CN106669564B - A kind of chloroacetate reaction kettle system of accident disposal - Google Patents
A kind of chloroacetate reaction kettle system of accident disposal Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1406—Multiple stage absorption
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/363—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by introduction of halogen; by substitution of halogen atoms by other halogen atoms
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B01J2219/00162—Controlling or regulating processes controlling the pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00245—Avoiding undesirable reactions or side-effects
- B01J2219/00256—Leakage
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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Abstract
The invention discloses a kind of chloroacetate reaction kettle system of accident disposal, including production of chloroacetic acid system and anxious switching system, production of chloroacetic acid system uses two-stage tandem chlorination, multistage absorption is carried out to the gas overflowed in main reaction kettle, improves the utilization rate of effecting reaction object and the purity of by-product；After system pressure drastically increases, can automatic switching-over pipeline valve, realize to the direct pressure release of system pressure, the time is short efficient；And, in order to further increase the collection of by-product, system normal reaction superpressure, when pressure value is 0.05~0.07Mpa, pressure in main reaction kettle is set directly to leak into tail gas absorbing system, when improper superpressure in system, when pressure value is more than 0.07Mpa, gas in two reaction kettles is quickly discharged into accident tail gas absorbing system by vacuum pump, realizes to the direct pressure release of pressure source, effectively avoids accident.
Description
Technical field
The present invention relates to production of chloroacetic acid field more particularly to a kind of chloroacetate reaction kettle system of accident disposal.
Background technology
Monoxone is a kind of important organic chemical industry's intermediate, is widely used in medicine, pesticide, dyestuff and a variety of organic chemistry
In production.With the progress and development of science and technology, the new application field of monoxone will be developed gradually, monoxone life
Production is very good with market prospects.
Currently, industrialized production method mainly has trichloro ethylene Hydrolyze method, chloracetyl chloride method and acetic acid catalysis
Three kinds of chloridising.And trichloro ethylene Hydrolyze method and chloracetyl chloride method be since raw material sources are limited and cost is higher, thus it is equal in China
Be not applied, using it is most be Catalytic Chlorination of acetic acid method.
Catalyst used in Catalytic Chlorination of acetic acid method mainly has iodine, red phosphorus, sulfonic acid chloride, Cosan, sulfuric acid, chlorosulfonic acid, three
Phosphorus chloride and acetic anhydride etc..Wherein, using acetic acid as raw material, catalyst is made with sulphur, chlorine is passed through in acetic acid, carry out chlorination,
Chlorated liquid by crystallization and rejection filter obtains chloroethene acid product, the method is commonly used at home now, be produce at present it is chloroacetic
The advantages of main method, this production method is that raw acetic acid is in liberal supply, and simple production process is easy, and investment of production is few.
When being reacted due to Catalytic Chlorination of acetic acid, the temperature of reaction kettle is higher, at 70~110 DEG C, have part not with acetic acid
The spillings such as chlorine, acetic acid vapor and the side reaction product hydrogen chloride gas of reaction, in order to improve effective raw material utilization rate and
The purity of by-product hydrochloric acid, so condenser is arranged in the gas outlet of reaction kettle, so that chlorine and acetic acid vapor to be condensed into
Liquid and being back in reaction kettle utilizes again.But chilled brine is generally in condenser, chilled brine after condenser damage
It flow in reaction kettle, the ammonia in brine in acid condition, reacts with chlorine and generates agene, exothermic heat of reaction, reaction kettle
Temperature drastically increases, and traditional jacket reactor cannot timely and effectively pass the heat that reaction generates, and make entirely to react
System overpressure can cause to explode if cannot release the pressure in reaction kettle in time.It is made in condenser damage or other factors
After being increased rapidly at reactor pressure, put on biochemical defence suit enters scene to staff's needs at the first time, by exhaust emissions valve
It is closed with chlorine regulating valve, opens the emergency episode drain valve in parallel with exhaust relief valve, system pipeline is carried out to vacuumize place
Reason reduces system pressure.But once there is more urgent serious situation, personnel will be unable to enter scene, can cause great
Casualties and property loss.
Invention content
Technical problem to be solved by the invention is to provide a kind of security contexts of chloroacetate reaction, work as reacting kettle inner pressure
When raising, energy automatic switching-over pipeline valve realizes a kind of chloroacetate reaction for effectively avoiding accident to occur to pressure release in reaction kettle
Kettle system of accident disposal.
In order to solve the above technical problems, the technical solution used in the present invention is：
A kind of chloroacetate reaction kettle system of accident disposal, including production of chloroacetic acid system, it is characterised in that：Further include
Emergent switching system；The production of chloroacetic acid system includes reaction main still, the secondary kettle of reaction, level-one condensing circuit, B-grade condensation time
Road and three-level condensing circuit；The entrance of the reaction main still, which connects, oriented is passed through the first of chlorine inside it into chlorine pipe；Described one
Grade condensing circuit includes the first condenser, and the gas overflowed from the reaction main still gas outlet enters the first condenser, through first
The liquid reflux that condenser is condensed into enters into reaction main still, forms level-one condensing circuit；The B-grade condensation circuit includes the
Two condensers, the gas overflowed from the first condenser gas outlet, which enters in the secondary kettle of reaction, to react, and is overflowed from reaction secondary kettle gas outlet
Gas enter the second condenser, the liquid reflux condensed through the second condenser, which enters, to be formed B-grade condensation in the secondary kettle of reaction and returns
Road；The three-level condensing circuit includes third condenser, and the gas overflowed from the second condenser gas outlet enters third condenser
Interior, the liquid reflux condensed through third condenser enters to react in main still, forms three-level condensing circuit；From third condenser gas outlet
The gas of spilling enters tail gas absorbing system；First condenser with react secondary kettle, the second condenser and third condenser with
And third condenser is equipped with switch valve with reacting on connecting line between main still；The emergent switching system includes emergent
Pipeline and controller；The gas outlet of emergency line connection reaction main still, on emergency line at the gas outlet of reaction main still
Equipped with the first emergent bleeder valve, the gas outlet of the secondary kettle of reaction is parallel to emergency line, and reacts the gas outlet of secondary kettle and answer
Pipeline between anxious pipeline is equipped with the second emergent bleeder valve；The outlet of the emergency line separates two branches in parallel,
In branch road be equipped with superpressure drain valve, and the branch way outlet be connected to tail gas absorbing system, and another branch road is equipped with pumping
Vacuum valve and vacuum pump, and the branch way outlet is connected to accident tail gas absorbing system；Third condenser gas outlet and tail gas
The first solenoid valve is equipped between absorption system；Described first is equipped with second solenoid valve into chlorine pipe；The reaction main still is equipped with
Detect the first pressure sensor of its internal pressure；The signal of the signal input part connection first pressure sensor of the controller
The control output end of output end, controller is separately connected the first solenoid valve, second solenoid valve, the first emergent bleeder valve, superpressure row
Put valve, vacuum pumping valve and vacuum pump.
Further technical solution is：The entrance of the secondary kettle of reaction connect it is oriented be passed through inside it the second of chlorine into
Chlorine pipe；The gas outlet of second condenser is also connected to the bottom for reacting main still inner cavity, is overflowed from the second condenser gas outlet
Gas enter reaction main still in reaction；The gas outlet of first condenser is connect with the air inlet of third condenser, from
The gas that one condenser gas outlet is overflowed enters in third condenser, and the condensation outlet end of third condenser connects with secondary kettle is reacted
Logical, the liquid reflux condensed through third condenser enters in the secondary kettle of reaction；Second condenser with react main still, first condensation
Device and third condenser and third condenser are equipped with switch valve with reacting on connecting line between main still；Described second
It is equipped with third solenoid valve into chlorine pipe；The secondary kettle of reaction is equipped with the second pressure sensor for detecting its internal pressure；It is described
The signal input part of controller is also connected with the signal output end of second pressure sensor, and the control output end of controller is also connected with
Two emergent bleeder valves.
Further technical solution is：The end of the emergency line is equipped with pressure sensor, the pressure sensor
Signal output end connection controller signal input part, the control output end of the controller connects warning device.
Further technical solution is：The warning device is audible-visual annunciator.
Further technical solution is：The reaction main still or the secondary kettle side of reaction are popped one's head in equipped with chlorine leak detection,
The signal input part of the signal output end connection controller of the chlorine leak detection probe.
It is using advantageous effect caused by above-mentioned technical proposal：
Using two-stage tandem chlorination, multistage absorption is carried out to the gas overflowed in main reaction kettle, improves effecting reaction object
Utilization rate and by-product purity；
After system pressure drastically increases, can automatic switching-over pipeline valve, realize to the direct pressure release of system pressure, time
It is short efficient；Also, in order to further increase the collection of by-product, when system normal reaction superpressure (0.05~0.07Mpa), make
Pressure directly leaks into tail gas absorbing system in main reaction kettle, and as improper superpressure (more than 0.07Mpa) in system, two anti-
It answers the gas in kettle to be quickly discharged into accident tail gas absorbing system by vacuum pump, realizes to the direct pressure release of pressure source, effectively avoid
Accident occurs.
Description of the drawings
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the structural schematic diagram of the present invention；
Fig. 2 is another structural schematic diagram of the present invention.
Specific implementation mode
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground describes, it is clear that described embodiment is only a part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, the every other implementation that those skilled in the art are obtained without making creative work
Example, shall fall within the protection scope of the present invention.
Many details are elaborated in the following description to facilitate a thorough understanding of the present invention, still the present invention can be with
Implemented different from other manner described here using other, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by following public specific embodiment.
Embodiment 1
As shown in Figure 1, a kind of chloroacetate reaction kettle system of accident disposal, including production of chloroacetic acid system, further include
Emergent switching system；The production of chloroacetic acid system is cold including reaction main still 10, the secondary kettle 20 of reaction, level-one condensing circuit, two level
Solidifying circuit and three-level condensing circuit.
It is used as main reaction kettle in reaction main still 10, and reacts the gas that secondary kettle 20 is connected in series, is overflowed from reaction main still 10
Body passes through the reflux of level-one condensing circuit, the absorption of reaction 20 assisted reaction of secondary kettle, the reflux of B-grade condensation circuit and three-level condensation successively
Circuit is flowed back, to carry out the recycling of effecting reaction object.
Specific equipment connection and reaction are as follows：
The entrance of the reaction main still 10 connect it is oriented the first of chlorine is passed through inside it into chlorine pipe 11, and react main still 10
Inside fill acetic acid and catalyst sulphur, under the catalytic action of high temperature and sulphur chlorine and acetic acidreaction generate product monoxone and
Byproduct hydrogen chloride；Since the temperature of reaction main still 10 is at 70~110 DEG C, so having gas (hydrogen chloride 54%, sulfur dioxide
0.2%, chlorine 32% and acetic acid vapor 13% and other gases 0.8%) it overflows；
The level-one condensing circuit includes the first condenser 30, and the gas overflowed from 10 gas outlet of the reaction main still enters
First condenser 30, the liquid being condensed into through the first condenser 30 (liquid chlorine and acetic acid) are passed back into reaction main still 10, are formed
Level-one condensing circuit；
The B-grade condensation circuit includes the second condenser 40, the gas (chlorination overflowed from 30 gas outlet of the first condenser
Hydrogen, sulfur dioxide, chlorine and acetic acid vapor etc.) enter reaction in the secondary kettle 20 of reaction, react equally filled in secondary kettle 20 acetic acid and
Catalyst sulphur, and react secondary kettle and be in keeping warm mode, so reaction pair kettle 20 can absorb a part of chlorine and acetic acid vapor,
The gas (hydrogen chloride, sulfur dioxide, chlorine and acetic acid vapor etc.) overflowed from 20 gas outlet of the secondary kettle of reaction enters the second condenser
40, the liquid (liquid chlorine and acetic acid) condensed through the second condenser 40 flows back into formation B-grade condensation circuit in the secondary kettle 20 of reaction；
The three-level condensing circuit includes third condenser 50, the gas (chlorination overflowed from 40 gas outlet of the second condenser
Hydrogen, sulfur dioxide, chlorine and acetic acid vapor etc.) enter in third condenser 50, the liquid (liquid chlorine condensed through third condenser 50
And acetic acid) pass back into reaction main still 10, form three-level condensing circuit；
Gas (hydrogen chloride 96%, acetic acid 3%, the sulfur dioxide 0.2% and other overflowed from 50 gas outlet of third condenser
Gas 0.8%) enter tail gas absorbing system；
From reaction main still 10 available gas (chlorine and acetic acid vapor) that overflows by 30 condensing reflux of the first condenser,
20 reactive absorption of the secondary kettle of reaction, 50 condensing reflux of 40 condensing reflux of the second condenser and third condenser.By using two level string
Join chlorination, multistage absorption is carried out to the gas overflowed in reaction main still 10, improves the utilization rate of effecting reaction object.
Since tail gas absorbing system is using the absorption of the hydrochloric acid progress hydrogen chloride gas of low concentration, when the concentration of hydrochloric acid reaches
It carries out extraction after 31% to sell, the gas by the absorption by Hydrochloric Acid of low concentration is mainly hydrogen chloride, improves the purity of by-product.
First condenser 30 with react secondary kettle 20, the second condenser 40 and third condenser 50 and third condenser
50 are equipped with switch valve with reacting on connecting line between main still 10, and above-mentioned switch valve is kept open,
Then above-mentioned reaction can carry out.
In order to detect the pressure change in reaction main still 10, and made accordingly according to the pressure value in detection reaction main still 10
The switching of pressure relief pipe, emergent switching system include emergency line 70 and controller.
Specific structure and handover operation are as follows：
The gas outlet of the connection reaction main still 10 of the emergency line 70, in the gas outlet of reaction main still 10 on emergency line 70
Place is equipped with the first emergent bleeder valve 73, and the gas outlet of the reaction pair kettle 20 is parallel to emergency line 70, and reacts secondary kettle 20
Pipeline between gas outlet and emergency line 70 is equipped with the second emergent bleeder valve 74；The outlet of the emergency line 70 separates two
The branch of item parallel connection, wherein a branch road is equipped with superpressure drain valve 71, and the branch way outlet is connected to tail gas absorbing system, separately
One branch road is equipped with vacuum pumping valve 72 and vacuum pump 75, and the branch way outlet is connected to accident tail gas absorbing system；
The first solenoid valve 51 is equipped between 50 gas outlet of third condenser and tail gas absorbing system；
Described first is equipped with second solenoid valve 13 into chlorine pipe 11；
The reaction main still 10 is equipped with the first pressure sensor 12 for detecting its internal pressure；
The signal output end of the signal input part connection first pressure sensor 12 of the controller, the control of controller are defeated
Outlet is separately connected the first solenoid valve 51, second solenoid valve 13, the first emergent bleeder valve 73, superpressure drain valve 71, vacuum pumping valve
72 and vacuum pump 75.
In production of chloroacetic acid system normal reaction, the first solenoid valve 51 and second solenoid valve 13 are in normally open, the
One emergent bleeder valve 73, the second emergent bleeder valve 74, superpressure drain valve 71, vacuum pumping valve 72 and vacuum pump 75 are in normally closed shape
State.
Pressure in the main still 10 of detection reaction in real time of first pressure sensor 12.When production of chloroacetic acid system normal reaction,
It is 0.03~0.05Mpa (not including 0.05Mpa) to react the pressure value in main still 10；When reaction is normal super in reaction main still 10
Pressure, pressure value is in 0.05~0.07Mpa；And when the first condenser 30 or third condenser 50 damage, chilled brine flow to reaction
In main still 10, or when the second condenser 40 damages, chilled brine is flow in reaction pair kettle 20, can all cause the ammonia in brine and chlorine
Gas reacts drastically heat release in acid condition, since traditional jacket reactor cannot timely and effectively pass the heat that reaction generates
It passs away, entire reacting system pressure is caused drastically to increase, pressure value is more than 0.07Mpa.First pressure sensor 12 will detect
To reaction main still 10 in pressure value be transferred to controller, controller is PLC controller.When the pressure value be 0.03~
When 0.05Mpa (not including 0.05Mpa), controller does not make any control operation；When the pressure value is in 0.05~0.07Mpa
When, controller controls second solenoid valve 13 and closes, and the first emergent bleeder valve 73 and superpressure drain valve 71 are opened, and are reacted in main still 10
Pressure be directly discharged into tail gas absorbing system, be no longer flow through other pipelines, when reaction main still 10 in pressure value drop to 0.05Mpa
When following, controller controls second solenoid valve 13 and opens, and the first emergent bleeder valve 73 and superpressure drain valve 71 are closed, and system is restored
Normal operating conditions；And when the pressure value is more than 0.07Mpa, controller controls the first solenoid valve 51 and second solenoid valve 13 is closed
It closes, the first emergent bleeder valve 73, the second emergent bleeder valve 74, vacuum pumping valve 72 and vacuum pump 75 are opened, and are reacted in main still 10
Pressure is quickly pumped into accident tail gas absorbing system by vacuum pump 75, and system is avoided to explode, until system pressure is near
0.03Mpa is hereinafter, staff enters maintenance or replaces the condenser of damage.
The present invention system pressure raising after, can automatic switching-over pipeline valve, realization system pressure source is directly let out
Pressure, time are short efficient；Also, in order to further increase the collection of by-product, 10 normal reaction superpressure of reaction main still (0.05~
When 0.07Mpa), pressure in reaction main still 10 is made directly to leak into tail gas absorbing system, when improper superpressure (is more than in system
When 0.07Mpa), the gas in two reaction kettles is quickly discharged into accident tail gas absorbing system by vacuum pump, realizes to pressure source
Direct pressure release, effectively avoids accident.
Also, the reaction main still 10 or 20 side of the secondary kettle of reaction are equipped with chlorine leak detection probe 80, and the chlorine is let out
The signal input part of the signal output end connection controller of leak detection probe 80.When pipeline breaks down, valve or flange failure,
When there is chlorine leakage, chlorine leak detection probe 80 detects chlorine, transmits the signal to controller, controller control the
One solenoid valve 51 and second solenoid valve 13 are closed, the first emergent bleeder valve 73, the second emergent bleeder valve 74, vacuum pumping valve 72 and true
Sky pump 75 is opened, and the pernicious gas (chlorine) in system is pumped, so that later stage worker enters repair, effectively avoids accident
And reduce personnel's injury.
Embodiment 2
As shown in Fig. 2, increasing on the architecture basics of embodiment 1 with lower structure, to complete reaction in reaction main still 10
Afterwards, do not have to stop production, but the secondary kettle 20 of reaction is utilized to be used as main reaction kettle, during to the reaction pair heating of kettle 20, will react
Feed liquid backward walking in main still 10 is kept the temperature after acetic acid and catalyst sulphur are then added again into reaction main still 10.It makes full use of
Time improves working efficiency.
Specifically structure is：
The entrance of the secondary kettle of the reaction 20, which connects, oriented is passed through the second of chlorine inside it into chlorine pipe 21；
The gas outlet of second condenser 40 is also connected to the bottom for reacting 10 inner cavity of main still, is gone out from the second condenser 40
The gas that gas port overflows enters reaction in reaction main still 10；
The gas outlet of first condenser 30 is connect with the air inlet of third condenser 50, from 30 outlet of the first condenser
Mouthful gas overflowed enters in third condenser 50, the condensation outlet end of third condenser 50 and react the pair connection of kettle 20, through the
The liquid reflux of three condensers 50 condensation enters in reaction pair kettle 20；
Second condenser 40 with react main still 10, the first condenser 30 and third condenser 50 and third condenser
50 are equipped with switch valve with reacting on connecting line between main still 10.
After reacting main still 10 and completing reaction, heat up to the secondary kettle 20 of reaction, using the secondary kettle 20 of reaction as when main reaction kettle,
By in embodiment 1 first condenser 30 with react secondary kettle 20, the second condenser 40 and third condenser 50 and third
Condenser 50 is turned off with the switch valve reacted on connecting line between main still 10.And by the second condenser 40 with react
Main still 10, the first condenser 30 and third condenser 50 and third condenser 50 with react connecting line between main still 10
Switch valve is opened.
The secondary kettle 20 of reaction is used as main reaction kettle, and reacts the gas that main still 20 is connected in series, is overflowed from reaction pair kettle 20
Pass through 40 condensing reflux of the second condenser successively, reaction 10 assisted reaction of main still absorbs, 30 condensing reflux of the first condenser and the
Three condensers, 50 condensing reflux.
Specific reaction is as follows：
Acetic acid and catalyst sulphur are filled in reaction pair kettle 10, chlorine and acetic acid are anti-under the catalytic action of high temperature and sulphur
Product monoxone and byproduct hydrogen chloride should be generated；Since the temperature of reaction pair kettle 20 is at 70~110 DEG C, so having gas
(hydrogen chloride 60%, sulfur dioxide 0.2%, chlorine 32% and acetic acid vapor 7% and other gases 0.8%) overflows；
The gas overflowed from 20 gas outlet of the secondary kettle of reaction enters the second condenser 40, is condensed into through the second condenser 40
Liquid (liquid chlorine and acetic acid) pass back into the secondary kettle of reaction 20；
The gas (hydrogen chloride, sulfur dioxide, chlorine and acetic acid vapor etc.) overflowed from 40 gas outlet of the second condenser enters
Reaction in main still 10 is reacted, reaction main still 10 is in keeping warm mode, so reaction main still 10 can absorb a part of chlorine and second
Acid vapour, the gas (hydrogen chloride, sulfur dioxide, chlorine and acetic acid vapor etc.) overflowed from 10 gas outlet of reaction main still enter first
Condenser 30, the liquid (liquid chlorine and acetic acid) condensed through the first condenser 30 flow back into reaction main still 10；
The gas (hydrogen chloride, sulfur dioxide, chlorine and acetic acid vapor etc.) overflowed from 30 gas outlet of the first condenser enters
In third condenser 50, the liquid (liquid chlorine and acetic acid) condensed through third condenser 50 passes back into reaction pair kettle 20；
Gas (hydrogen chloride 96%, acetic acid 3%, the sulfur dioxide 0.2% and other overflowed from 50 gas outlet of third condenser
Gas 0.8%) enter tail gas absorbing system.
The available gas (chlorine and acetic acid vapor) overflowed from reaction pair kettle 20 passes through the second condenser 40 and condenses successively
Reflux, the absorption of reaction 10 assisted reaction of main still, 50 condensing reflux of 30 condensing reflux of the first condenser and third condenser.By adopting
With two-stage tandem chlorination, secondary kettle 20 is reacted during being used as the use of pair kettle before, has absorbed part chlorine, shortening can
This divides the reaction time.By carrying out multistage absorption to the gas overflowed in the secondary kettle of reaction 20, the profit of effecting reaction object is improved
With rate and the purity of by-product.And after reaction main still 10 completes reaction, do not have to stop production, but directly to the secondary kettle of reaction 20
Heating shortens the time, improves working efficiency using the secondary kettle 20 of reaction as main reaction kettle.
In order to detect the pressure change in reaction pair kettle 20, and the pressure value in secondary kettle 20 is reacted according to detection and is made accordingly
The switching of pressure relief pipe, emergent switching system also increase on the basis of embodiment 1 with lower structure:
Described second is equipped with third solenoid valve 23 into chlorine pipe 21；
The secondary kettle 20 of reaction is equipped with the second pressure sensor 22 for detecting its internal pressure；
The signal input part of the controller is also connected with the signal output end of second pressure sensor 22, the control of controller
Output end is also connected with the second emergent bleeder valve 74.
In the secondary conduct of the kettle 20 main reaction kettle of reaction, production of chloroacetic acid system normal operation, the first solenoid valve 51 and third
Solenoid valve 23 is in normally open, second solenoid valve 13, the first emergent bleeder valve 73, the second emergent bleeder valve 74, superpressure discharge
Valve 71, vacuum pumping valve 72 and vacuum pump 75 are in normally off.
The specific handover operation of emergent switching system is as follows：
Pressure in the pair of detection reaction in real time of second pressure sensor 22 kettle 20.When production of chloroacetic acid system normal reaction,
Pressure value in reaction pair kettle 20 is 0.03~0.05Mpa (not including 0.05Mpa)；When reaction is normal super in the secondary kettle 20 of reaction
Pressure, pressure value is in 0.05~0.07Mpa；And when the first condenser 30 or third condenser 50 damage, chilled brine flow to reaction
In main still 10, or when the second condenser 40 damages, chilled brine is flow in reaction pair kettle 20, can all cause the ammonia in brine and chlorine
Gas reacts drastically heat release in acid condition, since traditional jacket reactor cannot timely and effectively pass the heat that reaction generates
It passs away, entire reacting system pressure is caused drastically to increase, pressure value is more than 0.07Mpa.Second pressure sensor 22 will detect
To the secondary kettle of reaction 20 in pressure value be transferred to controller, controller is PLC controller.When the pressure value be 0.03~
When 0.05Mpa (not including 0.05Mpa), controller does not make any control operation；When the pressure value is in 0.05~0.07Mpa
When, controller controls third solenoid valve 23 and closes, and the second emergent bleeder valve 74 and superpressure drain valve 71 are opened, and reacts in secondary kettle 20
Pressure be directly discharged into tail gas absorbing system, other pipelines are no longer flow through, when the pressure value in the secondary kettle of reaction 20 drops to 0.05Mpa
When following, controller controls third solenoid valve 23 and opens, and the second emergent bleeder valve 74 and superpressure drain valve 71 are closed, and system is restored
Normal operating conditions；And when the pressure value is more than 0.07Mpa, controller controls the first solenoid valve 51 and third solenoid valve 23 closes
It closes, the first emergent bleeder valve 73,74 vacuum pumping valve 72 of the second emergent bleeder valve and vacuum pump 75 are opened, and the pressure in secondary kettle 20 is reacted
Power is quickly pumped into accident tail gas absorbing system by vacuum pump 75, and system is avoided to explode, until system pressure is near
0.03Mpa is hereinafter, staff enters maintenance or replaces the condenser of damage.
The present invention system pressure raising after, can automatic switching-over pipeline valve, realization system pressure source is directly let out
Pressure, time are short efficient；Also, in order to further increase the collection of by-product, react 20 normal reaction superpressure of secondary kettle (0.05~
When 0.07Mpa), pressure in reaction pair kettle 20 is made directly to leak into tail gas absorbing system, when improper superpressure (is more than in system
When 0.07Mpa), the gas in two reaction kettles is quickly discharged into accident tail gas absorbing system by vacuum pump, realizes to pressure source
Direct pressure release, effectively avoids accident.
When there is chlorine leakage, chlorine leak detection probe 80 detects chlorine, transmits the signal to controller, controls
Device processed also controls third solenoid valve 23 and closes in addition to the valve that control switches in embodiment 1.
Embodiment 3
Difference from Example 1 is that the end of the emergency line 70 is equipped with pressure sensor 76, and the pressure passes
The signal input part of the signal output end connection controller of sensor 76, the control output end of the controller connects warning device.
When production of chloroacetic acid system just produces reaction, the first emergent bleeder valve 73 should be at closed state, and pressure sensor 76 can be examined
It surveys whether the first emergent bleeder valve 73 closes tightly, avoids reaction gas from being directly discharged from emergency line 70, cause wastage of material.When
When the pressure value that pressure sensor 76 is transferred to controller is more than 0, illustrate there is gas to pass through in emergency line 70, controller will
Alarm activation is controlled, warning the first emergent bleeder valve 73 of staff couple repairs.Wherein, warning device is acousto-optic report
Alert device.
Embodiment 4
Difference from Example 2 is that the end of the emergency line 70 is equipped with pressure sensor 76, and the pressure passes
The signal input part of the signal output end connection controller of sensor 76, the control output end of the controller connects warning device.
When production of chloroacetic acid system just produces reaction, the first emergent bleeder valve 73 and the second emergent bleeder valve 74 should be at closed state,
Pressure sensor 76 can detect the first emergent bleeder valve 73 and whether the second emergent bleeder valve 74 closes tightly, avoid reaction gas
It is directly discharged from emergency line 70, causes wastage of material.When the pressure value that pressure sensor 76 is transferred to controller is more than 0,
Illustrate there is gas to pass through in emergency line 70, controller will control alarm activation, and warning staff couple first is emergent
Bleeder valve 73 and the second emergent bleeder valve 74 repair.
Wherein, warning device is audible-visual annunciator.
It the above is only presently preferred embodiments of the present invention, anyone content according to the present invention makes the present invention a little
Simple modification, deformation and equivalent replacement each fall within protection scope of the present invention.
Claims (5)
1. a kind of chloroacetate reaction kettle system of accident disposal, including production of chloroacetic acid system, it is characterised in that：Further include answering
Anxious switching system；
The production of chloroacetic acid system includes reaction main still (10), the secondary kettle (20) of reaction, level-one condensing circuit, B-grade condensation circuit
With three-level condensing circuit；
The entrance of the reaction main still (10), which connects, oriented is passed through the first of chlorine inside it into chlorine pipe (11)；
The level-one condensing circuit includes the first condenser (30), and the gas overflowed from described reaction main still (10) gas outlet enters
First condenser (30), the liquid reflux being condensed into through the first condenser (30) enter into reaction main still (10), and it is cold to form level-one
Solidifying circuit；
The B-grade condensation circuit includes the second condenser (40), and the gas overflowed from the first condenser (30) gas outlet enters anti-
Reaction in secondary kettle (20) is answered, the gas overflowed from secondary kettle (20) gas outlet of reaction enters the second condenser (40), through the second condensation
The liquid reflux of device (40) condensation, which enters in the secondary kettle (20) of reaction, forms B-grade condensation circuit；
The three-level condensing circuit includes third condenser (50), and the gas overflowed from the second condenser (40) gas outlet enters the
In three condensers (50), the liquid reflux condensed through third condenser (50) enters to react in main still (10), forms three-level and is condensed back to
Road；
The gas overflowed from third condenser (50) gas outlet enters tail gas absorbing system；
First condenser (30) with to react secondary kettle (20), the second condenser (40) and third condenser (50) and third cold
Condenser (50) is equipped with switch valve with reacting on connecting line between main still (10)；
The emergent switching system includes emergency line (70) and controller；
The gas outlet of main still (10) is reacted in emergency line (70) connection, is reacting going out for main still (10) on emergency line (70)
The first emergent bleeder valve (73) is equipped at gas port, the gas outlet of the secondary kettle (20) of reaction is parallel to emergency line (70), and anti-
The pipeline between the gas outlet of secondary kettle (20) and emergency line (70) is answered to be equipped with the second emergent bleeder valve (74)；The emergent pipe
The outlet on road (70) separates two branches in parallel, wherein a branch road is equipped with superpressure drain valve (71), and the branch way outlet
It is connected to tail gas absorbing system, another branch road is equipped with vacuum pumping valve (72) and vacuum pump (75), and the branch way outlet and thing
Therefore tail gas absorbing system is connected to；
The third condenser (50) is equipped with the first solenoid valve (51) between gas outlet and tail gas absorbing system；
Described first is equipped with second solenoid valve (13) into chlorine pipe (11)；
The reaction main still (10) is equipped with the first pressure sensor (12) for detecting its internal pressure；
The signal output end of the signal input part connection first pressure sensor (12) of the controller, the control output of controller
End is separately connected the first solenoid valve (51), second solenoid valve (13), the first emergent bleeder valve (73), superpressure drain valve (71), takes out
Vacuum valve (72) and vacuum pump (75).
2. a kind of chloroacetate reaction kettle system of accident disposal according to claim 1, it is characterised in that：The reaction
The entrance of secondary kettle (20), which connects, oriented is passed through the second of chlorine inside it into chlorine pipe (21)；
The gas outlet of second condenser (40) is also connected to the bottom for reacting main still (10) inner cavity, from the second condenser (40)
The gas that gas outlet is overflowed enters reaction in reaction main still (10)；
The gas outlet of first condenser (30) is connect with the air inlet of third condenser (50), is gone out from the first condenser (30)
The gas that gas port overflows enters in third condenser (50), and the condensation outlet end of third condenser (50) connects with secondary kettle (20) is reacted
Logical, the liquid reflux condensed through third condenser (50) enters in the secondary kettle (20) of reaction；
Second condenser (40) with to react main still (10), the first condenser (30) and third condenser (50) and third cold
Condenser (50) is equipped with switch valve with reacting on connecting line between main still (10)；
Described second is equipped with third solenoid valve (23) into chlorine pipe (21)；
The secondary kettle (20) of reaction is equipped with the second pressure sensor (22) for detecting its internal pressure；
The signal input part of the controller is also connected with the signal output end of second pressure sensor (22), and the control of controller is defeated
Outlet is also connected with the second emergent bleeder valve (74).
3. a kind of chloroacetate reaction kettle system of accident disposal according to claim 1 or 2, it is characterised in that：It is described
The end of emergency line (70) is equipped with pressure sensor (76), and the signal output end of the pressure sensor (76) connects controller
Signal input part, the control output end of the controller connects warning device.
4. a kind of chloroacetate reaction kettle system of accident disposal according to claim 3, it is characterised in that：The alarm
Device is audible-visual annunciator.
5. a kind of chloroacetate reaction kettle system of accident disposal according to claim 1, it is characterised in that：The reaction
Main still (10) or secondary kettle (20) side of reaction are equipped with chlorine leak detection and pop one's head in (80), the chlorine leak detection probe (80)
Signal output end connects the signal input part of controller.
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| CN107670629B (en) * | 2017-11-09 | 2023-08-22 | 大丰鑫源达化工有限公司 | Device for separating salt from acid gas by utilizing tail gas |
| CN108043350B (en) * | 2017-12-13 | 2020-09-29 | 惠州市固德尔合成材料有限公司 | Reation kettle that fully has flaw detection of reaction |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN201610417U (en) * | 2009-12-25 | 2010-10-20 | 潍坊中业油脂有限公司 | Chlorination reaction device for chloroactic acid production |
| CN206587734U (en) * | 2017-03-21 | 2017-10-27 | 河北东华舰化工有限公司 | A kind of chloroacetate reaction kettle system of accident disposal |
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| US8101805B2 (en) * | 2011-04-20 | 2012-01-24 | King Abdulaziz City for Science and Technology (KACST) | Low pressure one-step gas-phase process for production of methyl isobutyl ketone |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201610417U (en) * | 2009-12-25 | 2010-10-20 | 潍坊中业油脂有限公司 | Chlorination reaction device for chloroactic acid production |
| CN206587734U (en) * | 2017-03-21 | 2017-10-27 | 河北东华舰化工有限公司 | A kind of chloroacetate reaction kettle system of accident disposal |
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Address after: 051430 equipment manufacturing base and HENGJING Road south of Shijiazhuang, Hebei Province Patentee after: Shijiazhuang Chiyuan Chemical Co., Ltd Address before: 051430 Hebei, Shijiazhuang equipment manufacturing base, Heng Well Road South Patentee before: HEBEI HUADONGJIAN CHEMICAL Co.,Ltd. |