CN109621466A - A kind of system and method for new caprolactam water solution evaporation production caprolactam - Google Patents
A kind of system and method for new caprolactam water solution evaporation production caprolactam Download PDFInfo
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- CN109621466A CN109621466A CN201811540202.XA CN201811540202A CN109621466A CN 109621466 A CN109621466 A CN 109621466A CN 201811540202 A CN201811540202 A CN 201811540202A CN 109621466 A CN109621466 A CN 109621466A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/26—Multiple-effect evaporating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D223/00—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom
- C07D223/02—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom not condensed with other rings
- C07D223/06—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D223/08—Oxygen atoms
- C07D223/10—Oxygen atoms attached in position 2
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Abstract
The invention discloses a kind of system and method for new caprolactam water solution evaporation production caprolactam, and system includes prevapourising unit and quadruple effect fair current evaporation element and heating flash evaporation unit；Prevapourising unit includes own water preevaporator, prevapourising gas phase condenser；Quadruple effect fair current evaporation element includes the effect feed pump for passing sequentially through pipeline connection, an effect evaporation feed heater, an effect reboiler, an effect destilling tower, two effect reboilers and two effect destilling towers etc.；Heating flash evaporation unit includes heating evaporation device etc.；Steam consumption can be substantially reduced using the system of the new caprolactam water solution evaporation production caprolactam of the present invention, it produces one ton of caprolactam and only needs 0.60 ton of steam or so, and multiple-effect evaporation technique in the prior art, it produces one ton of caprolactam and then needs 1.05 tons of steam or so, reduce by 0.45 ton of steam consumption or so, can be saved by producing one ton of caprolactam by 50 tons of recirculated water or so, reduce by 75 yuan/ton of production cost.
Description
Technical field
The present invention relates to caprolactam production technical field, specifically a kind of new caprolactam water solution evaporates production
The system and method for caprolactam.
Background technique
Currently, include that rearrangement reaction, organic matter extraction and water are stripped process in preparing process of caprolactam both domestic and external,
Water content is up to 70% or more in the caprolactam water solution of formation, therefore how energy-efficient water removal is caprolactam production
In steps necessary；The dehydration of existing caprolactam water solution mainly uses multiple-effect distillation and membrane separation process, wherein multiple-effect
The evaporation process of each effect is required to a large amount of steam in the way of distillation, and external steam consumption is huge, and the steam evaporated is also
A large amount of recirculated cooling water is needed to be condensed, energy waste is serious；Membrane separation process can save mass energy, but this method is divided
Amount in the water separated out containing caprolactam is higher, cannot recycle again, causes the waste and water pollution of caprolactam, and
And the organic film needed is easily swollen, industrialization is difficult.
At present the heat of 60~95 DEG C of the low-grade hot water from rearrangement reaction liquid cooler in caprolactam production by
It is not high in its temperature, and temperature range amplitude of variation is big, and this residual heat of reaction is difficult to recycle, and the industry passes through at present
Recirculated cooling water is cooling, removes this part reaction heat, therefore causes waste of both heat and recirculated water, how to handle or
Person is urgent problem to be solved in caprolactam production using the hot water of rearrangement reaction liquid cooler.Existing caprolactam dress simultaneously
The own water multiple-effect evaporation unit set is triple effect evaporation technique, and consuming quantity of steam is more, and the multiple-effect that existing apparatus how is transformed is steamed
Hair technique, to reduce steam consumption, and the problem to be solved faced at present.
Summary of the invention
To solve the above problems, the object of the present invention is to provide a kind of new caprolactam water solution evaporations to produce acyl in oneself
The system and method for amine.
The present invention to achieve the above object, is achieved through the following technical solutions:
A kind of system of new caprolactam water solution evaporation production caprolactam, including prevapourising unit, quadruple effect fair current
Evaporation element and heating flash evaporation unit；Wherein prevapourising unit includes own water preevaporator, prevapourising gas phase condenser；Quadruple effect is suitable
Flow evaporator unit includes the effect feed pump for passing sequentially through pipeline connection, an effect evaporation feed heater, an effect reboiler, an effect
Destilling tower, two effect reboilers, two effect destilling towers, triple effect reboiler, triple effect destilling tower, quadruple effect reboiler, quadruple effect destilling tower, quadruple effect
Evaporate gas phase condenser and four-effect evaporation fixed gas vacuum pump；Heating flash evaporation unit include heating evaporation device, flash separator and
Three-level vapor injection vacuum pumping system；
The hot water outlet of rearrangement reaction liquid cooler is connected with the housing inlet port of own water preevaporator, own water preevaporator
Top gas outlet is connect with prevapourising gas phase condenser, and the gas vent of prevapourising gas phase condenser connects four-effect evaporation gas phase
The liquid-phase outlet of the gas access of condenser, prevapourising gas phase condenser is connect with process condensate liquid bath；
The bottom tube body outlet of own water preevaporator is entered by the tube body of an effect feed pump and an effect evaporation feed heater
Mouth is connected, and the tube body entrance that reboiler is imitated with one in the tube body outlet of an effect evaporation feed heater is connected, and an effect reboiler passes through
Pipeline introduces extraneous steam, and the tube body outlet of an effect reboiler is connect with an effect destilling tower, and an effect destilling tower overhead vapor passes through
Pipeline is connected to two effect reboilers, and an effect destilling tower bottoms material outlet is connect with the material inlet of two effect reboilers；Two effects are again
The condensate outlet for boiling device is connect with the housing inlet port of an effect evaporation feed heater, and the shell of an effect evaporation feed heater goes out
Mouth is connect with process condensate liquid bath；
The gas liquid outlet of two effect reboilers is connect by pipeline with two effect destilling tower material inlets, the bottom of two effect destilling towers
Material outlet is connect with triple effect reboiler material inlet, and two effect destilling tower overhead vapors connect the shell of triple effect reboiler by pipeline
The housing outlets of body entrance, triple effect reboiler condense liquid bath by pipeline connection technology；The gas liquid outlet of triple effect reboiler passes through
Pipeline is connect with triple effect destilling tower material inlet, and bottoms material outlet and the quadruple effect reboiler material inlet of triple effect destilling tower connect
It connects, triple effect destilling tower overhead vapor connects the housing inlet port of quadruple effect reboiler by pipeline, and the housing outlets of quadruple effect reboiler are logical
Piping Joining Technology condenses liquid bath；The gaseous phase outlet of quadruple effect destilling tower connects four-effect evaporation gas phase condenser, four-effect evaporation gas
The gas vent of phase condenser is connect with four-effect evaporation fixed gas vacuum pump, the liquid-phase outlet and work of four-effect evaporation gas phase condenser
Skill condenses liquid bath connection, and the bottoms material outlet of quadruple effect destilling tower passes through four-effect evaporation discharge pump and heating evaporation device material inlet
Connection, the material outlet of heating evaporation device connect with flash separator, the gaseous phase outlet of heating evaporation device and quadruple effect destilling tower
The overhead vapor of centre inlet connection, flash separator is connect by three-level vapor injection vacuum pumping system with quadruple effect destilling tower,
The outlet at bottom of flash separator is connect with caprolactam surge tank.
Preferred system, the hot water outlet of rearrangement reaction liquid cooler also passes through pipeline and the shell of own water preevaporator goes out
Mouth is connected, and the pipeline connects hot water cooler, and hot water cooler is connect by heat-exchanger pump with rearrangement reaction cooler.
Preferred system, own water preevaporator top gas outlet by pipeline also with four-effect evaporation gas phase condenser
Gas access connection.
Preferred system, the own water preevaporator include gas-liquid separator and reboiler, gas-liquid separator and are boiled again
It is connected by the first connecting pipe with the second connecting pipe between device, the gas-liquid separator top position offers gas and goes out
Mouthful, for gas-liquid separation washing after steam flow into prevapourising gas phase condenser, the side of gas-liquid separator open up own water into
Mouthful, for receiving own water, liquidometer is installed on the downside of the own water inlet, the upper end of the liquidometer passes through on liquidometer
Nozzle is communicated with gas-liquid separator, and the lower end of liquidometer is communicated by liquidometer lower nozzle with gas-liquid separator, the liquidometer
Can real-time display go out the separator liquid level in gas-liquid separator, the side of the gas-liquid separator bottom position opens up the first own water
It exports, Liquid level adjusting valve, the flow of the own water outflow gas-liquid separator of controllable adjustable, gas-liquid separation is installed after the first own water out
Own water in device flows into an effect evaporation feed pump via the first own water out, is equipped at the gas-liquid separator bottom centre position
Second own water out, the second own water out are communicated with the first connecting pipe, inside the gas-liquid separator from top to bottom according to
Secondary to be equipped with wire mesh demister, own water distributor and packing section, wire mesh demister is used for except the mist carried secretly in devaporation, own water
Distributor is connected with own water inlet, and packing section is located at the lower part of own water distributor, pacifies in the gas-liquid separator lower inside
Anti-swirl baffle is filled, the anti-swirl baffle is located above the second own water out；
The other end of first connecting pipe connects the own water inlet of reboiler, and the own water inlet of reboiler is located at reboiler
At lower head, the reboiler includes several efficient heat-exchanging pipes of reboiler shell and internal setting, the reboiler shell
Top is upper cover, and the bottom end of reboiler shell is lower head, installs two tube sheets, two pipes up and down inside the reboiler
Reboiler is divided into three chambers by plate, and upper and lower two chambers are connected by efficient heat-exchanging pipe, intermediate cavity for efficient heat-exchanging pipe with
The heat exchange of hot water is equipped with hot water inlet in the side of reboiler upper part of the housing, and the lower part of the reboiler shell other side is equipped with heat
Water out, the hot water come from rearrangement reaction liquid cooler, enter inside reboiler from hot water inlet, change with efficient heat-exchanging pipe
Enter hot water cooler through hot water outlet again after heat, exhaust outlet, the row are offered at the position of reboiler upper part of the housing
Port prevents the heat-transfer effect for influencing reboiler, in reboiler lower part of the housing for discharging the intracorporal inert gas of reboiler shell
It is offered at position and leads leaching mouth, for discharging the hydrops in reboiler when parking, be equipped with again at the upper cover of the reboiler
Device gas liquid outlet is boiled, gas-liquid separator is equipped with corresponding gas-liquid import, the reboiler gas liquid outlet and gas-liquid import
Between connect the second connecting pipe；
When the operation of own water preevaporator, the own water for entering own water evaporation process is flowed into gas-liquid separation by own water inlet
In device, separated gas is passed through after wire mesh demister removes the mist of deentrainment by gas vent pre- in gas-liquid separator
It evaporates in gas phase condenser, the own water in gas-liquid separator passes through the second own water out and the first connecting pipe after packing section
It enters in reboiler, the hot water of the efficient heat-exchanging pipe in the reboiler and the discharge of rearrangement reaction liquid cooler carries out hot friendship
It after changing, then is flowed back in gas-liquid separator by the second connecting pipe, in circulation certain time, after temperature, liquid level reach requirement, evaporation
Qualified own water is continuously sent into an effect evaporation feed pump, the liquid level by Liquid level adjusting valve control by the first own water out
The aperture of regulating valve, keep the separator liquid level in gas-liquid separator be in liquidometer upper orifice and liquidometer lower nozzle position it
Between.
The invention also includes a kind of methods of new caprolactam water solution evaporation production caprolactam, including following step
It is rapid:
1. 60~95 DEG C of hot water of rearrangement reaction liquid cooler, which enters own water preevaporator, heats own water, by own water oneself
The mass concentration of lactams is evaporated to 36~37% by 29~31%, and own water preevaporator top gas phase steam enters prevapourising gas
Phase condenser is condensed, and condensate liquid enters process condensate liquid bath, uncooled gas enter four-effect evaporation gas phase condenser after
Continuous condensation, condensate liquid enter process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump；Own water preevaporator
Top gas phase vapor (steam) temperature is 50~75 DEG C, and the pressure of own water preevaporator is -30~-90KPa；
2. own 50~80 DEG C of water preevaporator bottom temp of own water is pumped into effect evaporation charging heating by an effect charging
Device exchanges heat with the process condensate of two effect reboilers, and the own water after heating enters an effect destilling tower and carries out gas-liquid separation
Washing, the effect evaporation technology steam that temperature is 120~135 DEG C after washing enter two effect reboilers, an effect distillation tower bottom
Own water flows into two effect reboilers under the pressure of 0.15~0.30MPa；Wherein one effect distillation the own water of tower bottom temperature be 120~
140 DEG C, mass concentration of the caprolactam in own water is 38~42%；
3. two effect reboilers are under the heating of an effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters two effects
Destilling tower carries out gas-liquid separation washing, and the two effect evaporation technology steam that temperature is 105~125 DEG C after washing enter triple effect and boil again
Device, inflow process condensate liquid bath after two process condensates for imitating reboiler shell sides evaporate feed heater cooling into an effect, two
The own water of effect distillation tower bottom flows into triple effect reboiler under the pressure of 0.05~0.15MPa；Wherein two effect distillation tower bottoms oneself
The temperature of water is 110~125 DEG C, and mass concentration of the caprolactam in own water is 48~52%；
4. triple effect reboiler is under the heating of two effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters triple effect
Destilling tower carries out gas-liquid separation washing, and the triple effect evaporation process steam that temperature is 90~110 DEG C after washing enters quadruple effect reboiler,
The process condensate water of triple effect reboiler shell side flows into process condensate liquid bath, and triple effect distills the own water of tower bottom in -30~0.05MPa
Pressure under flow into quadruple effect reboiler, wherein triple effect distillation the own water of tower bottom temperature be 90~115 DEG C, caprolactam is in own water
In mass concentration be 62~70%；
5. the own aqueous vapor liquid mixture that quadruple effect reboiler under the heating of triple effect evaporation process steam, is heated enters quadruple effect
Destilling tower carries out gas-liquid separation washing, and the four-effect evaporation process steam that temperature is 55~75 DEG C after washing enters four-effect evaporation gas phase
Condenser is condensed, and condensate liquid flows into process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump,
The pressure of quadruple effect destilling tower is -85~-95KPa；The process condensate of quadruple effect reboiler shell side flows into process condensate liquid bath, quadruple effect
The own water of distillation tower bottom is pumped into heating evaporation device by four-effect evaporation discharge, and wherein the temperature of the quadruple effect distillation own water of tower bottom is
70~90 DEG C, mass concentration of the caprolactam in own water is 85~95%；
6. the own water in heating evaporation device is heated to 125~130 DEG C by external steam, moisture further evaporates, and obtains pure
The caprolactam that degree is 99% or more, the water that the pressure of heating evaporation device is isolated at the top of -80~-93KPa, heating evaporation device
Steam enters quadruple effect destilling tower；
7. the caprolactam that purity is 99% or more flows into flash separator by pressure difference, the vapor of flash distillation is in three-level
Enter quadruple effect destilling tower under the suction of vapor injection vacuum pumping system, keep the pressure in flash separator be -98.5~-
The purity of caprolactam is increased to 99.5% or more by 99.8KPa, and the caprolactam for reaching the purity flows into caprolactam buffering
Tank.
Preferred method, step 1. in further include that 60~95 DEG C of hot water from rearrangement reaction liquid cooler is by pipe
Road is directly entered hot water cooler after mixing with the hot water of own water preevaporator housing outlets, 50 are water-cooled to circulating cooling~
Rearrangement reaction liquid cooler is recycled back by heat-exchanger pump after 85 DEG C and carries out heat exchange cycle.
Preferred method, step 1. in further include that it is cold that own water preevaporator top gas phase steam enters four-effect evaporation gas phase
Condenser is condensed, and condensate liquid enters process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump.
The present invention has the advantage that compared with prior art
Own water preevaporator and four are used in the system of the new caprolactam water solution evaporation production caprolactam of the present invention
Fair current evaporation element is imitated, own water preevaporator carries out oneself using the low hot water of 60~95 DEG C in rearrangement reaction liquid cooler of grade
The prevapourising of water is realized more than recycling present apparatus technique to the greatest extent by the effective use to this part tow taste heat
Heat, while reducing the dosage of recirculated cooling water；In addition to an effect reboiler need to be made with external steam in quadruple effect fair current evaporation element
Outside for heat source, two effect reboilers, triple effect reboiler and quadruple effect reboiler use one to imitate destilling tower overhead vapor as heat source,
The usage amount of external steam and cooling water has also been greatly reduced in the three-effect downstream evaporation process that compares, and has huge economy
Benefit and environmental benefit.
Steam can be substantially reduced using the system of the new caprolactam water solution evaporation production caprolactam of the present invention to disappear
Consumption produces one ton of caprolactam and only needs 0.60 ton of steam or so, and multiple-effect evaporation technique in the prior art, one ton of production oneself
Lactams then needs 1.05 tons of steam or so, reduces by 0.45 ton of steam consumption or so, and one ton of caprolactam of production can be saved
50 tons of recirculated water or so, reduce by 75 yuan/ton of production cost.Energy consumption cost can be saved every year by producing 200000 tons of caprolactam devices per year
15000000 yuan or more.
Detailed description of the invention
Fig. 1 is the equipment connection schematic diagram of new caprolactam water solution evaporation production caprolactam production system；
Fig. 2 is the structural schematic diagram of own water preevaporator；
Appended drawing reference: the own water of 1 gas-liquid separator, 2 reboiler, 3 first 4 second connecting pipe of connecting pipe, 5 gas vent 6 into
12 Liquid level adjusting valve 13 of the own water out of 9 liquidometer lower nozzle of mouthful 7 liquidometer, 8 liquidometer upper orifice, 10 separator liquid level 11 first the
Two 15 17 anti-swirl baffles of own 16 packing section of water distributor of own 14 wire mesh demister of water out, the 18 own water inlet 19 of reboiler is lower to be sealed
25 hot water outlet of first 20 reboiler shell 21 efficient heat-exchanging pipe, 22 upper cover, 23 tube sheet, 24 hot water inlet, 26 exhaust outlet 27 leads leaching mouth
28 reboiler gas liquid outlet, 29 gas-liquid import.
Specific embodiment
Own water in the present invention refers to the aqueous solution of caprolactam.
One effect destilling tower, two effect destilling towers, triple effect destilling tower and quadruple effect destilling tower are plate-type wash, feed liquor position
For the inlet of each effect reboiler；Own water preevaporator is filler knockout tower, and in the top feed liquor of packing section.
Four-effect evaporation fixed gas vacuum pump is conventional vacuum pump.
Flash separator is original non-standard equipment of existing apparatus, and with second level and pressure above vessel fabrication qualification
Enterprise can manufacture；Principle is after own water enters flash separator, and with the reduction of pressure, moisture is flashed from caprolactam
Out, and simultaneously the separation of vapor and caprolactam is carried out in the equipment；The equipment is also possible to 201220358300.3 1
Structure disclosed in kind flash separator, is existing equipment.
Three-level vapor injection vacuum pumping system is modular system, and the enterprise for having vacuum ejector manufacture qualification can make
It makes；The equipment is also possible to structure disclosed in 201720013834.5 three-level vapor injection vacuum pumping systems, is existing equipment.
Heating evaporation device is original non-standard equipment of existing apparatus, and with second level and pressure above vessel fabrication qualification
Enterprise can manufacture；Principle is that own water is evaporated in the equipment after steam heats, and then vapor is again and in oneself
Amide separation.The equipment can be structure disclosed in 201320072075.1 Novel heating evaporators, be existing equipment.
The pressure of an effect reboiler is identical as an effect pressure for destilling tower in the application, pressure and two effects of two effect reboilers
The pressure of destilling tower is identical, and the pressure of triple effect reboiler is identical as the pressure of triple effect destilling tower, the pressure of quadruple effect reboiler and four
The pressure for imitating destilling tower is identical.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of system of new caprolactam water solution evaporation production caprolactam, as shown in Figure 1, including prevapourising list
Member, quadruple effect fair current evaporation element and heating flash evaporation unit；Wherein prevapourising unit includes that own water preevaporator, prevapourising gas phase are cold
Condenser；Quadruple effect fair current evaporation element includes the effect feed pump for passing sequentially through pipeline connection, an effect evaporation feed heater, an effect
Reboiler, an effect destilling tower, two effect reboilers, two effect destilling towers, triple effect reboiler, triple effect destilling tower, quadruple effect reboiler, quadruple effect
Destilling tower, four-effect evaporation gas phase condenser and four-effect evaporation fixed gas vacuum pump；Heating flash evaporation unit includes heating evaporation device, dodges
Steam separator and three-level vapor injection vacuum pumping system；
The hot water outlet of rearrangement reaction liquid cooler is connected with the housing inlet port of own water preevaporator, own water preevaporator
Top gas outlet is connect with prevapourising gas phase condenser, and the gas vent of prevapourising gas phase condenser connects four-effect evaporation gas phase
The liquid-phase outlet of the gas access of condenser, prevapourising gas phase condenser is connect with process condensate liquid bath；
The bottom tube body outlet of own water preevaporator is entered by the tube body of an effect feed pump and an effect evaporation feed heater
Mouth is connected, and the tube body entrance that reboiler is imitated with one in the tube body outlet of an effect evaporation feed heater is connected, and an effect reboiler passes through
Pipeline introduces extraneous steam, and the tube body outlet of an effect reboiler is connect with an effect destilling tower, and an effect destilling tower overhead vapor passes through
Pipeline is connected to two effect reboilers, and an effect destilling tower bottoms material outlet is connect with the material inlet of two effect reboilers；Two effects are again
The condensate outlet for boiling device is connect with the housing inlet port of an effect evaporation feed heater, and the shell of an effect evaporation feed heater goes out
Mouth is connect with process condensate liquid bath；
The gas liquid outlet of two effect reboilers is connect by pipeline with two effect destilling tower material inlets, the bottom of two effect destilling towers
Material outlet is connect with triple effect reboiler material inlet, and two effect destilling tower overhead vapors connect the shell of triple effect reboiler by pipeline
The housing outlets of body entrance, triple effect reboiler condense liquid bath by pipeline connection technology；The gas liquid outlet of triple effect reboiler passes through
Pipeline is connect with triple effect destilling tower material inlet, and bottoms material outlet and the quadruple effect reboiler material inlet of triple effect destilling tower connect
It connects, triple effect destilling tower overhead vapor connects the housing inlet port of quadruple effect reboiler by pipeline, and the housing outlets of quadruple effect reboiler are logical
Piping Joining Technology condenses liquid bath；The gaseous phase outlet of quadruple effect destilling tower connects four-effect evaporation gas phase condenser, four-effect evaporation gas
The gas vent of phase condenser is connect with four-effect evaporation fixed gas vacuum pump, the liquid-phase outlet and work of four-effect evaporation gas phase condenser
Skill condenses liquid bath connection, and the bottoms material outlet of quadruple effect destilling tower passes through four-effect evaporation discharge pump and heating evaporation device material inlet
Connection, the material outlet of heating evaporation device are connect with flash separator, gaseous phase outlet and the quadruple effect destilling tower of heating evaporation device
The overhead vapor of centre inlet connection, flash separator is connect by three-level vapor injection vacuum pumping system with quadruple effect destilling tower,
The outlet at bottom of flash separator is connect with caprolactam surge tank.
Embodiment 2
A kind of system of new caprolactam water solution evaporation production caprolactam, the equipment of quadruple effect fair current evaporation element with
Embodiment 1 is identical, the difference is that, the hot water outlet of rearrangement reaction liquid cooler also passes through pipeline and own water preevaporator
Housing outlets are connected, and the pipeline connects hot water cooler, and hot water cooler is connected by heat-exchanger pump and rearrangement reaction cooler
It connects；This design can according to the adjusting of own water preevaporator heat carried out into own water preevaporator hot water amount, or
Person will can directly pass through when the failure of own water preevaporator is overhauled from the whole hot water for resetting reaction solution cooler
Overheat water cooler returns to rearrangement reaction liquid cooler after carrying out cooling, ensures hot water normal circulation.
Embodiment 3
A kind of system of new caprolactam water solution evaporation production caprolactam, the equipment of quadruple effect fair current evaporation element with
Embodiment 1 or embodiment 2 are identical, the difference is that, the outlet of the top gas of own water preevaporator by pipeline also and quadruple effect
Evaporate the gas access connection of gas phase condenser；When system operates normally, own water preevaporator top gas phase steams for this design
Vapour is condensed by prevapourising gas phase condenser, but when prevapourising gas phase condenser breaks down and overhauled,
Own water preevaporator top gas phase steam is directly entered four-effect evaporation gas phase condenser and is condensed, and ensure that this system just
Often operation.
Embodiment 4
A kind of method of new caprolactam water solution evaporation production caprolactam, comprising the following steps:
1. 60 DEG C of hot water of rearrangement reaction liquid cooler, which enters own water preevaporator, heats own water, by acyl in oneself in own water
The mass concentration of amine is evaporated to 36% by 29%, and own water preevaporator top gas phase steam enters the progress of prevapourising gas phase condenser
Condensation, condensate liquid enter process condensate liquid bath, and uncooled gas, which enters four-effect evaporation gas phase condenser, to be continued to condense, condensate liquid
Into process condensate liquid bath, fixed gas is vented by four-effect evaporation fixed gas vacuum pump；Own water preevaporator top gas phase steam
Temperature is 50 DEG C, and the pressure of own water preevaporator is -90KPa；
2. own 50 DEG C of water preevaporator bottom temp of own water is pumped into effect evaporation feed heater by an effect charging, with
The process condensate of two effect reboilers exchanges heat, and the own water after heating enters an effect destilling tower and carries out gas-liquid separation washing,
The effect evaporation technology steam that temperature is 120 DEG C after washing enters two effect reboilers, and the own water of an effect distillation tower bottom exists
Two effect reboilers are flowed under the pressure of 0.15MPa；Wherein the temperature of the effect distillation own water of tower bottom is 120 DEG C, and caprolactam exists
Mass concentration in own water is 38%；
3. two effect reboilers are under the heating of an effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters two effects
Destilling tower carries out gas-liquid separation washing, and the two effect evaporation technology steam that temperature is 105 DEG C after washing enter triple effect reboiler, two effects
The process condensate of reboiler shell side flows into process condensate liquid bath, two effect destilling towers after entering an effect evaporation feed heater cooling
The own water of bottom flows into triple effect reboiler under the pressure of 0.05MPa；Wherein the temperature of the two effect distillation own water of tower bottom is 110
DEG C, mass concentration of the caprolactam in own water is 48%；
4. triple effect reboiler is under the heating of two effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters triple effect
Destilling tower carries out gas-liquid separation washing, and triple effect evaporation process steam at a temperature of 90 °C enters quadruple effect reboiler, triple effect after washing
The process condensate water of reboiler shell side flows into process condensate liquid bath, and triple effect distills pressure of the own water of tower bottom in -30MPa and flows down
Enter quadruple effect reboiler, wherein the temperature of the triple effect distillation own water of tower bottom is 90 DEG C, and mass concentration of the caprolactam in own water is
62%；
5. the own aqueous vapor liquid mixture that quadruple effect reboiler under the heating of triple effect evaporation process steam, is heated enters quadruple effect
Destilling tower carries out gas-liquid separation washing, and the four-effect evaporation process steam that temperature is 55 DEG C after washing enters four-effect evaporation vapor condensation
Device is condensed, and condensate liquid flows into process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump, quadruple effect
The pressure of reboiler and quadruple effect destilling tower is -85KPa；The process condensate of quadruple effect reboiler shell side flows into process condensate liquid bath,
The own water of quadruple effect distillation tower bottom is pumped into heating evaporation device by four-effect evaporation discharge, wherein the temperature of the quadruple effect distillation own water of tower bottom
Degree is 70 DEG C, and mass concentration of the caprolactam in own water is 85%；
6. the own water in heating evaporation device is heated to 125 DEG C by external steam, moisture further evaporates, and obtains purity and is
99% or more caprolactam, the vapor that the pressure of heating evaporation device is isolated at the top of -80KPa, heating evaporation device enter
Quadruple effect destilling tower；
7. the caprolactam that purity is 99% or more flows into flash separator by pressure difference, the vapor of flash distillation is in three-level
Enter quadruple effect destilling tower under the suction of vapor injection vacuum pumping system, keeping the pressure in flash separator is -98.5KPa, will
The purity of caprolactam is increased to 99.5% or more, and the caprolactam for reaching the purity flows into caprolactam surge tank.
Embodiment 5
A kind of method of new caprolactam water solution evaporation production caprolactam, comprising the following steps:
1. 95 DEG C of hot water of rearrangement reaction liquid cooler, which enters own water preevaporator, heats own water, by acyl in oneself in own water
The mass concentration of amine is evaporated to 37% by 31%, and own water preevaporator top gas phase steam enters the progress of prevapourising gas phase condenser
Condensation, condensate liquid enter process condensate liquid bath, and uncooled gas, which enters four-effect evaporation gas phase condenser, to be continued to condense, condensate liquid
Into process condensate liquid bath, fixed gas is vented by four-effect evaporation fixed gas vacuum pump；Own water preevaporator top gas phase steam
Temperature is 75 DEG C, and the pressure of own water preevaporator is -30KPa；
2. own 80 DEG C of water preevaporator bottom temp of own water is pumped into effect evaporation feed heater by an effect charging, with
The process condensate of two effect reboilers exchanges heat, and the own water after heating enters an effect destilling tower and carries out gas-liquid separation washing,
The effect evaporation technology steam that temperature is 135 DEG C after washing enters two effect reboilers, and the own water of an effect distillation tower bottom exists
Two effect reboilers are flowed under the pressure of 0.30MPa；Wherein the temperature of the effect distillation own water of tower bottom is 140 DEG C, and caprolactam exists
Mass concentration in own water is 42%；
3. two effect reboilers are under the heating of an effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters two effects
Destilling tower carries out gas-liquid separation washing, and the two effect evaporation technology steam that temperature is 125 DEG C after washing enter triple effect reboiler, two effects
The process condensate of reboiler shell side flows into process condensate liquid bath, two effect destilling towers after entering an effect evaporation feed heater cooling
The own water of bottom flows into triple effect reboiler under the pressure of 0.15MPa；Wherein the temperature of the two effect distillation own water of tower bottom is 125
DEG C, mass concentration of the caprolactam in own water is 52%；
4. triple effect reboiler is under the heating of two effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters triple effect
Destilling tower carries out gas-liquid separation washing, and the triple effect evaporation process steam that temperature is 110 DEG C after washing enters quadruple effect reboiler, triple effect
The process condensate water of reboiler shell side flows into process condensate liquid bath, and triple effect distills the own water of tower bottom under the pressure of 0.05MPa
Quadruple effect reboiler is flowed into, wherein the temperature of the triple effect distillation own water of tower bottom is 115 DEG C, mass concentration of the caprolactam in own water
It is 70%；
5. the own aqueous vapor liquid mixture that quadruple effect reboiler under the heating of triple effect evaporation process steam, is heated enters quadruple effect
Destilling tower carries out gas-liquid separation washing, and the four-effect evaporation process steam that temperature is 75 DEG C after washing enters four-effect evaporation vapor condensation
Device is condensed, and condensate liquid flows into process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump, quadruple effect
The pressure of reboiler and quadruple effect destilling tower is -95KPa；The process condensate of quadruple effect reboiler shell side flows into process condensate liquid bath,
The own water of quadruple effect distillation tower bottom is pumped into heating evaporation device by four-effect evaporation discharge, wherein the temperature of the quadruple effect distillation own water of tower bottom
Degree is 90 DEG C, and mass concentration of the caprolactam in own water is 95%；
6. the own water in heating evaporation device is heated to 130 DEG C by external steam, moisture further evaporates, and obtains purity and is
99% or more caprolactam, the vapor that the pressure of heating evaporation device is isolated at the top of -93KPa, heating evaporation device enter
Quadruple effect destilling tower；
7. the caprolactam that purity is 99% or more flows into flash separator by pressure difference, the vapor of flash distillation is in three-level
Enter quadruple effect destilling tower under the suction of vapor injection vacuum pumping system, keeping the pressure in flash separator is -99.8KPa, will
The purity of caprolactam is increased to 99.5% or more, and the caprolactam for reaching the purity flows into caprolactam surge tank.
Embodiment 6
A kind of method of new caprolactam water solution evaporation production caprolactam, comprising the following steps:
1. 75 DEG C of hot water of rearrangement reaction liquid cooler, which enters own water preevaporator, heats own water, by acyl in oneself in own water
The mass concentration of amine is evaporated to 37% by 30%, and own water preevaporator top gas phase steam enters the progress of prevapourising gas phase condenser
Condensation, condensate liquid enter process condensate liquid bath, and uncooled gas, which enters four-effect evaporation gas phase condenser, to be continued to condense, condensate liquid
Into process condensate liquid bath, fixed gas is vented by four-effect evaporation fixed gas vacuum pump；Own water preevaporator top gas phase steam
Temperature is 60 DEG C, and the pressure of own water preevaporator is -50KPa；
2. own 65 DEG C of water preevaporator bottom temp of own water is pumped into effect evaporation feed heater by an effect charging, with
The process condensate of two effect reboilers exchanges heat, and the own water after heating enters an effect destilling tower and carries out gas-liquid separation washing,
The effect evaporation technology steam that temperature is 125 DEG C after washing enters two effect reboilers, and the own water of an effect distillation tower bottom exists
Two effect reboilers are flowed under the pressure of 0.20MPa；Wherein the temperature of the effect distillation own water of tower bottom is 125 DEG C, and caprolactam exists
Mass concentration in own water is 39%；
3. two effect reboilers are under the heating of an effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters two effects
Destilling tower carries out gas-liquid separation washing, and the two effect evaporation technology steam that temperature is 115 DEG C after washing enter triple effect reboiler, two effects
The process condensate of reboiler shell side flows into process condensate liquid bath, two effect destilling towers after entering an effect evaporation feed heater cooling
The own water of bottom flows into triple effect reboiler under the pressure of 0.10MPa；Wherein the temperature of the two effect distillation own water of tower bottom is 115
DEG C, mass concentration of the caprolactam in own water is 50%；
4. triple effect reboiler is under the heating of two effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters triple effect
Destilling tower carries out gas-liquid separation washing, and the triple effect evaporation process steam that temperature is 95 DEG C after washing enters quadruple effect reboiler, triple effect
The process condensate water of reboiler shell side flows into process condensate liquid bath, and triple effect distills pressure of the own water of tower bottom in -10MPa and flows down
Enter quadruple effect reboiler, wherein the temperature of the triple effect distillation own water of tower bottom is 95 DEG C, and mass concentration of the caprolactam in own water is
65%；
5. the own aqueous vapor liquid mixture that quadruple effect reboiler under the heating of triple effect evaporation process steam, is heated enters quadruple effect
Destilling tower carries out gas-liquid separation washing, and the four-effect evaporation process steam that temperature is 60 DEG C after washing enters four-effect evaporation vapor condensation
Device is condensed, and condensate liquid flows into process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump, quadruple effect
The pressure of reboiler and quadruple effect destilling tower is -90KPa；The process condensate of quadruple effect reboiler shell side flows into process condensate liquid bath,
The own water of quadruple effect distillation tower bottom is pumped into heating evaporation device by four-effect evaporation discharge, wherein the temperature of the quadruple effect distillation own water of tower bottom
Degree is 75 DEG C, and mass concentration of the caprolactam in own water is 90%；
6. the own water in heating evaporation device is heated to 126 DEG C by external steam, moisture further evaporates, and obtains purity and is
99% or more caprolactam, the vapor that the pressure of heating evaporation device is isolated at the top of -85KPa, heating evaporation device enter
Quadruple effect destilling tower；
7. the caprolactam that purity is 99% or more flows into flash separator by pressure difference, the vapor of flash distillation is in three-level
Enter quadruple effect destilling tower under the suction of vapor injection vacuum pumping system, keeping the pressure in flash separator is -98.9KPa, will
The purity of caprolactam is increased to 99.5% or more, and the caprolactam for reaching the purity flows into caprolactam surge tank.
Embodiment 7
A kind of method of new caprolactam water solution evaporation production caprolactam, comprising the following steps:
1. 85 DEG C of hot water of rearrangement reaction liquid cooler, which enters own water preevaporator, heats own water, by acyl in oneself in own water
The mass concentration of amine is evaporated to 38% by 30%, and own water preevaporator top gas phase steam enters the progress of prevapourising gas phase condenser
Condensation, condensate liquid enter process condensate liquid bath, and uncooled gas, which enters four-effect evaporation gas phase condenser, to be continued to condense, condensate liquid
Into process condensate liquid bath, fixed gas is vented by four-effect evaporation fixed gas vacuum pump；Own water preevaporator top gas phase steam
Temperature is 65 DEG C, and the pressure of own water preevaporator is -80KPa；
2. own 70 DEG C of water preevaporator bottom temp of own water is pumped into effect evaporation feed heater by an effect charging, with
The process condensate of two effect reboilers exchanges heat, and the own water after heating enters an effect destilling tower and carries out gas-liquid separation washing,
The effect evaporation technology steam that temperature is 130 DEG C after washing enters two effect reboilers, and the own water of an effect distillation tower bottom exists
Two effect reboilers are flowed under the pressure of 0.25MPa；Wherein the temperature of the effect distillation own water of tower bottom is 135 DEG C, and caprolactam exists
Mass concentration in own water is 40%；
3. two effect reboilers are under the heating of an effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters two effects
Destilling tower carries out gas-liquid separation washing, and the two effect evaporation technology steam that temperature is 120 DEG C after washing enter triple effect reboiler, two effects
The process condensate of reboiler shell side flows into process condensate liquid bath, two effect destilling towers after entering an effect evaporation feed heater cooling
The own water of bottom flows into triple effect reboiler under the pressure of 0.12MPa；Wherein the temperature of the two effect distillation own water of tower bottom is 122
DEG C, mass concentration of the caprolactam in own water is 50%；
4. triple effect reboiler is under the heating of two effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters triple effect
Destilling tower carries out gas-liquid separation washing, and the triple effect evaporation process steam that temperature is 105 DEG C after washing enters quadruple effect reboiler, triple effect
The process condensate water of reboiler shell side flows into process condensate liquid bath, and triple effect distills pressure of the own water of tower bottom in -5MPa and flows down
Enter quadruple effect reboiler, wherein the temperature of the triple effect distillation own water of tower bottom is 105 DEG C, and mass concentration of the caprolactam in own water is
68%；
5. the own aqueous vapor liquid mixture that quadruple effect reboiler under the heating of triple effect evaporation process steam, is heated enters quadruple effect
Destilling tower carries out gas-liquid separation washing, and the four-effect evaporation process steam that temperature is 72 DEG C after washing enters four-effect evaporation vapor condensation
Device is condensed, and condensate liquid flows into process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump, quadruple effect
The pressure of reboiler and quadruple effect destilling tower is -92KPa；The process condensate of quadruple effect reboiler shell side flows into process condensate liquid bath,
The own water of quadruple effect distillation tower bottom is pumped into heating evaporation device by four-effect evaporation discharge, wherein the temperature of the quadruple effect distillation own water of tower bottom
Degree is 88 DEG C, and mass concentration of the caprolactam in own water is 92%；
6. the own water in heating evaporation device is heated to 128 DEG C by external steam, moisture further evaporates, and obtains purity and is
99% or more caprolactam, the vapor that the pressure of heating evaporation device is isolated at the top of -90KPa, heating evaporation device enter
Quadruple effect destilling tower；
7. the caprolactam that purity is 99% or more flows into flash separator by pressure difference, the vapor of flash distillation is in three-level
Enter quadruple effect destilling tower under the suction of vapor injection vacuum pumping system, keeping the pressure in flash separator is -99.5KPa, will
The purity of caprolactam is increased to 99.5% or more, and the caprolactam for reaching the purity flows into caprolactam surge tank.
Embodiment 8
A kind of method of new caprolactam water solution evaporation production caprolactam with embodiment 4, only step 1. in
It further include that hot water of 60 DEG C of the hot water from rearrangement reaction liquid cooler through piping and own water preevaporator housing outlets is mixed
It is directly entered hot water cooler after conjunction, rearrangement reaction liquid cooling is recycled back into but by heat-exchanger pump after being water-cooled to 50 DEG C with circulating cooling
Device carries out heat exchange cycle.
And when prevapourising gas phase condenser is overhauled, own water preevaporator top gas phase steam enters four-effect evaporation
Gas phase condenser is condensed, and condensate liquid enters process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump.
Embodiment 9
A kind of method of new caprolactam water solution evaporation production caprolactam with embodiment 5, only step 1. in
It further include that hot water of 95 DEG C of the hot water from rearrangement reaction liquid cooler through piping and own water preevaporator housing outlets is mixed
It is directly entered hot water cooler after conjunction, rearrangement reaction liquid cooling is recycled back into but by heat-exchanger pump after being water-cooled to 85 DEG C with circulating cooling
Device carries out heat exchange cycle.
And when prevapourising gas phase condenser is overhauled, own water preevaporator top gas phase steam enters four-effect evaporation
Gas phase condenser is condensed, and condensate liquid enters process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump.
Embodiment 10
A kind of method of new caprolactam water solution evaporation production caprolactam with embodiment 6, only step 1. in
It further include that hot water of 75 DEG C of the hot water from rearrangement reaction liquid cooler through piping and own water preevaporator housing outlets is mixed
It is directly entered hot water cooler after conjunction, rearrangement reaction liquid cooling is recycled back into but by heat-exchanger pump after being water-cooled to 60 DEG C with circulating cooling
Device carries out heat exchange cycle.
And when prevapourising gas phase condenser is overhauled, own water preevaporator top gas phase steam enters four-effect evaporation
Gas phase condenser is condensed, and condensate liquid enters process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump.
Embodiment 11
As shown in Fig. 2, a kind of own water preevaporator includes gas-liquid separator 1 and reboiler 2, gas-liquid separator 1 and boil again
It is connected by the first connecting pipe 3 with the second connecting pipe 4 between device 2,1 top position of gas-liquid separator offers gas
Body outlet 5 flows into prevapourising gas phase condenser for the steam after gas-liquid separation washing, and the side of gas-liquid separator 1 opens up
Own water inlet 6 is equipped with liquidometer 7 in the downside of the own water inlet 6, the upper end of the liquidometer 7 is logical for receiving own water
It crosses liquidometer upper orifice 8 to communicate with gas-liquid separator 1, the lower end of liquidometer 7 passes through liquidometer lower nozzle 9 and gas-liquid separator 1
Communicate, the liquidometer 7 can real-time display go out the separator liquid level 10 in gas-liquid separator 1, the 1 bottom position of gas-liquid separator
The side set opens up the first own water out 11, installs Liquid level adjusting valve 12, the own water flow of controllable adjustable after the first own water out 11
The flow of gas-liquid separator 1 out, the own water in gas-liquid separator 1 flow into an effect evaporation feed pump via the first own water out 11,
The second own water out 13 is equipped at 1 bottom centre position of gas-liquid separator, the second own water out 13 is connect with first
Pipeline 3 communicates, and wire mesh demister 14, own water distributor 15 are from top to bottom sequentially installed with inside the gas-liquid separator 1 and is filled out
Expect section 16, wire mesh demister 14 is used for except the mist carried secretly in devaporation, and own water distributor 15 is connected with own water inlet 6, fills out
Material section 16 is located at the lower part of own water distributor 15, installs anti-swirl baffle 17 in 1 lower inside of gas-liquid separator, described anti-
It is vortexed baffle 17 and is located at the second own 13 top of water out；
The other end of first connecting pipe 3 connects the own water inlet 18 of reboiler, and the own water inlet 18 of reboiler is located at again
At the lower head 19 for boiling device 2, the reboiler 2 includes several efficient heat-exchanging pipes 21 of reboiler shell 20 and internal setting, institute
The top for stating reboiler shell 20 is upper cover 22, and the bottom end of reboiler shell 20 is lower head 19, inside the reboiler 2
Two tube sheets 23 of installation up and down, two tube sheets 23 divide reboiler 2 for three chambers, and upper and lower two chambers are connected by efficient heat-exchanging pipe 21
It connects, intermediate cavity is used for the heat exchange of efficient heat-exchanging pipe 21 and hot water, is equipped with hot water in the side on 20 top of reboiler shell
Import 24, the lower part of 20 other side of reboiler shell are equipped with hot water outlet 25, and the hot water comes from rearrangement reaction liquid cooler, from
Hot water inlet 24 enters inside reboiler 2, cold into hot water through hot water outlet 25 again after exchanging heat with efficient heat-exchanging pipe 21
But device offers exhaust outlet 26 at 20 upper position of reboiler shell, and the exhaust outlet 26 is for discharging reboiler shell 20
Interior inert gas prevents the heat-transfer effect for influencing reboiler, offers in 20 lower position of reboiler shell and leads leaching mouth 27,
For discharging the hydrops in reboiler 2 when parking, reboiler gas liquid outlet 28 is equipped at the upper cover 22 of the reboiler 2,
Gas-liquid separator 1 is equipped with corresponding gas-liquid import 29, connects between the reboiler gas liquid outlet 28 and gas-liquid import 29
Connect the second connecting pipe 4；
When the operation of own water preevaporator, the own water for entering own water evaporation process is flowed into gas-liquid point by own water inlet 6
From in device 1, separated gas is after wire mesh demister 14 removes the mist of deentrainment by gas vent in gas-liquid separator 1
5 are passed through in prevapourising gas phase condenser, and the own water in gas-liquid separator 1 passes through the second own 13 He of water out after packing section 16
First connecting pipe 3 enters in reboiler 2, the efficient heat-exchanging pipe 21 in the reboiler 2 and rearrangement reaction liquid cooler
It after the hot water of discharge carries out heat exchange, then is flowed back in gas-liquid separator 1 by the second connecting pipe 4, in circulation certain time, temperature
After degree, liquid level reach requirement, qualified own water is evaporated by the first own water out 11, is continuously sent by the control of Liquid level adjusting valve 12
Enter effect evaporation feed pump, the aperture of the Liquid level adjusting valve 12 keeps the separator liquid level 10 in gas-liquid separator 1 to be in liquid
Between position meter upper orifice 8 and 9 position of liquidometer lower nozzle.
Claims (7)
1. a kind of system of new caprolactam water solution evaporation production caprolactam, it is characterised in that: including prevapourising unit,
Quadruple effect fair current evaporation element and heating flash evaporation unit；Wherein prevapourising unit includes own water preevaporator, prevapourising vapor condensation
Device；Quadruple effect fair current evaporation element includes passing sequentially through the one of pipeline connection to imitate feed pump, an effect evaporation feed heater, an effect again
Device, an effect destilling tower, two effect reboilers, two effect destilling towers, triple effect reboiler, triple effect destilling tower, quadruple effect reboiler, quadruple effect is boiled to steam
Evaporate tower, four-effect evaporation gas phase condenser and four-effect evaporation fixed gas vacuum pump；Heating flash evaporation unit includes heating evaporation device, flash distillation
Separator and three-level vapor injection vacuum pumping system；
The hot water outlet of rearrangement reaction liquid cooler is connected with the housing inlet port of own water preevaporator, the top of own water preevaporator
Gas vent is connect with prevapourising gas phase condenser, and the gas vent of prevapourising gas phase condenser connects four-effect evaporation vapor condensation
The liquid-phase outlet of the gas access of device, prevapourising gas phase condenser is connect with process condensate liquid bath；
The tube body entrance phase that the bottom tube body outlet of own water preevaporator passes through an effect feed pump and an effect evaporation feed heater
Even, the tube body outlet of an effect evaporation feed heater is connected with the tube body entrance of an effect reboiler, and an effect reboiler passes through pipeline
Extraneous steam is introduced, the tube body outlet of an effect reboiler is connect with an effect destilling tower, and an effect destilling tower overhead vapor passes through pipeline
Two effect reboilers are connected to, an effect destilling tower bottoms material outlet is connect with the material inlet of two effect reboilers；Two effect reboilers
Condensate outlet with one effect evaporation feed heater housing inlet port connect, one effect evaporation feed heater housing outlets and
The connection of process condensate liquid bath；
The gas liquid outlet of two effect reboilers is connect by pipeline with two effect destilling tower material inlets, the bottoms material of two effect destilling towers
Outlet is connect with triple effect reboiler material inlet, and two effect destilling tower overhead vapors are entered by the shell that pipeline connects triple effect reboiler
Mouthful, the housing outlets of triple effect reboiler condense liquid bath by pipeline connection technology；The gas liquid outlet of triple effect reboiler passes through pipeline
It being connect with triple effect destilling tower material inlet, the bottoms material outlet of triple effect destilling tower is connect with quadruple effect reboiler material inlet, and three
The housing inlet port that destilling tower overhead vapor connects quadruple effect reboiler by pipeline is imitated, the housing outlets of quadruple effect reboiler pass through pipeline
Joining Technology condenses liquid bath；The gaseous phase outlet of quadruple effect destilling tower connects four-effect evaporation gas phase condenser, four-effect evaporation vapor condensation
The gas vent of device is connect with four-effect evaporation fixed gas vacuum pump, the liquid-phase outlet and process condensate of four-effect evaporation gas phase condenser
The bottoms material outlet of liquid bath connection, quadruple effect destilling tower is connect by four-effect evaporation discharge pump with heating evaporation device material inlet,
The material outlet of heating evaporation device is connect with flash separator, the middle part of the gaseous phase outlet of heating evaporation device and quadruple effect destilling tower into
The overhead vapor of mouth connection, flash separator is connect by three-level vapor injection vacuum pumping system with quadruple effect destilling tower, flash distillation point
Outlet at bottom from device is connect with caprolactam surge tank.
2. the system of the new caprolactam water solution evaporation production caprolactam of one kind according to claim 1, feature
Be: the hot water outlet of rearrangement reaction liquid cooler also passes through pipeline and is connected with the housing outlets of own water preevaporator, and should
Pipeline connects hot water cooler, and hot water cooler is connect by heat-exchanger pump with rearrangement reaction cooler.
3. the system of the new caprolactam water solution evaporation production caprolactam of one kind according to claim 1, feature
Be: the top gas outlet of own water preevaporator is also connected with the gas access of four-effect evaporation gas phase condenser by pipeline.
4. the system of the new caprolactam water solution evaporation production caprolactam of one kind according to claim 1, feature
Be: the own water preevaporator includes gas-liquid separator (1) and reboiler (2), gas-liquid separator (1) and reboiler (2)
Between be connected with the second connecting pipe (4) by the first connecting pipe (3), gas-liquid separator (1) top position opens up
There are gas vent (5), flows into prevapourising gas phase condenser for the steam after gas-liquid separation washing, gas-liquid separator (1)
Side opens up own water inlet (6), for receiving own water, is equipped with liquidometer (7) on the downside of the own water inlet (6), described
The upper end of liquidometer (7) is communicated by liquidometer upper orifice (8) with gas-liquid separator (1), and the lower end of liquidometer (7) passes through liquid level
Meter lower nozzle (9) communicated with gas-liquid separator (1), the liquidometer (7) can real-time display go out the separation in gas-liquid separator (1)
Device liquid level (10), the side of gas-liquid separator (1) bottom position open up the first own water out (11), the first own water out
(11) Liquid level adjusting valve (12) are installed afterwards, the flow of own water outflow gas-liquid separator (1) of controllable adjustable, gas-liquid separator (1)
Interior own water flows into an effect evaporation feed pump, gas-liquid separator (1) bottom centre position via the first own water out (11)
Place is equipped with the second own water out (13), and the second own water out (13) communicates with the first connecting pipe (3), the gas-liquid separation
Wire mesh demister (14), own water distributor (15) and packing section (16), silk screen foam removal are from top to bottom sequentially installed with inside device (1)
Device (14) is used for except the mist carried secretly in devaporation, and own water distributor (15) is connected with own water inlet (6), packing section (16) position
In the lower part of own water distributor (15), anti-swirl baffle (17) are installed in the gas-liquid separator (1) lower inside, the anti-whirlpool
Baffle (17) are flowed to be located above the second own water out (13)；
The other end of first connecting pipe (3) connects the own water inlet of reboiler (18), and the own water inlet of reboiler (18) is located at
At the lower head (19) of reboiler (2), the reboiler (2) includes that reboiler shell (20) and internal the several of setting efficiently change
Heat pipe (21), the top of the reboiler shell (20) are upper cover (22), and the bottom end of reboiler shell (20) is lower head
(19), reboiler (2) is divided into three in the reboiler (2) internal two tube sheets (23) of installation, two tube sheets (23) up and down
Chamber, upper and lower two chambers are connected by efficient heat-exchanging pipe (21), and heat of the intermediate cavity for efficient heat-exchanging pipe (21) and hot water is handed over
It changes, is equipped with hot water inlet (24) in the side on reboiler shell (20) top, the lower part of reboiler shell (20) other side is equipped with
Hot water outlet (25), the hot water come from rearrangement reaction liquid cooler, enter reboiler (2) inside from hot water inlet (24),
Enter hot water cooler through hot water outlet (25) again with after efficient heat-exchanging pipe (21) heat exchange, on reboiler shell (20) top
It is offered at position exhaust outlet (26), the exhaust outlet (26) is used to discharge the inert gas in reboiler shell (20), prevents
The heat-transfer effect for influencing reboiler offers in reboiler shell (20) lower position and leads leaching mouth (27), for arranging when parking
The hydrops in reboiler (2) is put, is equipped with reboiler gas liquid outlet (28) at the upper cover (22) of the reboiler (2), gas-liquid
Separator (1) is equipped with corresponding gas-liquid import (29), the reboiler gas liquid outlet (28) and gas-liquid import (29) it
Between connect the second connecting pipe (4)；
When the operation of own water preevaporator, the own water for entering own water evaporation process is flowed into gas-liquid separation by own water inlet (6)
In device (1), separated gas is after wire mesh demister (14) remove the mist of deentrainment by gas in gas-liquid separator (1)
Outlet (5) be passed through in prevapourising gas phase condenser, the own water in gas-liquid separator (1) by packing section (16) after pass through second oneself
Water out (13) and the first connecting pipe (3) enter in reboiler (2), the efficient heat-exchanging pipe in the reboiler (2)
(21) after carrying out heat exchange with the hot water of rearrangement reaction liquid cooler discharge, then gas-liquid separation flowed back to by the second connecting pipe (4)
In device (1), in circulation certain time, after temperature, liquid level reach requirement, evaporates qualified own water and pass through the first own water out
(11), an effect evaporation feed pump is continuously sent by Liquid level adjusting valve (12) control, the aperture of the Liquid level adjusting valve (12) is protected
Hold the separator liquid level (10) in gas-liquid separator (1) be in liquidometer upper orifice (8) and liquidometer lower nozzle (9) position it
Between.
5. a kind of method of new caprolactam water solution evaporation production caprolactam, it is characterised in that: the following steps are included:
1. 60~95 DEG C of hot water of rearrangement reaction liquid cooler, which enters own water preevaporator, heats own water, by acyl in oneself in own water
The mass concentration of amine is evaporated to 36~37% by 29~31%, and it is cold that own water preevaporator top gas phase steam enters prevapourising gas phase
Condenser is condensed, and condensate liquid enters process condensate liquid bath, and it is cold that uncooled gas enters the continuation of four-effect evaporation gas phase condenser
Solidifying, condensate liquid enters process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump；At the top of own water preevaporator
Gas phase steam temperature is 50~75 DEG C, and the pressure of own water preevaporator is -30~-90KPa；
2. own 50~80 DEG C of water preevaporator bottom temp of own water is pumped into effect evaporation feed heater by an effect charging, with
The process condensate of two effect reboilers exchanges heat, and the own water after heating enters an effect destilling tower and carries out gas-liquid separation washing,
The effect evaporation technology steam that temperature is 120~135 DEG C after washing enters two effect reboilers, and the own water of an effect distillation tower bottom exists
Two effect reboilers are flowed under the pressure of 0.15~0.30MPa；Wherein the temperature of the effect distillation own water of tower bottom is 120~140 DEG C,
Mass concentration of the caprolactam in own water is 38~42%；
3. two effect reboilers, under the heating of an effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters two effect distillations
Tower carries out gas-liquid separation washing, and the two effect evaporation technology steam that temperature is 105~125 DEG C after washing enter triple effect reboiler, and two
The process condensate for imitating reboiler shell side, which enters after an effect evaporates feed heater cooling, flows into process condensate liquid bath, two effect distillations
The own water of tower bottom flows into triple effect reboiler under the pressure of 0.05~0.15MPa；The wherein temperature of the two effect distillation own water of tower bottom
Degree is 110~125 DEG C, and mass concentration of the caprolactam in own water is 48~52%；
4. triple effect reboiler is under the heating of two effect evaporation technology steam, the own aqueous vapor liquid mixture being heated enters triple effect distillation
Tower carries out gas-liquid separation washing, and the triple effect evaporation process steam that temperature is 90~110 DEG C after washing enters quadruple effect reboiler, triple effect
The process condensate water of reboiler shell side flows into process condensate liquid bath, and triple effect distills pressure of the own water in -30~0.05MPa of tower bottom
Quadruple effect reboiler is flowed under power, wherein the temperature of the triple effect distillation own water of tower bottom is 90~115 DEG C, and caprolactam is in own water
Mass concentration is 62~70%；
5. the own aqueous vapor liquid mixture that quadruple effect reboiler under the heating of triple effect evaporation process steam, is heated enters quadruple effect distillation
Tower carries out gas-liquid separation washing, and the four-effect evaporation process steam that temperature is 55~75 DEG C after washing enters four-effect evaporation vapor condensation
Device is condensed, and condensate liquid flows into process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump, quadruple effect
The pressure of destilling tower is -85~-95KPa；The process condensate of quadruple effect reboiler shell side flows into process condensate liquid bath, quadruple effect distillation
The own water of tower bottom is pumped into heating evaporation device by four-effect evaporation discharge, wherein quadruple effect distillation the own water of tower bottom temperature be 70~
90 DEG C, mass concentration of the caprolactam in own water is 85~95%；
6. the own water in heating evaporation device is heated to 125~130 DEG C by external steam, moisture further evaporates, and obtains purity and is
99% or more caprolactam, the vapor that the pressure of heating evaporation device is isolated at the top of -80~-93KPa, heating evaporation device
Into quadruple effect destilling tower；
7. the caprolactam that purity is 99% or more flows into flash separator by pressure difference, the vapor of flash distillation is in three-level steam
It sprays and enters quadruple effect destilling tower under the suction of pumped vacuum systems, keeping the pressure in flash separator is -98.5~-99.8KPa,
The purity of caprolactam is increased to 99.5% or more, the caprolactam for reaching the purity flows into caprolactam surge tank.
6. the method for the new caprolactam water solution evaporation production caprolactam of one kind according to claim 5, feature
Be: step 1. in further include that 60~95 DEG C of the hot water from rearrangement reaction liquid cooler is through piping and own water prevapourising
It is directly entered hot water cooler after the hot water mixing of device housing outlets, is water-cooled to after 50~85 DEG C with circulating cooling by heat-exchanger pump
It is recycled back into rearrangement reaction liquid cooler and carries out heat exchange cycle.
7. the method for the new caprolactam water solution evaporation production caprolactam of one kind according to claim 5, feature
Be: step 1. in further include that own water preevaporator top gas phase steam enters four-effect evaporation gas phase condenser and condensed, cold
Lime set enters process condensate liquid bath, and fixed gas is vented by four-effect evaporation fixed gas vacuum pump.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013170A (en) * | 2019-12-26 | 2020-04-17 | 聊城鲁西聚酰胺新材料科技有限公司 | Caprolactam water solution energy-saving evaporation system and method |
| CN111635348A (en) * | 2020-06-22 | 2020-09-08 | 聊城鲁西聚酰胺新材料科技有限公司 | Application and system of screw vacuum pump in caprolactam refining process production |
| CN111686477A (en) * | 2020-06-30 | 2020-09-22 | 聊城鲁西聚酰胺新材料科技有限公司 | Caprolactam extraction liquid washing tower, system and process |
| CN112142669A (en) * | 2020-07-14 | 2020-12-29 | 中国石油化工股份有限公司 | High-efficiency dehydration method of caprolactam |
| CN112439219A (en) * | 2019-09-05 | 2021-03-05 | 中石油吉林化工工程有限公司 | Four-effect evaporator for preparing acrylonitrile |
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2018
- 2018-12-17 CN CN201811540202.XA patent/CN109621466A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112439219A (en) * | 2019-09-05 | 2021-03-05 | 中石油吉林化工工程有限公司 | Four-effect evaporator for preparing acrylonitrile |
| CN111013170A (en) * | 2019-12-26 | 2020-04-17 | 聊城鲁西聚酰胺新材料科技有限公司 | Caprolactam water solution energy-saving evaporation system and method |
| CN111635348A (en) * | 2020-06-22 | 2020-09-08 | 聊城鲁西聚酰胺新材料科技有限公司 | Application and system of screw vacuum pump in caprolactam refining process production |
| CN111686477A (en) * | 2020-06-30 | 2020-09-22 | 聊城鲁西聚酰胺新材料科技有限公司 | Caprolactam extraction liquid washing tower, system and process |
| CN111686477B (en) * | 2020-06-30 | 2022-07-29 | 聊城鲁西聚酰胺新材料科技有限公司 | Caprolactam extraction liquid washing tower, system and process |
| CN112142669A (en) * | 2020-07-14 | 2020-12-29 | 中国石油化工股份有限公司 | High-efficiency dehydration method of caprolactam |
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