temperature control of the tail condenser is 15-30 DEG C.
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| CN201762265U (en) * | 2010-06-01 | 2011-03-16 | 山东滨化东瑞化工有限责任公司 | Anti-corrosion system device during the production of trichloroethylene |
| CN102267868A (en) * | 2010-06-01 | 2011-12-07 | 滨化集团股份有限公司 | Industrial production apparatus for trichloroethylene |
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