CN208907089U - Oxidation unit during a kind of cyclohexane oxidation process production cyclohexanone - Google Patents
Oxidation unit during a kind of cyclohexane oxidation process production cyclohexanone Download PDFInfo
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- CN208907089U CN208907089U CN201821639586.6U CN201821639586U CN208907089U CN 208907089 U CN208907089 U CN 208907089U CN 201821639586 U CN201821639586 U CN 201821639586U CN 208907089 U CN208907089 U CN 208907089U
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Abstract
The utility model discloses oxidation units during a kind of cyclohexane oxidation process production cyclohexanone, are mainly made of one or more tail gas washing towers, oxidation reactor, regulating valve and pipeline, and configure corresponding pipeline and valve；Tail gas washing tower is connected with oxidation reactor, the oxidized tail gas being discharged from cyclohexane oxidation device enters in tower from washing tail gas tower bottom, the medium temperature hexamethylene come from pipeline enters in tower from washing tail gas top of tower, part cyclohexanol, cyclohexanone, cyclohexyl hydroperoxide are condensed and enter in hexamethylene liquid phase in oxidized tail gas, and flow automatically from washing tail gas tower bottom to oxidation reactor or decomposition reactor, present apparatus oxidized tail gas recovery unit is discharged into after then summarizing from washing tail gas top of tower discharge oxidized tail gas.After the utility model, by the content of cyclohexanol, cyclohexanone and cyclohexyl hydroperoxide in reduction cyclohexane oxidation process in oxidation reaction charging, reaction yield is improved, the energy consumptions such as steam, the cooling water of alkane rectification are reduced, is of great significance to reduction device material loss and energy loss.
Description
Technical field
The invention belongs to chemical technology field, it is related to oxidation unit during a kind of cyclohexane oxidation process production cyclohexanone.
Background technique
It is the important intermediate for preparing caprolactam, adipic acid that cyclohexane oxidation, which prepares cyclohexanone, cyclohexanol or KA oil,；Ring
Hexanone still produces the industrial chemicals of the chemicals such as caprolactone, and a kind of excellent solvent, is the main way of hexamethylene Application in Chemical Engineering
Diameter.
Air oxidation of cyclohexane technique is still domestic and international prevailing technology, including without catalysis and has catalytic oxidation technique；Generally
Think, in cyclohexane oxidation process, cyclohexane oxidation is a radical reaction, cyclohexanol, cyclohexanone and cyclohexyl
Hydrogen peroxide is all the initiator of cyclohexane oxidation, makes liquid phase hexamethylene and oxygen that oxidation reaction occur and generates cyclohexyl peroxide
Change hydrogen (CHHP)；CHHP is unstable, and cyclohexanol, cyclohexanone etc., while CHHP, hexamethylene are readily broken down under oxidation reaction condition
Pure and mild cyclohexanone etc. all is easier to be oxidized than hexamethylene, and special cyclohexanone is more easily and by the further oxygen of free oxygen in liquid phase
At acid, acid occurs esterification with alcohols in reaction system again and generates the multi-products such as ester metaplasia.
In order to reduce side reaction, cyclohexane oxidation device is generally using more series connection, and series connection number of units is more, liquid phase
Just closer to plug flow, oxidization-hydrogenation ratio is higher for the flowing of mixture；Type of reactor is divided into stirring-type and inner draft tube formula；Reaction
Hexamethylene is fed successively with oxidized tail gas, steam heat-exchanging, after being heated to 175 DEG C or so, is sequentially entered generally by 4 ~ 7 series connection groups
At oxidation reactor, is contacted with air and oxidation reaction occurs；Cyclohexane oxidation is exothermic reaction, and oxidation reaction heat is mainly by hexamethylene
Alkane is evaporated and is removed, and by control reaction temperature and reaction pressure, adjusts hexamethylene evaporation capacity, to realize that reacting balance carries out；
Gas-liquid separation occurs in every reactor upper space, tail gas contains a large amount of hexamethylene gases, nitrogen, oxygen, and reaction life
At carbon monoxide, carbon dioxide, cyclohexanol, cyclohexanone, CHHP etc., enter oxidized tail gas recovery unit；Liquid product is certainly
Flow into next reactor that the reaction was continued.
Conversion ratio is higher, and oxidation product is higher by the chance of further deep oxidation, and selectivity is lower；General conversion ratio is every
Increase by 1%, yield will decline 4%.In order to obtain reasonable oxidization-hydrogenation ratio, the conversion ratio of hexamethylene keeps very low, about 3.5mol%
~5mol%, afterbody reaction after oxidation solution in be on a small quantity hexamethylene oxidation product, such as: cyclohexanol, cyclohexanone, CHHP,
And a small amount of acid and ester, the overwhelming majority are unreacted hexamethylene；Unreacted hexamethylene is after the purification of device correlation unit
And it recycles.
Oxidizing reaction temperature is high, can improve the conversion ratio of oxidation reaction, but can aggravate the decomposition of CHHP in oxidation reactor
With the deep oxidation of cyclohexanol cyclohexanone, reduction causes selectivity and yield.The oxidizing reaction temperature of most commercial plants is 165
DEG C ~ 185 DEG C of ranges, pressure is in 1.0 ~ 1.5MPa range；Oxidizing reaction temperature has heating sequence, constant temperature sequence or cooling sequence point
Cloth, majority is using cooling sequence；There is device using directly a small amount of low temperature hexamethylene is passed through to oxidation reactor, instead as adjusting
Answer the ancillary measure of temperature.
Oxidation solution product is separated by catalytic decomposition CHHP, organic matter with lye, and the organic matter isolated send hexamethylene to steam
Evaporate unit；Hexamethylene distillation unit generally uses triple effect or multi-effect distilling technique, from different tower tops distillate it is qualified, in it is mild low
The hexamethylene of temperature, the hexamethylene of different temperatures send oxidation unit and oxidized tail gas recovery unit back to, and the hexamethylene that tower reactor obtains
Pure and mild cyclohexanone mixture (KA oil) is sent to alcohol ketone refined unit；Alcohol ketone refined unit uses high vacuum multitower process, cyclohexanol
It is separated with cyclohexanone mixture through more rectifying column rectifying, the cyclohexanone or and cyclohexanone of isolated qualification；Hexamethylene when necessary
Alcohol returns to alcohol ketone refined unit after dehydrogenation obtains thick cyclohexanone.
The oxidized tail gas of every oxidation reactor discharge, Main Components are exactly by the vapour-saturated nitrogen of hexamethylene, also
Contain cyclohexanone, cyclohexanol, cyclohexyl hydroperoxide etc.；The oxidized tail gas of each oxidation reactor discharge summarizes heel row to aoxidizing tail
Gas recovery unit, the unit are mainly made of heat exchange tower system and scrubbing tower system.Oxidized tail gas successively passes through heat exchange tower and washes
Tower is washed, the medium temperature sent respectively with alkane rectification unit, low temperature hexamethylene carry out heat transfer and mass transfer, recycle organic in oxidized tail gas
Object (hexamethylene, cyclohexanone, cyclohexanol, cyclohexyl hydroperoxide etc.), is layered, the major part that reaction system is taken out of by grease
Water separation, while also hexamethylene, the hexamethylene of recycling and condensation are fed using the pre- thermal oxide of heat of evaporation of gas phase hexamethylene in tail gas
Alkane is recirculated back to oxidation reactor together；The oxidized tail gas of most organic is removed again through absorption and sorption or other techniques
Method processing is discharged after reaching environment protectment protection.
Cyclohexane oxidation is a radical reaction, and cyclohexanol, cyclohexanone and CHHP are drawing for the oxidation reaction
Send out agent；For no catalytic air oxidation method technique, feeding needs to cause containing a small amount of cyclohexanol, cyclohexanone, CHHP to rise in hexamethylene
Effect；Cyclohexyl hydroperoxide, cyclohexanol and cyclohexanone etc. all are easier to be oxidized than hexamethylene, and special cyclohexanone is in the reaction
Under the conditions of be easier to be oxidized to organic acid, acid occurs esterification with alcohol again and generates ester, reduces reaction yield；Feed hexamethylene
In cyclohexanol, cyclohexanone, CHHP about 50% or more by deep oxidation, thus increase hexamethylene and sodium hydroxide consumption；Work as charging
In hexamethylene when the too high levels of cyclohexanol, cyclohexanone, CHHP, device hexamethylene consumption value can be significantly raised；Concrete embodiment is,
When alcohol ketone content is high in hexamethylene rectification cell return hexamethylene, device hexamethylene consumption value can be increased.
There are two sources for existing commercial plant, oxidation charging hexamethylene and its alcohol ketone contained.First is that oxidation reaction tail gas
Hexamethylene, cyclohexanone, cyclohexanol, the CHHP of middle saturation, oxidized tail gas automatic oxidation reaction device are directly returned to oxidized tail gas after coming out
Unit is received, cyclohexanone, cyclohexanol and CHHP do not carry out decrement treatment in this burst of logistics or material, and almost all returns after condensing
Hexamethylene is condensed into charging, finally and is imported in oxidation reaction charging hexamethylene, amount accounts for about oxidation charging hexamethylene middle ring
2/3rds of hexanol, cyclohexanone and CHHP total amount.Second is that from the hexamethylene that oxidation reaction liquid product recycles, content has largely
Cyclohexane oxidation product separates after catalytic decomposition, alkali separation to hexamethylene rectification cell rectifying, after isolating crude glycol ketone
Cyclohexanol and cyclohexanone still a small amount of in hexamethylene are recycled, alcohol ketone content is one of most important Con trolling index of device, generally will
The control of alcohol ketone total content is below 0.1% in hexamethylene；The alcohol ketone amount of the part account for about oxidation charging in cyclohexanol, cyclohexanone and
The one third of CHHP total amount.
Currently, the cyclohexanone, cyclohexanol, the content of CHHP in commercial plant in oxidized tail gas are big, and without decrement treatment
Enter in charging hexamethylene again, Returning oxidation reactor；Only the hexamethylene of product liquid recycling is refined, that is to say, that only
It can be controlled by adjusting the content of alcohol ketone in the distillate hexamethylene of alkane rectification unit the top of the distillation column in oxidation charging hexamethylene
Alcohol ketone amount；And hexamethylene alkane rectification will produce high-purity hexamethylene and need to consume a large amount of steam and cooling water.
Utility model content
In order to overcome the shortcomings of the prior art, the present invention is provided during a kind of cyclohexane oxidation process production cyclohexanone
Oxidation unit, the oxidized tail gas containing cyclohexanol, cyclohexanone and CHHP that cyclohexane oxidation process is discharged are washed and are dropped
Temperature processing is washed with medium temperature hexamethylene by Returning oxidation reactor after part cyclohexanol, cyclohexanone and CHHP condensation in oxidized tail gas
Wash rear not condensed oxidized tail gas discharge be aggregated into after the tail gas recycle cell processing of the present apparatus as oxidation reactor into
Material shortens cyclohexanol, hexamethylene to reduce the content of cyclohexanol, cyclohexanone and CHHP in oxidation reactor hexamethylene combined feed
When stop under ketone and CHHP high temperature, reaching reduces device material loss, while mitigating hexamethylene rectifier unit hexamethylene middle ring
The requirement of hexanone, hexamethylene alcohol content reduces the energy consumptions such as the steam of hexamethylene rectification cell.
Technical solution of the present invention:
Oxidation unit during a kind of cyclohexane oxidation process production cyclohexanone, mainly by one or more tail gas washing towers,
Oxidation reactor, regulating valve and pipeline composition, and configure corresponding pipeline and valve；Tail gas washing tower and oxidation reactor phase
Even, automatic oxidation reaction device discharge oxidized tail gas enter in tower from washing tail gas tower bottom, from pipeline come medium temperature hexamethylene from
Washing tail gas top of tower enters in tower, and part cyclohexanol, cyclohexanone, cyclohexyl hydroperoxide are condensed and enter in oxidized tail gas
In hexamethylene liquid phase, and flow automatically from washing tail gas tower bottom to oxidation reactor or decomposition reactor, from washing tail gas top of tower
Discharge oxidized tail gas is discharged into present apparatus oxidized tail gas recovery unit after then summarizing.
From cyclohexane oxidation device be discharged oxidized tail gas (pressure be 10~15bar, temperature be 160~185 DEG C) from
Washing tail gas tower bottom enters in tower, and the medium temperature hexamethylene come from pipeline enters in tower from washing tail gas top of tower, and the two is in tower
Interior generation exchanges heat and mass transfer, and part cyclohexanol, cyclohexanone, CHHP are condensed and enter in hexamethylene liquid phase in oxidized tail gas, and
Flow automatically from washing tail gas tower bottom to oxidation reactor or decomposition reactor, is then converged from washing tail gas top of tower discharge oxidized tail gas
The General Logistics Department is discharged into present apparatus oxidized tail gas recovery unit.
Wherein the setting of tail gas washing tower can be correspondingly arranged 1 or more oxidation reactors with every oxidation reactor
Merge 1 tail gas washing tower of setting；Be preferably provided with last platform oxidation reactor be connected tail gas washing tower 1, or with Mo Tai and inverse
Second oxidation reactor merges the tail gas washing tower 1 that is connected.
Wherein oxidation reactor can be 4~7 oxidation reactor series connection, preferably 5~6 oxidation reactor series connection.
The unlimited oxidized tail gas recovery unit from the present apparatus of medium temperature hexamethylene, or come from present apparatus hexamethylene alkane rectification list
Member.Hexamethylene, hexamethylene rectification cell hexamethylene before can be oxidation reactor charging hexamethylene, cyclohexane feed heating,
It is preferred that oxidation reactor feeds hexamethylene.
Wherein tail gas washing tower is packed tower perhaps one of plate column or a void tower or slack tank；Tower reason
It is 1~6, preferably 1~3 by plate number；Top of tower is equipped with thermometer, detects the temperature of overhead.
Oxidation technology improved method during a kind of cyclohexane oxidation process production cyclohexanone, cyclohexane oxidation process is discharged
The oxidized tail gas containing cyclohexanol, cyclohexanone and cyclohexyl hydroperoxide washed and cooled down with medium temperature hexamethylene, aoxidize tail
Part cyclohexanol, cyclohexanone and CHHP are condensed with washing rear hexamethylene back to oxidation reactor or decomposition reaction in gas
Device, not condensed oxidized tail gas discharge are aggregated into present apparatus oxidized tail gas recovery unit.
Tail gas washing tower operating pressure is identical as oxidation reactor, and overhead gas outlet temperature enters tower temperature lower than oxidized tail gas
5~10 DEG C, preferably 2~5 DEG C of degree.
Tail gas washing tower is no more than 10% (weight) of oxidation reaction combined feed alkane using the addition total amount of medium temperature hexamethylene,
Preferably more than 5%(weight), regulating valve is configured on medium temperature cyclohexane feed pipeline.
The medium temperature hexamethylene temperature is 60~150 DEG C, preferably 125~145 DEG C；Hexamethylene is the hexamethylene being refined
Alkane, wherein the sum of cyclohexanol, cyclohexanone and CHHP three's content are less than 2500ppm(mass), preferably smaller than 1500ppm(matter
Amount).
The preferred 400-700ppm of CHHP amount (weight) in the oxidation reaction charging hexamethylene.
Tower top oxidized tail gas discharge temperature alarm setting is 145 DEG C after washed, utilizes adjusting valve regulation medium temperature hexamethylene
Additional amount, to control oxidized tail gas discharge temperature.
The present invention on oxidation reactor by increasing tail gas washing tower, with the hexamethylene of medium temperature in scrubbing tower to oxidation tail
Gas carries out washing and handles with cooling, so that part cyclohexanol, cyclohexanone, CHHP in oxidized tail gas be made to be returned directly to oxidation reaction
Device or decomposition reactor；From scrubber overhead discharge reduce cyclohexanol, cyclohexanone, cyclohexyl hydroperoxide content oxidized tail gas
It is aggregated into present apparatus oxidized tail gas processing unit.It can reach following purpose using the washing of medium temperature hexamethylene, first is that reducing discharge oxygen
Change tail gas in cyclohexanol, cyclohexanone and CHHP content, second is that will not wash away completely cyclohexanone in oxidized tail gas, cyclohexanol and
CHHP, thus a certain amount of cyclohexanol, cyclohexanol and CHHP are needed as inducer, in particular for a certain amount of in oxidation reaction
CHHP initiated oxidation reaction, inventor obtain after study CHHP oxidation reaction charging object preferred scope be 400-700
Ppm (weight).
These technologies can reduce oxidized tail gas part and be brought into cyclohexanol, cyclohexanol and cyclohexyl in oxidation reactor charging
Hydrogen peroxide 3000ppm (weight), especially cyclohexyl hydroperoxide 2000ppm (weight), can be by hexamethylene rectifying column hexamethylene
Cyclohexanone, hexamethylene alcohol content are raw with 100,000 tons/year of cyclohexane oxidation process from 800ppm (weight) to 1350ppm (weight) in alkane
Pimelinketone device meter is produced, 1.15 tons/h of steam consumption can be reduced, saves 632 tons/h of cooling water；Due to reducing cyclohexyl peroxidating
Hydrogen enters the amount in oxidation reactor, and oxidation reaction by-products reduce 5-10%, so that cyclohexanone yield can be improved, 100,000 tons/
Year scale can reduce hexamethylene every year and consume 500-1200 tons.
Detergent using the medium temperature hexamethylene of oxidation reactor charging as tail gas washing tower in the present invention, can be effective
The alcohol ketone that ground reduces in oxidized tail gas crosses content, but retains a certain amount of CHHP.Induction of a certain amount of CHHP to oxidation reaction
There is positive effect, retains a certain amount of CHHP amount, the production efficiency of oxidation reaction can be maintained.
Detailed description of the invention
Fig. 1 is Cyclohexane Oxidation Unit schematic diagram after improving；
In figure: 1- cyclohexane feed heater, 2- oxidation reactor is serial, and 4 oxidation reactors series connection are shown as in figure,
It can be more than 4 oxidation reactor series connection, 3- oxidized tail gas recovery unit, 4- is decomposed and alkali separation system, 5- hexamethylene essence
Evaporate system, 6- tail gas washing tower, 7- exhaust temperature meter, 8- charging hexamethylene regulating valve
SM- middle pressure steam SCM- steam condensation water.
Fig. 2 is existing Cyclohexane Oxidation Unit schematic diagram；
In figure: 1- cyclohexane feed heater, 2- oxidation reactor is serial, and 4 oxidation reactors series connection are shown as in figure,
It can be more than 4 reactor series connection, 3- oxidized tail gas recovery unit, 4- is decomposed and alkali separation system, 5- hexamethylene alkane rectification system
System
SM- middle pressure steam SCM- steam condensation water.
Specific embodiment
Cyclohexane oxidation process produces oxidation technology improved method during cyclohexanone, mainly by one or more washing tail gas
Tower 6, oxidation reactor 2, regulating valve 8 and pipeline composition, and configure corresponding pipeline and valve；It is arranged from cyclohexane oxidation device
Oxidized tail gas (pressure is 10~15bar, and temperature is 160~185 DEG C) out enters in tower from washing tail gas tower bottom, from pipeline
The medium temperature hexamethylene come enters in tower from washing tail gas top of tower, and heat exchange and mass transfer, oxidized tail gas middle part occur in tower for the two
Divide cyclohexanol, cyclohexanone, cyclohexyl hydroperoxide to be condensed and enter in hexamethylene liquid phase, and flows automatically from washing tail gas tower bottom
To oxidation reactor or decomposition reactor, present apparatus oxidation tail is discharged into after then summarizing from washing tail gas top of tower discharge oxidized tail gas
Gas recovery unit.
For the pimelinketone device of 100kt/a cyclohexane oxidation process, conversion rate of oxidation considers by 3.5%, Tables 1 and 2 difference
For under two kinds of operating conditions, oxidation reaction feeds source and the composition of hexamethylene.
1 oxidation reaction of table charging hexamethylene and alcohol ketone cross source table, operating condition one
Note 1: cyclohexanol+cyclohexanone content is 800ppm in the hexamethylene that hexamethylene rectification cell comes, and is free of CHHP.
Note 2: it is to respectively refer to cyclohexanol, cyclohexanone and CHHP that alcohol ketone, which is crossed,.
2 oxidation reaction of table charging hexamethylene and alcohol ketone cross source table, operating condition two
Note 1, hexamethylene rectification cell recycling hexamethylene in cyclohexanol+cyclohexanone content be 1200ppm, be free of CHHP.
2, alcohol ketone crosses finger ring hexanol, cyclohexanone and CHHP respectively.
Oxidation charging cyclohexane amount about 485110.2kg/h, wherein being 365028.8kg/h from hexamethylene alkane rectification, about
The 75% of the total alkane amount of Zhan, the hexamethylene 120081.4kg/h from oxidized tail gas recycling, accounts for about the 25% of total alkane amount.From upper 1 He of table
Table can be seen that cyclohexanol, cyclohexanone and cyclohexyl hydroperoxide are mainly from oxidized tail gas in oxidizing ethyle alkyl charging, even if ring
When alcohol ketone total amount reaches 1200ppm in the hexamethylene that hexane rectification cell distillates, alcohol ketone crosses content also less than alcohol in oxidation charging
Ketone crosses the one third of total amount.Therefore, it takes simple and low cost mode to reduce and brings oxidation charging hexamethylene into oxidized tail gas
Alcohol ketone crosses content in alkane, advantageously reduces charging hexamethylene alcohol ketone and crosses content, reduces device material consumption, is conducive to expand hexamethylene essence
Unit operating flexibility is evaporated, the steam consumption of the unit is reduced.
Embodiment 1:
Oxidation reactor is 6 series connection, and #6 oxidation reactor connects tail gas washing tower, feeds 130 DEG C using oxidation reaction
Hexamethylene oxidized tail gas in tail gas washing tower is washed and cooled down, and tail gas washing tower operating pressure is 12-13 bar,
Part cyclohexanol, cyclohexanone, cyclohexyl hydroperoxide are condensed and enter in hexamethylene liquid phase in oxidized tail gas, and wash from tail gas
It washs tower bottom and flow to oxidation reactor certainly.Oxidized tail gas crosses content and drops to 7500ppm, alkane by 9620 ppm by washing, alcohol ketone
Alcohol ketone amount is 800ppm in rectification cell hexamethylene.
Entrance alcohol ketone is reduced in this way and crosses additional amount, and alcohol ketone crosses content and drops to 2440ppm, CHHP by original 2980ppm
Content drops to 580ppm by 990ppm.
It has used oxidation reaction to feed 130-150 DEG C of hexamethylene to wash oxidized tail gas, it will not depth washing oxidation
The content that alcohol ketone is crossed in tail gas especially remains a certain amount of cyclohexyl hydroperoxide content, induction is played in oxidation reactor
Reagentia does not reduce oxidizing reaction rate, keeps the production capacity of oxidation reaction.
Due to reducing the content that alcohol ketone is crossed in oxidation charging, especially cyclohexyl hydroperoxide content is reduced, and is being aoxidized
Reaction process improves the content that oxidation solution active principle alcohol ketone is crossed, and reduces the content of by-product acids and ester, 100,000 tons/year of rings
Hexanone device can reduce hexamethylene and consume 800 tons.
Embodiment 2:
Oxidation reactor is 6 series connection, and #5 connect tail gas washing tower with #6 oxidation reactor, feeds ring using oxidation reaction
Hexane oxidized tail gas in tail gas washing tower is washed and cooled down, and tail gas washing tower operating pressure is 12-13 bar, oxygen
Change part cyclohexanol in tail gas, cyclohexanone, cyclohexyl hydroperoxide are condensed and enter in hexamethylene liquid phase, and from washing tail gas
Tower bottom flow to oxidation reactor certainly.Oxidized tail gas crosses content and drops to 6980ppm by 9620 ppm by washing, alcohol ketone；Alkane essence
Evaporating alcohol ketone amount in unit hexamethylene is 800ppm.
Entrance alcohol ketone is reduced in this way and crosses additional amount, and alcohol ketone crosses content and drops to 2320ppm, CHHP by original 2980ppm
Content drops to 400ppm by 990ppm.
It has used oxidation reaction to feed 130-150 DEG C of hexamethylene and has carried out carry out washing tail gas, it will not depth washing oxidation tail
The content that alcohol ketone is crossed in gas especially remains a certain amount of cyclohexyl hydroperoxide content, and it is anti-that induction is played in oxidation reactor
It should act on, not reduce oxidizing reaction rate, keep the production capacity of oxidation reaction.
Due to reducing the content that alcohol ketone is crossed in oxidation charging, especially cyclohexyl hydroperoxide content is reduced, and is being aoxidized
Reaction process improves the content that oxidation solution active principle alcohol ketone is crossed, and reduces the content of by-product acids and ester, 100,000 tons/year of rings
Hexanone device can reduce hexamethylene and consume 1200 tons.
Embodiment 3:
Oxidation reactor is 6 series connection, and #5 is connect tail gas washing tower with #6 oxidation reactor, fed using oxidation reaction
140 DEG C of hexamethylenes oxidized tail gas in tail gas washing tower is washed and cooled down, and tail gas washing tower operating pressure is 13-15
Bar, part cyclohexanol, cyclohexanone, cyclohexyl hydroperoxide are condensed and enter in hexamethylene liquid phase in oxidized tail gas, and from tail
Gas wash tower bottom flow to oxidation reactor certainly.Oxidized tail gas is crossed content and is dropped to by 9620 ppm by washing, alcohol ketone
6980ppm；Alcohol ketone amount is 1350ppm in alkane rectification unit hexamethylene.
Entrance alcohol ketone is reduced in this way and crosses additional amount, and alcohol ketone crosses content and drops to 2620ppm, hexamethylene by original 2980ppm
Base content of hydrogen peroxide drops to 400ppm by 990ppm.
It has used oxidation reaction to feed 130-150 DEG C of hexamethylene and has carried out carry out washing tail gas, it will not depth washing oxidation tail
The content that alcohol ketone is crossed in gas especially remains a certain amount of cyclohexyl hydroperoxide content, and it is anti-that induction is played in oxidation reactor
It should act on, not reduce oxidizing reaction rate, keep the production capacity of oxidation reaction.
Due to reducing the content that alcohol ketone is crossed in oxidation charging, especially cyclohexyl hydroperoxide content is reduced, and is being aoxidized
Reaction process improves the content that oxidation solution active principle alcohol ketone is crossed, and reduces the content of by-product acids and ester, 100,000 tons/year of rings
Hexanone device can reduce hexamethylene and consume 1000 tons.
Since the cyclohexanol in alkane rectification process hexamethylene and cyclohexanone ketone content are increased to 1350ppm by 800ppm, steam
Vapour consumption can reduce 1150kg/h, can save within such 1 year 9200 tons of steam, rectifying column can reduce 2-6 block tower tray.
Embodiment 4:
Oxidation reactor is 6 series connection, and #6 oxidation reactor connects tail gas washing tower, feeds 140 DEG C using oxidation reaction
Hexamethylene oxidized tail gas in tail gas washing tower is washed and cooled down, and tail gas washing tower operating pressure is 13-15 bar,
Part cyclohexanol, cyclohexanone, cyclohexyl hydroperoxide are condensed and enter in hexamethylene liquid phase in oxidized tail gas, and wash from tail gas
It washs tower bottom and flow to oxidation reactor certainly.Oxidized tail gas crosses content and drops to 7500ppm by 9620 ppm by washing, alcohol ketone；Alkane
Alcohol ketone amount is 1200ppm in rectification cell hexamethylene.
Entrance alcohol ketone is reduced in this way and crosses additional amount, and alcohol ketone crosses content and drops to 2740ppm, hexamethylene by original 2980ppm
Base content of hydrogen peroxide drops to 580ppm by 990ppm.
It has used oxidation reaction to feed 120-150 DEG C of hexamethylene and has carried out carry out washing tail gas, it will not depth washing oxidation tail
The content that alcohol ketone is crossed in gas especially remains a certain amount of cyclohexyl hydroperoxide content, and it is anti-that induction is played in oxidation reactor
It should act on, not reduce oxidizing reaction rate, keep the production capacity of oxidation reaction.
Due to reducing the content that alcohol ketone is crossed in oxidation charging, especially cyclohexyl hydroperoxide content is reduced, and is being aoxidized
Reaction process improves the content that oxidation solution active principle alcohol ketone is crossed, and reduces the content of by-product acids and ester, 100,000 tons/year of rings
Hexanone device can reduce hexamethylene and consume 750 tons.
Since the cyclohexanol in alkane rectification process hexamethylene and cyclohexanone ketone content are increased to 1200ppm by 800ppm, steam
Vapour consumption can reduce 920kg/h, can save within such 1 year 7360 tons of steam, rectifying column can reduce 2-6 block tower tray.
Embodiment 5
Oxidation reactor is 6 series connection, and #6 oxidation reactor connects tail gas washing tower, before oxidation reaction charging heating
120 DEG C of hexamethylenes oxidized tail gas in tail gas washing tower is washed and cooled down, and tail gas washing tower operating pressure is 13-15
Bar, part cyclohexanol, cyclohexanone, cyclohexyl hydroperoxide are condensed and enter in hexamethylene liquid phase in oxidized tail gas, and from tail
Gas wash tower bottom flow to oxidation reactor certainly.Oxidized tail gas is crossed content and is dropped to by 9620 ppm by washing, alcohol ketone
6890ppm；Alcohol ketone amount is 1200ppm in alkane rectification unit hexamethylene.
Entrance alcohol ketone is reduced in this way and crosses additional amount, and alcohol ketone crosses content and drops to 2680ppm, CHHP by original 2980ppm
Content drops to 500ppm by 990ppm.
It has used oxidation reaction charging to heat preceding 120 DEG C of hexamethylenes and has carried out carry out washing tail gas, it will not depth washing oxidation
The content that alcohol ketone is crossed in tail gas especially remains a certain amount of CHHP content, plays induced reaction in oxidation reactor, do not have
There is reduction oxidizing reaction rate, keeps the production capacity of oxidation reaction.
Due to reducing the content that alcohol ketone is crossed in oxidation charging, especially cyclohexyl hydroperoxide content is reduced, and is being aoxidized
Reaction process improves the content that oxidation solution active principle alcohol ketone is crossed, and reduces the content of by-product acids and ester, 100,000 tons/year of rings
Hexanone device can reduce hexamethylene and consume 600 tons.
Since the cyclohexanol in alkane rectification process hexamethylene and cyclohexanone ketone content are increased to 1200ppm by 800ppm, steam
Vapour consumption can reduce 920kg/h, can save within such 1 year 7360 tons of steam, rectifying column can reduce 2-6 block tower tray.
Embodiment 6
Oxidation reactor is 6 series connection, and #6 oxidation reactor connects tail gas washing tower, uses 60 DEG C of hexamethylene rectification cell
Hexamethylene oxidized tail gas in tail gas washing tower is washed and cooled down, and tail gas washing tower operating pressure is 13-15 bar,
Part cyclohexanol, cyclohexanone, cyclohexyl hydroperoxide are condensed and enter in hexamethylene liquid phase in oxidized tail gas, and wash from tail gas
It washs tower bottom and flow to oxidation reactor certainly.Oxidized tail gas crosses content and drops to 5000ppm by 9620 ppm by washing, alcohol ketone；Alkane
Alcohol ketone amount is 1200ppm in rectification cell hexamethylene.
Entrance alcohol ketone is reduced in this way and crosses additional amount, and alcohol ketone crosses content and drops to 2240ppm, CHHP by original 2980ppm
Content drops to 200ppm by 990ppm.
It has used oxidation reaction to feed 60 DEG C of hexamethylenes and has carried out carry out washing tail gas, depth washs alcohol ketone mistake in oxidized tail gas
Content, cause oxidation reaction feed in CHHP drop to 200 ppm, to oxidation reaction inducing action weaken, the life of oxidation reaction
Production capacity power reduces 5-8%.
Due to reducing the content that alcohol ketone is crossed in oxidation charging, especially cyclohexyl hydroperoxide content is reduced, and is being aoxidized
Reaction process improves the content that oxidation solution active principle alcohol ketone is crossed, and reduces the content of by-product acids and ester, 100,000 tons/year of rings
Hexanone device can reduce hexamethylene and consume 500 tons.
Since the cyclohexanol in alkane rectification process hexamethylene and cyclohexanone ketone content are increased to 1200ppm by 800ppm, steam
Vapour consumption can reduce 920kg/h, can save within such 1 year 7360 tons of steam, rectifying column can reduce 2-6 block tower tray.
Claims (8)
1. oxidation unit during a kind of cyclohexane oxidation process production cyclohexanone, mainly by one or more tail gas washing towers, oxygen
Change reactor, regulating valve and pipeline composition, and configures corresponding pipeline and valve；Tail gas washing tower is connected with oxidation reactor,
The oxidized tail gas of automatic oxidation reaction device discharge enters in tower from washing tail gas tower bottom, and the medium temperature hexamethylene come from pipeline is from tail gas
Enter in tower at the top of scrubbing tower, part cyclohexanol, cyclohexanone, cyclohexyl hydroperoxide are condensed and enter hexamethylene in oxidized tail gas
In alkane liquid phase, and flow automatically from washing tail gas tower bottom to oxidation reactor or decomposition reactor, is discharged from washing tail gas top of tower
Oxidized tail gas is discharged into present apparatus oxidized tail gas recovery unit after then summarizing.
2. oxidation unit during cyclohexane oxidation process production cyclohexanone according to claim 1, it is characterised in that tail gas is washed
1 or more oxidation reactors merging 1 tail gas washing tower of setting can be correspondingly arranged with every oxidation reactor by washing tower.
3. oxidation unit during cyclohexane oxidation process production cyclohexanone according to claim 2, it is characterised in that last platform oxygen
Change the connected tail gas washing tower 1 of reactor, or the tail gas washing tower 1 that is connected with Mo Tai and second from the bottom oxidation reactor merging
Platform.
4. oxidation unit during cyclohexane oxidation process production cyclohexanone according to claim 1, it is characterised in that oxidation is anti-
Device is answered to can be 4~7 oxidation reactor series connection.
5. oxidation unit during cyclohexane oxidation process production cyclohexanone according to claim 1, it is characterised in that medium temperature ring
Hexane pipeline is connected with oxidation reaction feeding line.
6. oxidation unit during cyclohexane oxidation process production cyclohexanone according to claim 1, it is characterised in that tail gas is washed
Washing tower is packed tower perhaps one of plate column or a void tower or slack tank；Tower number of theoretical plate is 1~6.
7. oxidation unit during cyclohexane oxidation process production cyclohexanone according to claim 6, it is characterised in that tail gas is washed
Washing tower theoretical cam curve is 1~3.
8. oxidation unit during cyclohexane oxidation process production cyclohexanone according to claim 1, it is characterised in that tail gas is washed
Column overhead portion is washed equipped with thermometer, into the medium temperature hexamethylene pipeline of tail gas washing tower on regulating valve is housed.
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| CN112174790A (en) * | 2019-07-04 | 2021-01-05 | 南京延长反应技术研究院有限公司 | Reinforcing system and process for producing cyclohexanone by cyclohexane oxidation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112174790A (en) * | 2019-07-04 | 2021-01-05 | 南京延长反应技术研究院有限公司 | Reinforcing system and process for producing cyclohexanone by cyclohexane oxidation method |
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