CN105061311A - Caprolactam refining technology - Google Patents
Caprolactam refining technology Download PDFInfo
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- CN105061311A CN105061311A CN201510498124.1A CN201510498124A CN105061311A CN 105061311 A CN105061311 A CN 105061311A CN 201510498124 A CN201510498124 A CN 201510498124A CN 105061311 A CN105061311 A CN 105061311A
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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)
- Treatment Of Water By Ion Exchange (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a caprolactam refining technology comprising steps as follows: before an ion exchange procedure, performing alkaline washing, dehydration and water extraction procedures on benzene caproate solution obtained after benzene extraction. Compared with the prior art, the caprolactam refining technology has the advantages that before the water extraction procedure, two times of desalted water washing technologies are changed into alkaline washing and water washing technologies, so that the content of ammonium sulfate in a fed liquid is decreased, meanwhile, the content of organic impurities is decreased, the running load in the follow-up ion exchange procedure is reduced, the service life of ion exchange resin is prolonged, the reoperation frequency is reduced, the running cost and the labor intensity are reduced, and the product quality is improved.
Description
Technical field
The invention belongs to ε-caprolactam production field, specifically, is the process for refining about a kind of ε-caprolactam separating-purifying.
Background technology
ε-caprolactam is one of important source material of synthon and synthetic resins, mainly for the manufacture of tynex (nylon 6), resin and film etc.At present, the industrial method from cyclohexanone-oxime production hexanolactam adopts oleum and cyclohexanone-oxime generation liquid phase Beckmann rearrangement, and rearrangement product need carry out separating-purifying through following operation and refine: neutralization, benzene extraction, benzene own washing, water extraction, ion-exchange, hydrogenation, evaporation, distillation etc.The separating-purifying operation of rearrangement reaction product is more, and the impurity that the existence of reason inorganic salt ammonium sulfate and rearrangement side reaction produce causes.According to prior art, removing of ammonium sulfate mainly relies on ion-exchange process, water is extracted the 30% own aqueous solution that obtains through anion and cation exchange resin, the inorganic impurities such as ammonium sulfate residual in the removing aqueous solution, and passing through the adsorption remove portion organic impurity of this resin, other organic impurity is then by the removing of the operation such as follow-up hydrogenation, distillation.In current art, for ensureing production smooth running, usually need arrange two cover ion exchange reaction devices, a set of operation, a set of regeneration is for subsequent use.Because the own water liquid of ion-exchange charging is in acid, and the processing power of anionite-exchange resin only has the half of Zeo-karb, therefore often overlaps ion exchange reaction device and comprises two anion exchangers and a cation exchanger.When ion-exchange resins replacing power drops to feed liquid index arrival controlling valu after former competent about 60% or ion-exchange, just need to switch regeneration.Generally, namely a set of ion exchange resin runs needs regeneration for about 7 days, and along with the raising of production load, or foreign matter content raises, from surrendering material Quality Down, regeneration period can shorten to about 4 days, even occurs that spare resin not yet completes regeneration, can not meet the situation of production requirement at spent ion exchange resin.Need a large amount of de-salted water of consumption, nitric acid, sodium hydroxide as regenerator, and to produce a large amount of waste water in ion-exchange resins regenerative process, therefore prior art intermediate ion exchanges operation and is subject to the puzzlement that the regeneration period is short, regenerator consumption is high and wastewater discharge is large always.
Refer to Fig. 1, it is prior art process for preparing caprolactam schematic flow sheet.As shown in Figure 1, cyclohexanone-oxime and fuming acid carry out Beckmann rearrangement, and neutralized rearrangement mixture obtains the own liquid of benzene through neutralization, benzene extraction, specific conductivity about 80-150 μ about the s/cm usually of the own liquid of benzene.Benzene own liquid a from benzene extraction draws to enter through the first take away pump 2 and is equipped with in the coalescer 3 of ceramic packing in the own liquid storage tank 1 of benzene, first take away pump 2 source line adds de-salted water b, carry out first time washing, and then again add de-salted water b through the second take away pump 4 and enter eddy flow water trap 5 and be separated, carry out second time washing.In the process, the inorganic impurities such as part of sulfuric acid ammonium and a small amount of organic impurity enter aqueous phase and remove from the own liquid of benzene through dehydration, and after being separated, the own liquid of benzene is drawn from water trap 5 top, and the own liquid specific conductivity of the benzene obtained is about 25-50 μ about s/cm usually.Because in the own liquid of benzene, host inorganic impurity is ammonium sulfate, therefore namely the height of the own liquid specific conductivity of benzene correspond to the number of inorganic impurity content.
Summary of the invention
Easily saturated in order to solve ion exchange resin, the not enough problem that regeneration period is short, ion exchange resin feed impurities content must be reduced, to extend the object in resin regeneration cycle, the object of the present invention is to provide a kind of process for refining of hexanolactam, its the method can significantly reduce foreign matter content in ion exchange resin feeding liquid, reduces plastic resin treatment load, and then extends the regeneration period.
For reaching aforementioned object, the invention provides following technical scheme, a kind of process for refining of hexanolactam, this technological process comprises:
Before entering ion-exchange process, the own liquid of benzene obtained after being extracted by benzene carries out alkali cleaning, dehydration, water extraction process.
As the present invention one preferred embodiment, the alkali lye that described caustic wash process uses is 10-50% sodium hydroxide solution, and its consumption is the own liquid of 1-10g/kg benzene.
As the present invention one preferred embodiment, described alkali cleaning is carried out in coalescer, and described dehydration is carried out in water trap, and described water extraction process carries out in water extraction tower, and described coalescer, water trap are connected successively with water extraction tower.
As the present invention one preferred embodiment, the first take away pump is connected with before described coalescer, the own liquid storage tank of benzene is connected with before described first take away pump, be connected with the second take away pump between described coalescer and water trap, described caustic wash process add the ingress of alkali lye position at described first take away pump.
As the present invention one preferred embodiment, static mixer I is connected with before described first take away pump, described caustic wash process add alkali lye position in described static mixer I ingress, described alkali lye enters described coalescer by described static mixer I and the first take away pump successively.
As the present invention one preferred embodiment, static mixer II is connected with between described first take away pump and coalescer, described caustic wash process add alkali lye position in described static mixer II ingress, described alkali lye enters described coalescer by described static mixer II successively.
As the present invention one preferred embodiment, be filled with ceramic packing in described coalescer or be provided with Liquid liquid Separation formula filter core.
As the present invention one preferred embodiment, described ceramic packing is Intalox saddle packing.
As the present invention one preferred embodiment, the temperature of described caustic wash process is the temperature 35-50 DEG C of 35-50 DEG C, described washing step, and described washing step adopts de-salted water, and described desalination electrical conductivity of water is not more than 5 μ s/cm, pH value is 5-7.5.
As the present invention one preferred embodiment, the electric conductivity of described de-salted water is not more than 1 μ s/cm, pH value is between 5.5-6.5.
Beneficial effect of the present invention: compared with prior art, caprolactam refining technique provided by the invention, original twice de-salted water washing is changed into alkali cleaning, washing process before being included in water extraction process, not only reduce the content of ammonium sulfate in feeding liquid, also reduce the content of organic impurity simultaneously, thus alleviate subsequent ion exchange operation operating load, realize extending the ion exchange resin life-span, reduce the regenerative operation frequency, reduce working cost and labour intensity, the object of improving the quality of products.
Accompanying drawing explanation
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
Below in conjunction with specific embodiment, novel process of the present invention is described in detail.
Alleged herein " embodiment " or " embodiment " refers to special characteristic, structure or the characteristic that can be contained at least one implementation of the present invention.Different local in this manual " in one embodiment " occurred not all refers to same embodiment, neither be independent or optionally mutually exclusive with other embodiments embodiment.
Caprolactam refining technique of the present invention, it is before entering ion-exchange process, and the own liquid of benzene obtained after being extracted by benzene carries out alkali cleaning, dehydration, water extraction process.
Refer to Fig. 2, it is caprolactam refining process flow diagram of the present invention.As shown in Figure 2, described alkali cleaning is carried out in coalescer 23, and described dehydration is carried out in water trap 25, and described water extraction process carries out in water extraction tower (not shown), and described coalescer 23, water trap 25 are connected successively with water extraction tower.The first take away pump 22 is connected with before described coalescer 23, the own liquid storage tank 21 of benzene is connected with before described first take away pump 22, be connected with the second take away pump 24 between described coalescer 23 and water trap 25, described caustic wash process add the ingress of alkali lye f position at described first take away pump 22.
Benzene own liquid a from benzene extraction is drawn by the own liquid storage tank 21 of benzene, coalescer 23 was sent to before this via the first take away pump 22, alkali lye f can inject before the first take away pump 22 entrance, by the laggard described coalescer 23 of impeller (not shown) mixing effect mixing in the pump housing of the first take away pump 22.Alkali lye f also can introduce before the static mixer 26 on the import or export pipeline being arranged on the first take away pump 22, and in static mixer 26, liquid own with benzene fully mixes laggard coalescer 23.Coalescer 23 is the vertical equipment of an in-built coalescent pack, and wire feeding can be ceramic coalescent pack, also can be hydro carbons dealkalize liquid liquid single-purpose filtering element to realize the cohesion of alkali droplet in the own solution system of benzene, sedimentation, separation.Due to adding of alkali lye f, on the one hand aqueous phase densities is raised, increase and organic phase density difference, be convenient to be separated with organic phase, on the other hand, alkali lye f can carry out alkali cleaning to the sulphur trioxide carried secretly in the own liquid of benzene and organic impurity, be separated after making impurity enter aqueous phase, improve the own liquid quality of benzene.The own liquid of benzene introduces de-salted water before the second take away pump 24 afterwards, enters spinning liquid water trap 25 carry out dehydration and be separated in the pump housing of the second take away pump 24 with the own liquid of benzene after fully mixing.In water trap 25, the inorganic impurity in being soluble in the aqueous phase is separated with the own liquid of organic phase-benzene completely by centrifugation principle, ensure that carrying foreign matter content secretly in organic phase and the own liquid of benzene is down to minimum.
In the present invention, added concentration of lye can between 10%-50%, preferably 30%, 42% or 45% liquid sodium hydroxide solution, add-on is the own liquid of 1-10g/kg benzene, require that controlling the own liquid caustic soda degree of discharging benzene is less than 5mmol/kg, preferably be less than 1mmol/kg, preferably be less than 0.5mmol/kg, washing de-salted water consumption is 10-25g/kg.
In the inventive method, add the specific conductivity of the own liquid of benzene before alkali usually between 80-150 μ s/cm, extinction value is about 1.0-1.5 (290nm), after alkali cleaning, washing process, the specific 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, thus makes to extract through water, enter the corresponding reduction of own water liquid specific conductivity of ion-exchange process, namely the processing load of ion exchange resin obviously alleviates.
In method provided by the invention, its alkaline cleaning procedure condition is: service temperature 35-50 DEG C, and washing conditions is: service temperature 35-50 DEG C, washing de-salted water specific conductivity is not more than 5 μ s/cm, preferably be not more than 1 μ s/cm, pH value between 5-7.5, preferably between 5.5-6.5.After alkali cleaning and dehydration are separated, gained aqueous phase returns to the own tank of benzene from top, and carry out wash-out again to the own liquid of benzene, after wash-out, aqueous phase under gravity, discharges, deliver to water treatment system after settlement separate from the own pot bottom of benzene.
The change and however, residual base liquid hold-up of evaluating inorganic impurity content in the own liquid of benzene before and after process is with the following method adopted in the present invention:
The own liquid conductance measurement of benzene
With the 100mL graduated cylinder of a drying, measure 100mL sample and inject a dry separating funnel, add 25mL water, with forced oscillation stratification after a minute, aqueous phase is transferred in 50mL tall form beaker, measure the specific conductivity of sample.
The potential of hydrogen of the own liquid of benzene measures
With the 100mL transfer pipet of a drying, measure 100mL sample and inject a dry separating funnel, add 25mL neutral distillation water, with forced oscillation stratification after a minute, transferred to by aqueous phase in 50mL tall form beaker, if solution is red-purple, be expressed as acidity, being titrated to solution with 0.01N standard titration solution is greyish-green, if solution is green, be expressed as alkalescence, being titrated to solution with 0.01N Hydrochloric Standard Titration is greyish-green.The potential of hydrogen x of the own liquid of benzene represents with mmol/L, and its calculation formula is:
x＝cV*10
The mensuration of the own liquid extinction value of benzene
Get the own liquid sample of benzene and be about 50mL, inject 1cm silica cuvette, analysis tertiary effluent is injected another silica cuvette.At 290nm place, make reference with water, measure absorbance A 1 with ultraviolet spectrophotometer, replace the own liquid sample of benzene to carry out blank determination with water, measured value is the correction value A0 of cuvette, and correction value must not be greater than 0.003.The extinction value calculation formula of the own liquid of benzene is:
x＝A1-A0
Embodiment 1
By cyclohexanone-oxime (purity 99.95%) and fuming acid by carrying out Beckmann rearrangement, then through neutralization, benzene extraction, obtain the own liquid of benzene.The own liquid index of benzene: specific conductivity: 83 μ s/cm, extinction value is 1.04.Benzene own liquid a from benzene extraction draws from the own liquid storage tank 21 of benzene, send in coalescer 23 with alkali lye through the first take away pump 22 after the pump housing of the first take away pump 22 mixes, alkali lye is 42% mass concentration sodium hydroxide solution, add-on is the own liquid of 2g/kg benzene, coalescent pack is loaded in coalescer 23, filler pattern is ceramic saddle/rings (Intalox), and at coalescer 23 upper part discharge port sampling analysis, now the own liquid specific conductivity of benzene is 28 μ s/cm.The aqueous phase (underlying liquid d) obtained that condenses in coalescer 23 is drawn from bottom, sends into the own liquid storage tank 21 of benzene through return tube from top.The own liquid of benzene of drawing from coalescer 23 top mixes at the second take away pump 24 with the de-salted water c introduced at the second take away pump 24 entrance through the second take away pump 24, enters subsequently and revolves water trap 25.Inject de-salted water specific conductivity and be less than 1 μ s/cm, amount of water is the own liquid of 12g/kg benzene, the filling of water trap 25 inside is separated the cyclone pipe of minor amount of water, after dehydration, the own liquid of benzene is by water trap 25 Base top contact, the extraction tower e that anhydrates is sent to ion-exchange process, aqueous phase (underlying liquid d) is drawn by bottom water trap 25, sends into the own liquid storage tank 21 of benzene through return tube from top.To the own liquid sampling analysis of the benzene of Base top contact, the own liquid specific conductivity of benzene is 12 μ s/cm herein, extinction value 0.66, basicity 0.2mmol/L.Wherein, the underlying liquid in the own liquid storage tank 21 of benzene enters water treatment b by bottom liquid pump 27.
Embodiment 2
By cyclohexanone-oxime (purity 99.95%) and fuming acid by carrying out Beckmann rearrangement, then through neutralization, benzene extraction, obtain the own liquid of benzene.The own liquid index of benzene: specific conductivity: 107 μ s/cm, extinction value is 1.27.Benzene own liquid a from benzene extraction draws from the own liquid storage tank 21 of benzene, through the first take away pump 22, mix with the alkali lye introduced in static mixer 26 on the first take away pump 22 source line, send in coalescer 23, alkali lye is 30% mass concentration sodium hydroxide solution, and add-on is the own liquid of 3.5g/kg benzene, coalescent pack is loaded in coalescer 23, filler pattern is ceramic saddle/rings (Intalox), and at coalescer 23 upper part discharge port sampling analysis, now the own liquid specific conductivity of benzene is 25 μ s/cm.The aqueous phase obtained that condenses in coalescer 23 is drawn from bottom, sends into the own liquid storage tank 21 of benzene through return tube from top.The own liquid of benzene of drawing from coalescer 23 top mixes at the pump housing with the de-salted water c introduced at the second take away pump 24 entrance through the second take away pump 24, enters cyclone flow type water trap 25 subsequently.Inject de-salted water specific conductivity and be less than 1 μ s/cm, amount of water is the own liquid of 18g/kg benzene, the filling of water trap 25 inside is separated the cyclone pipe of minor amount of water, after dehydration, the own liquid of benzene is by water trap 25 Base top contact, the extraction tower e that anhydrates is sent to ion-exchange process, aqueous phase (underlying liquid d) is drawn by bottom water trap, sends into the own liquid storage tank 21 of benzene through return tube from top.To the own liquid sampling analysis of the benzene of Base top contact, the own liquid specific 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 carrying out Beckmann rearrangement, then through neutralization, benzene extraction, obtain the own liquid of benzene.The own liquid index of benzene: specific conductivity: 95 μ s/cm, extinction value is 1.13.Benzene own liquid a from benzene extraction draws from benzene own liquid storage tank 21 bottom, send in coalescer 23 with alkali lye through the first take away pump 22 after the first take away pump 22 mixes, alkali lye is 20% mass concentration sodium hydroxide solution, add-on is the own liquid of 9g/kg benzene, loads caustic alkali liquid liquid coalescer filter core in separating hydrocarbons, LCS2H1AH in coalescer 23, service temperature 45 DEG C, pressure is normal pressure, and at coalescer upper part discharge port sampling analysis, now the own liquid specific conductivity of benzene is 28 μ s/cm.The aqueous phase (underlying liquid d) obtained that condenses in coalescer is drawn from bottom, sends into the own liquid storage tank 21 of benzene through return tube from top.The own liquid of benzene of drawing from coalescer 23 top mixes at the pump housing with the de-salted water introduced at the second take away pump 24 entrance through the second take away pump 24, enters cyclone flow type water trap 25 subsequently.Inject de-salted water specific conductivity and be less than 1 μ s/cm, amount of water is the own liquid of 10g/kg benzene of the own liquid of benzene, the filling of water trap 25 inside is separated the cyclone pipe of minor amount of water, after dehydration, the own liquid of benzene is by water trap Base top contact, the extraction tower e that anhydrates is sent to ion-exchange process, aqueous phase (d: underlying liquid) is drawn by bottom water trap 25, sends into the own liquid storage tank 21 of benzene through return tube from top.To the own liquid sampling analysis of the benzene of Base top contact, the own liquid specific conductivity of benzene is 8 μ s/cm herein, extinction value 0.73, basicity 0.3mmol/L.
Control experiment
By cyclohexanone-oxime (purity 99.95%) and fuming acid by carrying out Beckmann rearrangement, then through neutralization, benzene extraction, obtain the own liquid of benzene.The own liquid index of benzene: specific conductivity: 95 μ s/cm, extinction value is 1.13.The own liquid of benzene is after the own liquid storage tank bottom of benzene is drawn, respectively at the de-salted water that the first take away pump 1, second take away pump 2 entrance is introduced, the addition of twice de-salted water is the own liquid of 15g/kg benzene, to the own liquid sampling analysis of the benzene of water trap Base top contact, specific conductivity is 28 μ s/cm, extinction value 0.92, acidity 2.0mmol/L.
Caprolactam refining technique provided by the invention, it by adding alkali lye in advance in the charging of water extraction tower and the own liquid of benzene, the inorganic impurity that the own liquid of original benzene is carried secretly and organic impurity more easily enter aqueous phase removing in coalescer and water trap, for ensureing that alkali lye is not brought into rear operation, the own liquid of benzene after alkali cleaning is again through washing, thus realize the content reducing inorganic impurity and organic impurity in the own liquid of benzene, alleviate the object of ion exchange resin treatment load.
It should be noted that, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (10)
1. a caprolactam refining technique, is characterized in that: this technological process comprises:
Before entering ion-exchange process, the own liquid of benzene obtained after being extracted by benzene carries out alkali cleaning, dehydration, water extraction process.
2. caprolactam refining technique according to claim 1, is characterized in that: the alkali lye that described caustic wash process uses is 10-50% sodium hydroxide solution, and described alkali lye consumption is the own liquid of 1-10g/kg benzene.
3. caprolactam refining technique according to claim 1, it is characterized in that: described alkali cleaning is carried out in coalescer, described dehydration is carried out in water trap, and described water extraction process carries out in water extraction tower, and described coalescer, water trap are connected successively with water extraction tower.
4. caprolactam refining technique according to claim 3, it is characterized in that: before described coalescer, be connected with the first take away pump, the own liquid storage tank of benzene is connected with before described first take away pump, be connected with the second take away pump between described coalescer and water trap, described caustic wash process add the ingress of alkali lye position at described first take away pump.
5. caprolactam refining technique according to claim 4, it is characterized in that: before described first take away pump, be connected with static mixer I, described caustic wash process add alkali lye position in described static mixer I ingress, described alkali lye enters described coalescer by described static mixer I and the first take away pump successively.
6. caprolactam refining technique according to claim 4, it is characterized in that: between described first take away pump and coalescer, be connected with static mixer II, described caustic wash process add alkali lye position in described static mixer II ingress, described alkali lye enters described coalescer by described static mixer II successively.
7. caprolactam refining technique according to claim 3, is characterized in that: be filled with ceramic packing in described coalescer or be provided with Liquid liquid Separation formula filter core.
8. caprolactam refining technique according to claim 7, is characterized in that: described ceramic packing is Intalox saddle packing.
9. caprolactam refining technique according to claim 1, it is characterized in that: the temperature of described caustic wash process is 35-50 DEG C, the temperature 35-50 DEG C of described washing step, described washing step adopts de-salted water, and described desalination electrical conductivity of water is not more than 5 μ s/cm, pH value is 5-7.5.
10. caprolactam refining technique according to claim 9, is characterized in that: the electric conductivity of described de-salted water is not more than 1 μ s/cm, pH value is between 5.5-6.5.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107118156A (en) * | 2017-06-26 | 2017-09-01 | 山东清创化工有限公司 | A kind of caprolactam separation and purification technique |
| CN107556240A (en) * | 2016-08-24 | 2018-01-09 | 沧州旭阳化工有限公司 | A kind of system of caprolactam refining method and refined caprolactam |
| CN109694349A (en) * | 2017-10-24 | 2019-04-30 | 中国石油化工股份有限公司 | A kind of method of caprolactam refining |
| 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 |
| CN111848325A (en) * | 2020-07-14 | 2020-10-30 | 中国石油化工股份有限公司 | Method and system for washing cumene raw material with alkali by using CHPPO (chlorinated Polypropylene oxide) device |
| 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 |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2185374C2 (en) * | 1996-08-02 | 2002-07-20 | Родья Фибер Э Резэн Энтермедиат | Method of lactam treatment |
| CN101049980A (en) * | 2007-05-23 | 2007-10-10 | 徐明光 | Method for comprehensive utilization for benzene extracting concentrated solution of residue wastewater |
| CN103864689A (en) * | 2012-12-07 | 2014-06-18 | 帝斯曼知识产权资产管理有限公司 | Method for preparing caprolactam |
| CN103896840A (en) * | 2012-12-28 | 2014-07-02 | 帝斯曼知识产权资产管理有限公司 | Method and equipment for continuously producing epsilon-caprolactam |
| CN104098495A (en) * | 2014-07-28 | 2014-10-15 | 湘潭大学 | Method for improving caprolactam refining process |
| CN104193663A (en) * | 2014-08-27 | 2014-12-10 | 河北美邦工程科技有限公司 | Purification process for caprolactam |
| CN104557705A (en) * | 2013-10-15 | 2015-04-29 | 中国石油化工股份有限公司 | Method and device for refining caprolactam |
| CN104817422A (en) * | 2015-05-08 | 2015-08-05 | 河北美邦工程科技股份有限公司 | Treatment method of crude benzene residual liquid in back-extraction step in production process of caprolactam |
-
2015
- 2015-08-13 CN CN201510498124.1A patent/CN105061311B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2185374C2 (en) * | 1996-08-02 | 2002-07-20 | Родья Фибер Э Резэн Энтермедиат | Method of lactam treatment |
| CN101049980A (en) * | 2007-05-23 | 2007-10-10 | 徐明光 | Method for comprehensive utilization for benzene extracting concentrated solution of residue wastewater |
| CN103864689A (en) * | 2012-12-07 | 2014-06-18 | 帝斯曼知识产权资产管理有限公司 | Method for preparing caprolactam |
| CN103896840A (en) * | 2012-12-28 | 2014-07-02 | 帝斯曼知识产权资产管理有限公司 | Method and equipment for continuously producing epsilon-caprolactam |
| CN104557705A (en) * | 2013-10-15 | 2015-04-29 | 中国石油化工股份有限公司 | Method and device for refining caprolactam |
| CN104098495A (en) * | 2014-07-28 | 2014-10-15 | 湘潭大学 | Method for improving caprolactam refining process |
| CN104193663A (en) * | 2014-08-27 | 2014-12-10 | 河北美邦工程科技有限公司 | Purification process for caprolactam |
| CN104817422A (en) * | 2015-05-08 | 2015-08-05 | 河北美邦工程科技股份有限公司 | Treatment method of crude benzene residual liquid in back-extraction step in production process of caprolactam |
Non-Patent Citations (4)
| Title |
|---|
| 化学工业部产品销售公司: "《化工产品手册（统配部管产品）》", 28 February 1982 * |
| 林少炜: "己内酰胺萃取精制过程研究", 《北京化工大学硕士学位论文》 * |
| 沈新元: "《化学纤维手册》", 30 September 2008 * |
| 谢丽,等: "环己酮肟气相贝克曼重排反应产物己内酰胺的精制研究", 《石油炼制与化工》 * |
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| CN107118156A (en) * | 2017-06-26 | 2017-09-01 | 山东清创化工有限公司 | A kind of caprolactam separation and purification technique |
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| 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 |
| CN111848325A (en) * | 2020-07-14 | 2020-10-30 | 中国石油化工股份有限公司 | Method and system for washing cumene raw material with alkali by using CHPPO (chlorinated Polypropylene oxide) device |
| 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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