CN105061311B - A kind of process for refining of caprolactam - Google Patents
A kind of process for refining of caprolactam Download PDFInfo
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- CN105061311B CN105061311B CN201510498124.1A CN201510498124A CN105061311B CN 105061311 B CN105061311 B CN 105061311B CN 201510498124 A CN201510498124 A CN 201510498124A CN 105061311 B CN105061311 B CN 105061311B
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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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D201/00—Preparation, separation, purification or stabilisation of unsubstituted lactams
- C07D201/16—Separation or purification
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- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
A kind of caprolactam refining technique of the present invention, the technical process include：Before ion-exchange process is entered, the own liquid of benzene obtained after benzene is extracted carries out alkali cleaning, dehydration, water extraction process.Compared with prior art, caprolactam refining technique provided by the invention, it is included in before water extraction process and the washing of original desalted water twice is changed to alkali cleaning, washing process, the content of ammonium sulfate in feeding liquid is not only reduced, while also reduces the content of organic impurities, process operating load is exchanged so as to mitigate subsequent ion, realize and extend the ion exchange resin life-span, the regenerative operation frequency is reduced, reduces operating cost and labor intensity, improves the purpose of product quality.
Description
Technical field
The invention belongs to epsilon-caprolactams production field, is on a kind of epsilon-caprolactams separating-purifying specifically
Process for refining.
Background technology
Epsilon-caprolactams are one of important source materials of synthetic fibers and synthetic resin, mainly for the manufacture of Fypro
(nylon 6), resin and film etc..At present, industrially from cyclohexanone oxime production caprolactam method be using oleum with
Liquid phase Beckmann rearrangement occurs for cyclohexanone oxime, and rearrangement product need to carry out separating-purifying through following process and refine：Neutralize, benzene extraction
Take, benzene oneself washing, water extraction, ion exchange, hydrogenation, evaporation, distillation etc..The separating-purifying process of rearrangement reaction product is more,
Reason is the presence of inorganic salts ammonium sulfate and reset caused by impurity caused by side reaction.According to prior art, ammonium sulfate
Removing relies primarily on ion-exchange process, and the own aqueous solution of 30% that water is obtained by extraction removes water through anion and cation exchange resin
The inorganic impurities such as the ammonium sulfate remained in solution, and part organic impurities is removed by the suction-operated of the resin, it is other organic
Impurity is then removed by processes such as follow-up hydrogenation, distillations.In current art, even running is produced to ensure, need to generally set two
Set ion-exchange reactions device, a set of operation, a set of regeneration are standby.It is in acidity because ion exchange feeds own aqueous, and anion
The disposal ability of exchanger resin only has the half of cationic ion-exchange resin, thus often cover ion-exchange reactions device include two the moon from
Sub- exchanger and a cation exchanger.When ion-exchange resins diadochy drops to original competent 60% or so or ion friendship
When changing rear feed liquid index arrival controlling value, it is necessary to switching regeneration.Generally, a set of ion exchange resin is run about 7 days
Need to regenerate, and as produce load improves, or impurity content rise, from material Quality Down is surrendered, the regeneration period can shorten to 4
It or so, or even spare resin occur and not yet complete to regenerate, the situation of production requirement can not have been met in spent ion exchange resin.
Need to consume substantial amounts of desalted water, nitric acid, sodium hydroxide in ion-exchange resins regenerative process as regenerative agent, and produce a large amount of waste water,
Therefore ion-exchange process is constantly subjected to that the regeneration period is short, regenerative agent consumption is high in the prior art and that wastewater discharge is big is tired
Disturb.
Referring to Fig. 1, it is prior art process for preparing caprolactam schematic flow sheet.As shown in figure 1, cyclohexanone oxime with
Fuming acid carries out Beckmann rearrangement, and neutralized rearrangement mixture is neutralized, the own liquid of benzene is obtained by extraction in benzene, and the electrical conductivity of the own liquid of benzene is usual
About 80-150 μ s/cm or so.The own liquid a of benzene from benzene extraction draws to enter through the first feeding engine 2 from the own liquid storage tank 1 of benzene and is equipped with
In the coalescer 3 of ceramic packing, desalted water b is added on the suction line of the first feeding engine 2, carries out first time washing, Ran Houzai
Add desalted water b again through the second feeding engine 4 to separate into eddy flow dehydrator 5, carry out second and wash.In the process, portion
The inorganic impurities such as point ammonium sulfate and a small amount of organic impurities enter aqueous phase and removed through being dehydrated from the own liquid of benzene, and the own liquid of benzene is from de- after separation
The top of hydrophone 5 is drawn, the obtained own liquid electrical conductivity of benzene normally about 25-50 μ s/cm or so.Because host inorganic impurity is in the own liquid of benzene
Ammonium sulfate, thus the height of the own liquid electrical conductivity of benzene be correspond to inorganic impurity content number.
The content of the invention
In order to solve the easy saturation of ion exchange resin, regeneration period short insufficient problem, it is necessary to reduce ion exchange resin
Feed impurities content, to extend the purpose in resin regeneration cycle, it is an object of the invention to provide a kind of the refined of caprolactam
Technique, its this method can significantly reduce impurity content in ion exchange resin feeding liquid, reduce resin treatment load, and then extend
Regeneration period.
To reach object defined above, the invention provides following technical scheme, a kind of process for refining of caprolactam, the technique
Process includes：
Before ion-exchange process is entered, the own liquid of benzene obtained after benzene is extracted carries out alkali cleaning, dehydration, water extraction process.
As one preferred embodiment of the invention, the alkali lye that the caustic wash process uses is 10-50% sodium hydroxides
Solution, its dosage are the own liquid of 1-10g/kg benzene.
As one preferred embodiment of the invention, the alkali cleaning is carried out in coalescer, and the dehydration is in dehydrator
Middle progress, the water extraction process are carried out in water extraction tower, and the coalescer, dehydrator and water extraction tower are sequentially connected.
It is connected with the first feeding engine as one preferred embodiment of the invention, before the coalescer, described first
The own liquid storage tank of benzene is connected with before feeding engine, the second feeding engine, the alkali cleaning work are connected between the coalescer and dehydrator
Sequence adds alkali lye position in the porch of first feeding engine.
As one preferred embodiment of the invention, static mixer I is connected with before first feeding engine, it is described
In the porch of static mixer I, the alkali lye passes sequentially through the He of static mixer I for the alkali lye position that adds of caustic wash process
First feeding engine enters the coalescer.
As one preferred embodiment of the invention, static mixing is connected between first feeding engine and coalescer
Device II, the caustic wash process plus alkali lye position in the porch of static mixer II, the alkali lye passes sequentially through described quiet
State blender II enters the coalescer.
As one preferred embodiment of the invention, ceramic packing is filled with the coalescer or is provided with liquid liquid point
From formula filter core.
As one preferred embodiment of the invention, the ceramic packing is Intalox saddle.
As one preferred embodiment of the invention, the temperature of the caustic wash process is 35-50 DEG C, the washing step
35-50 DEG C of temperature, the washing step uses desalted water, and the electrical conductivity of the desalted water is not more than 5 μ s/cm, pH value 5-
7.5。
As one preferred embodiment of the invention, the conductance of the desalted water is no more than 1 μ s/cm, pH value
Between 5.5-6.5.
Beneficial effects of the present invention：Compared with prior art, caprolactam refining technique provided by the invention, is included in water
The washing of original desalted water twice is changed to alkali cleaning, washing process before extraction process, not only reduces containing for ammonium sulfate in feeding liquid
Amount, while the content of organic impurities is also reduced, process operating load is exchanged so as to mitigate subsequent ion, realizes that extending ion hands over
Change resin life, reduce the regenerative operation frequency, reduce operating cost and labor intensity, improve the purpose of product quality.
Brief description of the drawings
Fig. 1 is prior art process for preparing caprolactam schematic flow sheet；
Fig. 2 is caprolactam refining process flow diagram of the present invention.
Embodiment
New technology of the present invention is described in detail with reference to specific embodiment.
" one embodiment " or " embodiment " referred to herein refers to may be included at least one implementation of the present invention
Special characteristic, structure or characteristic." in one embodiment " that different places occur in this manual not refers both to same
Individual embodiment, nor the single or selective embodiment mutually exclusive with other embodiment.
The caprolactam refining technique of the present invention, its before ion-exchange process is entered, the benzene that is obtained after benzene is extracted oneself
Liquid carries out alkali cleaning, dehydration, water extraction process.
Referring to Fig. 2, it is caprolactam refining process flow diagram of the present invention.As shown in Fig. 2 the alkali cleaning is poly-
Being carried out in knot device 23, the dehydration is carried out in dehydrator 25, and the water extraction process is carried out in water extraction tower (not shown),
The coalescer 23, dehydrator 25 and water extraction tower are sequentially connected.The first feeding engine 22, institute are connected with before the coalescer 23
The own liquid storage tank 21 of benzene is connected with before stating the first feeding engine 22, the second feeding is connected between the coalescer 23 and dehydrator 25
Pump 24, the caustic wash process add alkali lye f positions in the porch of first feeding engine 22.
The own liquid a of benzene from benzene extraction is drawn by the own liquid storage tank 21 of benzene, is sent to coalescer via the first feeding engine 22 before this
23, alkali lye f can inject before the entrance of the first feeding engine 22, (not shown) mixed by impeller in the pump housing of the first feeding engine 22
Cooperation mixes the laggard coalescer 23.Alkali lye f also can be on the import or export pipeline installed in the first feeding engine 22
Introduced before static mixer 26, laggard coalescer 23 is sufficiently mixed with the own liquid of benzene in static mixer 26.Coalescer 23 is one
The vertical equipment of built-in coalescent pack, wire feeding can be ceramic coalescent packs, also can be hydro carbons dealkalize liquid liquid single-purpose filtering element
To realize cohesion, sedimentation, separation of the alkali droplet in the own solution system of benzene.Due to alkali lye f addition, on the one hand make aqueous phase close
Degree rise, increase with organic phase density contrast, be easy to organic phase separation, on the other hand, alkali lye f can be to carrying secretly in the own liquid of benzene
Sulfur trioxide and organic impurities carry out alkali cleaning, impurity is separated after entering aqueous phase, improve the own liquid quality of benzene.The own liquid of benzene is afterwards
Desalted water is introduced before two feeding engines 24, spinning liquid dehydrator is entered after being sufficiently mixed in the pump housing of the second feeding engine 24 with the own liquid of benzene
25 carry out dehydration separation.In dehydrator 25, inorganic impurity in being soluble in the aqueous phase by centrifuge principle and organic phase-benzene oneself
Liquid is kept completely separate, it is ensured that organic phase is to carry impurity content in the own liquid of benzene secretly to minimize.
Added concentration of lye can be between 10%-50% in the present invention, the liquid sodium hydroxide of preferably 30%, 42% or 45%
Solution, addition are the own liquid of 1-10g/kg benzene, it is desirable to which the control discharging own liquid caustic soda degree of benzene is less than 5mmol/kg, preferably smaller than 1mmol/
Kg, more preferably less than 0.5mmol/kg, washing are 10-25g/kg with desalination water consumption.
In the inventive method, add the electrical conductivity of the own liquid of benzene before alkali generally between 80-150 μ s/cm, extinction value about 1.0-
1.5 (290nm), after alkali cleaning, washing process, the electrical conductivity of the own liquid of benzene can be down to 5-15 μ s/cm, and extinction value can be down to 0.6-
0.9, so that being extracted through water, the own aqueous electrical conductivity into ion-exchange process accordingly reduces, i.e. the place of ion exchange resin
Reason load substantially mitigates.
In method provided by the invention, its alkaline cleaning procedure condition is：35-50 DEG C of operation temperature, washing conditions are：Operation temperature
35-50 DEG C of degree, washing are not more than 5 μ s/cm with desalination water conductivity, and preferably no greater than 1 μ s/cm, pH value is excellent between 5-7.5
It is selected between 5.5-6.5.Gained aqueous phase is returned in the own tank of benzene from top after alkali cleaning and dehydration separation, and the own liquid of benzene is washed again
De-, aqueous phase under gravity, from the own pot bottom discharge of benzene after sedimentation separation, delivers to water treatment system after elution.
The change of inorganic impurity content and however, residual base in the own liquid of benzene before and after the processing are evaluated in the present invention with the following method
Liquid hold-up：
The own liquid conductance measurement of benzene
With the 100mL graduated cylinders dried, measure 100mL samples and inject in a dry separatory funnel, add 25mL water,
With stratification after forced oscillation one minute, aqueous phase is transferred in 50mL beakers in tall form, measures the electrical conductivity of sample.
The acid-base value measure of the own liquid of benzene
With the 100mL pipettes dried, measure 100mL samples and inject in a dry separatory funnel, add 25mL
Neutral distillation water, with stratification after forced oscillation one minute, aqueous phase is transferred in 50mL beakers in tall form, if solution is in aubergine
Acidity is then expressed as, it is in celadon to be titrated to solution with 0.01N standard titration solutions, and alkalescence is expressed as if solution is in green,
It is in celadon to be titrated to solution with 0.01N Hydrochloric Standard Titrations.The acid-base value x of the own liquid of benzene represents that it is calculated with mmol/L
Formula is：
X=cV*10
The measure of the own liquid extinction value of benzene
The own liquid sample about 50mL of benzene is taken, is injected in 1cm silica cuvettes, analysis is injected into another quartz with tertiary effluent and inhaled
In receives pond.At 290nm, reference is made with water, absorbance A 1 is measured with ultraviolet specrophotometer, is entered with water instead of the own liquid sample of benzene
Line blank determines, and measured value is the corrected value A0 of absorption cell, and corrected value cannot be greater than 0.003.The extinction value of the own liquid of benzene calculates public
Formula is：
X=A1-A0
Embodiment 1
Cyclohexanone oxime (purity 99.95%) and fuming acid are extracted by Beckmann rearrangement, then neutralized, benzene is carried out
Take, obtain the own liquid of benzene.The own liquid index of benzene：Electrical conductivity：83 μ s/cm, extinction value 1.04.The own liquid a of benzene from benzene extraction is from benzene
Own liquid storage tank 21 is drawn, and is being sent into through the first feeding engine 22 with alkali lye after the pump housing of the first feeding engine 22 mixes in coalescer 23,
Alkali lye is 42% mass concentration sodium hydroxide solution, and addition is the own liquid of 2g/kg benzene, loads coalescent pack in coalescer 23, fills out
Material pattern is ceramic saddle/rings (Intalox), and in the upper part discharge port sampling analysis of coalescer 23, now the own liquid electrical conductivity of benzene is 28
μs/cm.(underlying liquid d) is drawn the aqueous phase for condensing to obtain in coalescer 23 from bottom, is sent into the own liquid of benzene from top through recurrent canal and is stored up
Tank 21.From the own liquid of benzene that the top of coalescer 23 is drawn through the second feeding engine 24 and the desalted water in the introducing of the entrance of the second feeding engine 24
C mixes in the second feeding engine 24, subsequently enters rotation dehydrator 25.Injection desalination water conductivity is less than 1 μ s/cm, and amount of water is
The own liquid of 12g/kg benzene, the cyclone pipe of the inside of dehydrator 25 filling separation minor amount of water, the own liquid of benzene is by the top of dehydrator 25 after dehydration
Draw, go water extraction tower e to be sent to ion-exchange process, (underlying liquid d) is drawn aqueous phase by the bottom of dehydrator 25, through recurrent canal from top
Portion is sent into the own liquid storage tank 21 of benzene.To the own liquid sampling analysis of benzene of Base top contact, the own liquid electrical conductivity of benzene is 12 μ s/cm herein, delustring
Value 0.66, basicity 0.2mmol/L.Wherein, the underlying liquid in the own liquid storage tank 21 of benzene enters water process b by bottom liquid pump 27.
Embodiment 2
By cyclohexanone oxime (purity 99.95%) and fuming acid by Beckmann rearrangement is carried out, then neutralized, benzene extraction, obtain
To the own liquid of benzene.The own liquid index of benzene：Electrical conductivity：107 μ s/cm, extinction value 1.27.The own liquid a of benzene from benzene extraction is from the own liquid of benzene
Storage tank 21 is drawn, through the first feeding engine 22, the alkali in the static mixer 26 on the suction line of the first feeding engine 22 with introducing
Liquid mixes, and is sent into coalescer 23, and alkali lye is 30% mass concentration sodium hydroxide solution, and addition is the own liquid of 3.5g/kg benzene, gathers
Coalescent pack is loaded in knot device 23, filler pattern is ceramic saddle/rings (Intalox), in the sampling point of the upper part discharge port of coalescer 23
Analysis, now the own liquid electrical conductivity of benzene is 25 μ s/cm.Condense obtained aqueous phase in coalescer 23 to draw from bottom, through recurrent canal from top
Portion is sent into the own liquid storage tank 21 of benzene.The own liquid of benzene drawn from the top of coalescer 23 is through the second feeding engine 24 with entering in the second feeding engine 24
The desalted water c that mouth introduces mixes in the pump housing, subsequently enters liquid rotary type dehydrator 25.Injection desalination water conductivity is less than 1 μ s/cm,
Amount of water is the own liquid of 18g/kg benzene, and the cyclone pipe of the inside of dehydrator 25 filling separation minor amount of water, the own liquid of benzene is by being dehydrated after dehydration
The Base top contact of device 25, water extraction tower e is gone to be sent to ion-exchange process, (underlying liquid d) is drawn aqueous phase by dehydrator bottom, through returning
Pipe is sent into the own liquid storage tank 21 of benzene from top.To the own liquid sampling analysis of benzene of Base top contact, the own liquid electrical conductivity of benzene is 9 μ s/cm herein,
Extinction value 0.81, basicity 0.3mmol/L.
Embodiment 3
By cyclohexanone oxime (purity 99.95%) and fuming acid by Beckmann rearrangement is carried out, then neutralized, benzene extraction, obtain
The own liquid of benzene.The own liquid index of benzene：Electrical conductivity：95 μ s/cm, extinction value 1.13.The own liquid a of benzene from benzene extraction is from the own liquid storage tank of benzene
21 bottoms are drawn, and are being sent into through the first feeding engine 22 with alkali lye after the first feeding engine 22 mixes in coalescer 23, alkali lye 20%
Mass concentration sodium hydroxide solution, addition are the own liquid of 9g/kg benzene, and caustic alkali liquid liquid in separating hydrocarbons is loaded in coalescer 23
Coalescer filter element, LCS2H1AH, 45 DEG C of operation temperature, pressure is normal pressure, in coalescer upper part discharge port sampling analysis, now benzene
Own liquid electrical conductivity is 28 μ s/cm.(underlying liquid d) is drawn the aqueous phase for condensing to obtain in coalescer from bottom, through recurrent canal from top
It is sent into the own liquid storage tank 21 of benzene.From the own liquid of benzene that the top of coalescer 23 is drawn through the second feeding engine 24 and in the entrance of the second feeding engine 24
The desalted water of introducing mixes in the pump housing, subsequently enters liquid rotary type dehydrator 25.Injection desalination water conductivity is less than 1 μ s/cm, adds water
Measure the own liquid of 10g/kg benzene for the own liquid of benzene, the cyclone pipe of the inside of dehydrator 25 filling separation minor amount of water, after dehydration the own liquid of benzene by
Dehydrator Base top contact, water extraction tower e is gone to be sent to ion-exchange process, aqueous phase (d：Underlying liquid) drawn by the bottom of dehydrator 25,
Through recurrent canal the own liquid storage tank 21 of benzene is sent into from top.To the own liquid sampling analysis of benzene of Base top contact, the own liquid electrical conductivity of benzene is 8 herein
μ s/cm, extinction value 0.73, basicity 0.3mmol/L.
Control experiment
By cyclohexanone oxime (purity 99.95%) and fuming acid by Beckmann rearrangement is carried out, then neutralized, benzene extraction, obtain
The own liquid of benzene.The own liquid index of benzene：Electrical conductivity：95 μ s/cm, extinction value 1.13.After the own liquid of benzene is drawn from the own liquid storage tank bottom of benzene, point
Not in the first feeding engine 1, the entrance of the second feeding engine 2 introduce desalted water, twice the addition of desalted water be 15g/kg benzene oneself
Liquid, to the own liquid sampling analysis of benzene of dehydrator Base top contact, electrical conductivity is 28 μ s/cm, extinction value 0.92, acidity 2.0mmol/L.
Caprolactam refining technique provided by the invention, it is by water extraction tower charging being in advance to add alkali in the own liquid of benzene
Liquid, the inorganic impurity and organic impurities for making the own liquid entrainment of original benzene more easily enter aqueous phase in coalescer and dehydrator and removed
Go, to ensure that alkali lye is not brought into rear process, the own liquid of the benzene after alkali cleaning by washing, is reduced in the own liquid of benzene so as to realize again
The content of inorganic impurity and organic impurities, mitigate the purpose of ion exchange resin treatment load.
It should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to preferable
The present invention is described in detail embodiment, it will be understood by those within the art that, can be to the technology of the present invention
Scheme is modified or equivalent substitution, and without departing from the spirit and scope of technical solution of the present invention, it all should cover in this hair
Among bright right.
Claims (5)
- A kind of 1. caprolactam refining technique, it is characterised in that：The technical process includes：, will before ion-exchange process is entered The own liquid of benzene obtained after benzene extraction carries out alkali cleaning, dehydration, washing step and water extraction process, the alkali lye that the caustic wash process uses For 10-50% sodium hydroxide solutions, the alkali lye dosage is the own liquid of 1-10g/kg benzene；The temperature of the caustic wash process is 35-50 DEG C, 35-50 DEG C of the temperature of the washing step, the washing step uses desalted water, and the electrical conductivity of the desalted water is not more than 5 μ s/cm, pH value 5-7.5；The alkali cleaning is carried out in coalescer, and the dehydration is carried out in dehydrator, and the water extracts work Sequence is carried out in water extraction tower, and the coalescer, dehydrator and water extraction tower are sequentially connected, and the is connected with before the coalescer One feeding engine, first feeding engine are connected with the own liquid storage tank of benzene before, second are connected between the coalescer and dehydrator Feeding engine, the caustic wash process add alkali lye position in the porch of first feeding engine.
- 2. caprolactam refining technique according to claim 1, it is characterised in that：It is connected with before first feeding engine Static mixer I, the caustic wash process add alkali lye position to be passed sequentially through in the porch of static mixer I, the alkali lye The feeding engine of static mixer I and first enters the coalescer.
- 3. caprolactam refining technique according to claim 1, it is characterised in that：First feeding engine and coalescer it Between be connected with static mixer II, the caustic wash process plus alkali lye position in the porch of static mixer II, the alkali Liquid passes sequentially through the static mixer II and enters the coalescer.
- 4. caprolactam refining technique according to claim 1, it is characterised in that：Ceramics are filled with the coalescer to fill out Expect or be provided with Liquid liquid Separation formula filter core.
- 5. caprolactam refining technique according to claim 4, it is characterised in that：The ceramic packing is that square saddle type is filled out Material.
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| CN107556240B (en) * | 2016-08-24 | 2020-10-30 | 沧州旭阳化工有限公司 | Caprolactam refining method and system |
| CN107118156B (en) * | 2017-06-26 | 2020-08-28 | 山东清创化工有限公司 | Caprolactam separation and refining process |
| CN109694349B (en) * | 2017-10-24 | 2022-10-14 | 中国石油化工股份有限公司 | Caprolactam refining method |
| CN111229332A (en) * | 2020-02-14 | 2020-06-05 | 福建永荣科技有限公司 | Device for washing caprolactam to improve period of ion-exchange resin |
| CN111875542A (en) * | 2020-07-03 | 2020-11-03 | 聊城鲁西聚酰胺新材料科技有限公司 | Refining method of caprolactam extraction liquid |
| CN111848325B (en) * | 2020-07-14 | 2023-05-09 | 中国石油化工股份有限公司 | Method and system for alkaline washing of cumene raw material by CHPPO device |
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