CN205575970U - Caprolactam refining plant - Google Patents
Caprolactam refining plant Download PDFInfo
- Publication number
- CN205575970U CN205575970U CN201620239506.2U CN201620239506U CN205575970U CN 205575970 U CN205575970 U CN 205575970U CN 201620239506 U CN201620239506 U CN 201620239506U CN 205575970 U CN205575970 U CN 205575970U
- Authority
- CN
- China
- Prior art keywords
- caprolactam
- hydrogenation reactor
- refining device
- tower
- rectifying column
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Other In-Based Heterocyclic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to a caprolactam refining plant, its characterized in that: mainly constitute by extraction tower, rectifying column, hydrogenation ware, lightness -removing column, caprolactam distillation system and pipeline, thick caprolactam aqueous solution management says and gets into extraction tower upper portion that the benzene management is said and is connected through the pipeline entering extraction tower lower part between other each towers and the system. The utility model relates to a caprolactam refining plant who does not need water reextraction, ion exchange, evaporation step.
Description
Technical field
This utility model belongs to chemical technology field, relates to a kind of caprolactam refining device, need not water back extraction, ion exchange, the caprolactam refining device of evaporation step particularly to a kind of.
Background technology
Caprolactam, as a kind of important chemical industry monomer, is to produce nylon-6 fiber, resin and the raw material of engineering plastics." Organic Chemicals complete works of " the 2nd edition volume 3 describes caprolactam production method and industrial front, mainly has photo-nitrosation of cyclohexane process, Ketohexamethylene-hydroxylamine assay, toluene method etc..Owing to caprolactam synthetic route is longer, react more complicated, with the generation of a lot of side reactions, cause crude caprolactam exists various impurity.Fiber manufacturing industry is the highest to the purity requirement of caprolactam, it is therefore necessary to as much as possible by impurity removing by suitable method.
Impurity in caprolactam substantially can be divided into following three kinds: one to be raw-material bringing into；Two is the impurity that in production process, side reaction produces；Three is that finished product caprolactam is owing to preserving improper generation qualitative change.The quality of caprolactam is evaluated by a series of quality index such as permanganate number, ultraviolet suction rate, electrical conductivity, volatile base.The impurity affecting rate of absorbing UV mainly has the compound of uv absorption at 290nm, includes heterocyclic compound, azo-compound etc. specifically.The impurity affecting volatile base mainly can generate the compound of ammonia in a heated condition, mainly includes aliphatic and aromatic amine.The impurity affecting electrical conductivity is mainly inorganic compound and a part of acylate etc. that ionization can occur.
Industrially manufacturing caprolactam is under oleum catalytic condition, cyclohexanone-oxime is made to carry out Beckmann rearrangement and generate caprolactam, after rearrangement reaction, the mixed solution ammonia containing oleum and caprolactam is neutralized, produce ammonium sulfate, more isolated and purified ammonium sulfate and crude amide.Generally, first extract by organic solvent-benzene, obtain the benzole soln containing about 30% caprolactam.Owing to caprolactam is the important source material of synthesizing polyamides, the above-mentioned benzole soln containing about 30% caprolactam needs to refine further to can be only achieved requirement highly purified to polyamide raw materials.The process for purification of traditional caprolactam is: benzene extraction → water back extraction → ion exchange → hydrogenation → evaporation → distillation, technological process is complicated and process feedwater amount is big.
Chinese patent CN1272491 discloses a kind of method of hexanolactam hydrofining, caprolactam solution containing impurity is contacted with hydrogen in magnetically stabilized bed reactor, with Raney's nickel or the amorphous alloy using nickel as main active component as catalyst, crude caprolactam is carried out hydrofinishing.Chinese patent CN 102584703 discloses and a kind of removes the extracting process of trace impurity in caprolactam water solution, use alkane or the alkane mixed solution with aromatic hydrocarbon as extractant, by selective extraction, remove the organic impurities in crude caprolactam water solution.Chinese patent CN 1453271 discloses and a kind of removes the method for trace impurity in caprolactam aqueous solution, by using electrodialytic membranes to remove the inorganic impurity in crude caprolactam water solution and micro organic impurity, thus conductivity and the extinction value of caprolactam water solution are greatly reduced.Use the method that hydrogenation or electrodialysis refine, although the caprolactam of high-quality can be obtained, but there is the shortcoming that equipment investment is big, and the method using special solvent extracting and refining, although it is simple to operate, but owing to caprolactam can be dissolved in water so that raffinate phase inevitably remains a certain amount of caprolactam, causes the loss of caprolactam.The evaporating concentration process energy consumption of crude caprolactam water solution is the most considerable, Chinese patent CN1323786 discloses benzene water azeotropic distillation de-benzene process, do not use the unit operations such as benzene extraction, back extraction and evaporation, but the benzene-own liquid after caprolactam benzene extracts adds the water as entrainer, take off benzene by benzene steaming tower azeotropic distillation, energy-saving and cost-reducing aspect superiority clearly.But owing to not having water back extraction operation, end product quality has uncertainty.
Although the subtractive processes such as extraction, distillation can remove partial impurities, but for some trace or physico-chemical property impurity removal poor effect close with caprolactam.This class regular refiner method is difficult to the impurity removed, can use the methods such as the extraction of hydrogenation, special solvent, electrodialysis or ion exchange resin absorption that crude caprolactam is refined.Ion exchange resin is a kind of to have swapping or the polymer adsorbed containing high molecular reactive group of netted stereochemical structure with the material in solution, and its high molecular reactive group is usually polyprotic acid or polyacid base.When solution is by resin bed, the active ion of resin itself, by according to the difference of chemical affinity and the same sex ion generation exchange process in solution, carries out adsorption with resin surface in resin space simultaneously.Wherein, resin anion (R.A.) can adsorb acid impurities, it is possible to extinction value at the electrical conductivity of reduction caprolactam water solution and 290nm；Cationic resin then can remove alkaline impurities, can play an important role reduction volatile base index and electrical conductivity.Generally speaking, ion exchange resin can be effectively improved caprolactam product quality index 290nm extinction value and electrical conductivity, improves end product quality.The attached technology of ion-exchange absorption is the technology of a kind of energy-saving, environment-friendly and high-efficiency, and equipment is simple, and easy to operate, resin can be reused, and will not bring new impurity into, has the advantage that other purification techniquess are incomparable.
" synthetic fiber industry " volume 26 the 2nd phase report HPO technique in 2003 have employed the attached technology of ion-exchange absorption, the caprolactam water solution of 30wt% is swapped adsorption experiment, after the attached effect of ion-exchange absorption, small-scale inorganic impurity and extinction value organic impurities that it contains reduce, and at aqueous solution 290nm, extinction value reduces about 1/3.But HPO technique yet suffers from a lot of problem during answering spent ion exchange resin, e.g., ion exchange resin cycle of operation is shorter, and resin regeneration is frequent；Resin utilization rate is low, and resin iron is seriously polluted." synthetic fiber industry " volume 31 the 6th interim employing macroporous resin D072, D152, D201, D301 etc. in 2008 have carried out dynamic adsorption experiment as adsorbent resin to the crude caprolactam water solution of 5wt%, test result indicate that, several resins all between 60%-80%, present good absorption property to the removal efficiency of impurity." chemical industry progress " volume 24 the 6th interim reporting in 2005 has carried out exchange adsorption experiment as adsorbent to the crude caprolactam solution of the 30wt% after the extraction of toluene method process for refining toluene and water back extraction using activated carbon, NACF and ion exchange resin, result shows when extinction value all reduces by 30%, and activated carbon, active carbon fibre peacekeeping ion exchange resin are respectively 26.7ml/g, 67.48ml/g, 46.66ml/g to the adsorption capacity of impurity.Having carried out again the test of NACF and the group technology absorption caprolactam water solution of ion exchange resin on the basis of the above results, result shows, when extinction value reduces by 50%, dynamic adsorption capacity is 36.67ml/g.But, owing to this crude caprolactam solution of choosing of research is from after toluene method process for refining water back extraction operation, this crude caprolactam solution impurity content is the highest, the cycle of operation of active carbon fibre peacekeeping ion exchange resin will be the shortest, resin and NACF frequent regeneration will be caused, therefore can not meet the condition of commercial Application.
Summary of the invention
The purpose of this utility model is to provide a kind of caprolactam refining device, cancels water back extraction in prior art, ion exchange, evaporization process, reaches energy-conservation, reduces discharging and put forward high-quality purpose.
The technical solution of the utility model:
A kind of caprolactam refining device, is mainly made up of extraction tower, rectifying column, hydrogenation reactor, lightness-removing column, caprolactam Distallation systm；Crude caprolactam water solution enters extraction tower top, benzene enters extraction tower bottom, extraction tower top is connected with rectifying column, rectifying column bottom connects reboiler, rectifying column tower top is benzene aquatic solution gaseous phase outlet, and tower reactor is by being connected with hydrogenation reactor feed pump import, and hydrogenation reactor feed pump is connected with hydrogenation reactor feed preheater import, hydrogenation reactor feed preheater is connected with hydrogenation reactor top, and hydrogenation reactor top is connected to hydrogen feed tube；Hydrogenation reactor material outlet is connected with lightness-removing column, and lightness-removing column top is connected with gaseous phase outlet, and bottom connects reboiler；Lightness-removing column tower reactor is connected with caprolactam Distallation systm, and the condenser of caprolactam Distallation systm is connected with vacuum system, and the liquid-phase outlet of condenser is connected with essence caprolactam product tank, has residual liquid to export bottom caprolactam Distallation systm.
Described lightness-removing column is connected to vacuum system.
Described rectifying column is connected to vacuum system.
Described hydrogenation reactor is fixed bed hydrogenation reactor.
Described hydrogenation reactor bottom connects knockout drum.
Described rectifying column is the distillation system of cascade towers.
Described rectifying column is the distillation system of parallel two towers.
Described caprolactam Distallation systm is the Distallation systm of three set series connection.
Described caprolactam refining device, is connected to caustic washing system before or after extraction tower.
It is to be connected with each other by pipeline that described equipment connects.
This utility model for the method for caprolactam refining is: be neutralized by mixed solution ammonia containing oleum and caprolactam after rearrangement reaction, produces ammonium sulfate, more isolated and purified ammonium sulfate and crude caprolactam water solution；First by organic solvent-benzene, crude caprolactam solution is extracted, obtain the benzole soln containing 20-40% caprolactam, caprolactam benzole soln after extraction carries out rectification, a small amount of water is added at the bottom of tower, to maintain bottom product aqueous 5-10%(weight), 90%-95%(weight at the bottom of tower after rectification) caprolactam water solution send to hydrogenation, overhead product be benzene send back to benzene tank circulation；Caprolactam water solution hydrogenation uses fixed bed reactors and with Al2O3Nickel or palladium catalyst for carrier；Caprolactam water solution after hydrogenation, after pre-distillation removing moisture with light component, enters the caprolactam product that Distallation systm distillation obtains refining.
During being carried out caprolactam refining by this utility model, first adding alkali and process crude caprolactam water solution, alkali liquor is the sodium hydroxide solution of mass concentration 4-60%, and its consumption is every kg crude caprolactam water solution 2-50 gram.
During being carried out caprolactam refining by this utility model, alkaline cleaning benzene extraction after caprolactam benzole soln, alkali liquor be mass concentration be 2-10% sodium hydroxide solution, its consumption is every kilogram of caprolactam benzole soln 3-20 gram.
Caprolactam benzole soln rectification process in this utility model, rectification is to operate under pressurization, normal pressure or decompression state, preferably two effect series connection distillation operation techniques, the first tower pressurized operation, the second tower decompression operation；First rectifying column does not add water and directly steams benzene, tower top pressure 0.2-0.25MPa, tower reactor operation temperature 160-165 DEG C, tower top operation temperature 140-145 DEG C；Second distillation column decompression operation, adds desalted water as entrainer, the caprolactam water solution aqueous 5-10%(weight of maintenance tower reactor extraction in operating process), tower top pressure 0.02-0.06 MPa(A), tower top temperature 60-70 DEG C, bottom temperature 100-105 DEG C.
Caprolactam benzole soln rectification process in this utility model, uses two effect rectification process of parallel two towers, the first tower pressurized operation, the second tower decompression operation；First rectifying tower pressure on top surface 0.2-0.25MPa, tower reactor operation temperature 160-165 DEG C, tower top operation temperature 140-145 DEG C, add desalted water as entrainer, the caprolactam water solution aqueous 5-10%(weight of maintenance tower reactor extraction in operating process)；Second distillation column decompression operation, adds desalted water as entrainer, the caprolactam water solution aqueous 5-10%(weight of maintenance tower reactor extraction in operating process), tower top pressure 0.02-0.06 MPa(A), tower top temperature 60-70 DEG C, bottom temperature 100-105 DEG C.
In this utility model, caprolactam water solution hydrogenation uses fixed bed reactors, and catalyst is Al2O3Mix in blender or hydrogenation stirred tank any appliance for nickel or the palladium catalyst of carrier, caprolactam water solution and first strand of hydrogen, make hydrogen degree of saturation in caprolactam water solution reach 30 ~ 100%；Then in the presence of any one, the crude caprolactam water solution containing dissolved hydrogen and second strand of hydrogen are carried out sufficient gas-liquid-solid hydrogenation reaction in fixed bed reactors at a kind of load-type nickel or palladium fixed bed hydrogenation catalyst；Caprolactam water solution content is 5 ~ 10 mass %；Hydrogenation reaction temperature range is 70 ~ 150 DEG C, and pressure is 0.1 ~ 0.3MPa, and the air speed of caprolactam solution is 1 ~ 50h-1。
In this utility model, de-light point of caprolactam water solution after hydrogenation is by rectification under vacuum removing moisture and light composition impurity, the pressure of rectification under vacuum is 0.35-1.5 KPa (A), distilled by decompression, caprolactam solution concentration is brought up to 99.9%(mass) more than, remove light composition impurity simultaneously.
Caprolactam distillation in this utility model, the caprolactam liquid from lightness-removing column is stored in caprolactam surge tank, continually adds a small amount of Caustic soda in caprolactam liquid.Caustic soda is delivered to the caprolactam circulation fluid of caprolactam surge tank circulating pump from alkali liquor feed pot by Caustic soda dosing pump.For ensureing that a small amount of alkali liquor is mixed homogeneously with the solution in caprolactam surge tank, equipped with injector mixer in caprolactam surge tank.Still the caprolactam solution containing a small amount of higher impurity and water sends into Distallation systm from caprolactam surge tank, Distallation systm is made up of caprolactam distillation column vaporizer and caprolactam separated device and caprolactam distiller condenser, and its operation pressure is about 0.5KPa.A.
Caprolactam distillation can be the series connection distillation of many Distallation systms, preferably three Distallation systm series connection distillations.
Accompanying drawing explanation
Fig. 1: a kind of caprolactam refining device schematic diagram.
In figure: 1-extraction tower 2-rectifying column 3-hydrogenation reactor 4-lightness-removing column 5-caprolactam Distallation systm 6-rectifying column reboiler 7-hydrogenation reactor feed pump 8-lightness-removing column reboiler 9-caprolactam Distallation systm feed pump 10-hydrogenation reactor feed preheater 15-caprolactam evaporator for distillation；
After 11-crude caprolactam water solution 12-benzene 13-caprolactam benzole soln 14-extraction, caprolactam water solution 33-hydrogenation reactor after waste water 21-desalted water 22-caprolactam water solution 23-benzene aquatic solution 31-hydrogen 32-hydrogenation is to knockout drum logistics the 41-de-light component gently steamed of caprolactam 42-and moisture 51-caprolactam residual liquid 53-Distallation systm after the distillation of caprolactam product 52-and connection WH-hot water of vacuum system after refined after de-light.
Detailed description of the invention
Embodiment 1
Ammonium sulfate and crude caprolactam water solution 21024kg/h will be isolated, wherein caprolactam 14549 kg/h, water 5918 kg/h, ammonium sulfate 187.2 kg/h, inorganic matter 217.5 kg/h, Organic substance 151.2 kg/h, add extraction tower bottom, benzene 53060 kg/h is added on extraction tower top, the most aqueous 60 kg/h, carry out being obtained by extraction caprolactam benzole soln 69559.7 kg/h, wherein caprolactam 14547.6 kg/h, benzene 52975.9 kg/h, ammonium sulfate 3.6 kg/h, water 1957 kg/h, Organic substance 75.6 kg/h；Tower reactor is benzene extraction remaining liquid, predominantly water, wherein contains a small amount of benzene, caprolactam and Organic substance and inorganic matter.
It is that 5% sodium hydroxide solution carries out countercurrent washing at caustic wash tower by the caprolactam benzole soln obtained from extraction tower and mass concentration, sodium hydroxide solution enters from caustic wash tower top, caprolactam benzole soln enters from caustic wash tower bottom, sodium hydroxide solution consumption is the 5 ‰ of caprolactam benzole soln weight, tower top obtains caprolactam benzole soln 68589.2kg/h after purification, wherein caprolactam 14546.6kg/h, benzene 52973.5kg/h, Organic substance 75.6kg/h, remaining is water.It is alkaline washing residual liquid, predominantly sodium hydrate aqueous solution at the bottom of caustic wash tower.
Caprolactam benzole soln through alkali cleaning being carried out in rectifying column rectification, feeds as 68589.5kg/h, wherein caprolactam 14546.6kg/h, benzene 52973.5kg/h, Organic substance 75.6kg/h, remaining is water.Supplementing desalted water in tower reactor, maintaining tower kettle product caprolactam water content is 5-10%；Tower top pressure is 0.05-0.055MPa (absolute pressure), tower top temperature 70-75 DEG C, bottom temperature 110-115 DEG C.Tower kettle product: caprolactam 14546.6kg/h, water 800-1200 kg/h, Organic substance 15.6 kg/h；Overhead product: benzene-aqueous solution, wherein benzene 52973.5kg/h, water 7985kg/h, Organic substance 60 kg/h.
Embodiment 2
Above with embodiment 1, simply the rectification of caprolactam benzole soln selects parallel two towers technique, and the benzene-water vapour obtained by the tower top of the first rectifying column evaporates thermal source as the tower reactor of Second distillation column.The caprolactam benzole soln obtained after alkali cleaning is carried out the first rectifying column and Second distillation column respectively according to the ratio of 55:45, first rectifying column uses evaporation as thermal source, control tower pressure on top surface is 0.15-0.2 MPa (absolute pressure), tower top temperature is 115-120 DEG C, bottom temperature 130-140 DEG C；Second distillation column uses the top gaseous phase of the first rectifying column to be thermal source, and control tower pressure on top surface is 0.02-0.03 MPa (absolute pressure), and tower top temperature is 60-65 DEG C, bottom temperature 95-100 DEG C.
Embodiment 3
Tower kettle product caprolactam water solution embodiment 1 obtained is hydrogenated with in fixed bed hydrogenation reactor, and catalyst is Al2O3Mix in blender or hydrogenation stirred tank any appliance for nickel or the palladium catalyst of carrier, caprolactam water solution and first strand of hydrogen, make hydrogen degree of saturation in caprolactam water solution reach 30 ~ 100%；Then in the presence of any one, the crude caprolactam water solution containing dissolved hydrogen and second strand of hydrogen are carried out sufficient gas-liquid-solid hydrogenation reaction in fixed bed reactors at a kind of load-type nickel or palladium fixed bed hydrogenation catalyst；Caprolactam water solution content is 5 ~ 10 mass %；Hydrogenation reaction temperature range is 70 ~ 150 DEG C, and pressure is 0.1 ~ 0.3MPa, and the air speed of caprolactam solution is 1 ~ 50h-1。
Embodiment 4
By the caprolactam water solution after hydrogenation by rectification under vacuum removing moisture and light composition impurity, the pressure of rectification under vacuum is 0.35-1.5 KPa (A), distilled by decompression, caprolactam solution concentration brought up to 99.9%(mass) more than, remove light composition impurity simultaneously.
Embodiment 5
Being distilled by the caprolactam of removing moisture with light component, distillation uses three Distallation systm series connection distillations, and the most secondary caprolactam adds the first Distallation systm and steams the caprolactam of about 65-75%, and the caprolactam steamed enters products pot as product；Remaining caprolactam entrance after-fractionating system being distilled, continues to steam the caprolactam of about 65-75%, by detection, if meeting product requirement to be put into products pot, as do not met product requirement, joining the first Distallation systm；The caprolactam of after-fractionating system spare adding the 3rd Distallation systm row distillation, steams 65-75% caprolactam and add the first Distallation systm, remaining material returns ammonium sulfate device above.
Claims (10)
1. a caprolactam refining device, it is characterised in that: mainly it is made up of extraction tower (1), rectifying column (2), hydrogenation reactor (3), lightness-removing column (4), caprolactam Distallation systm (5)；Crude caprolactam water solution enters extraction tower (1) top, benzene enters extraction tower (1) bottom, extraction tower (1) top is connected with rectifying column (2), rectifying column (2) bottom connects reboiler (6), rectifying column (2) tower top is benzene aquatic solution gaseous phase outlet, tower reactor is by being connected with hydrogenation reactor feed pump (7) import, hydrogenation reactor feed pump (7) is connected with hydrogenation reactor feed preheater (10) import, hydrogenation reactor feed preheater (10) is connected with hydrogenation reactor (3) top, and hydrogenation reactor (3) top is connected to hydrogen feed tube；Hydrogenation reactor (3) material outlet is connected with lightness-removing column (4), and lightness-removing column (4) top is connected with gaseous phase outlet, and bottom connects reboiler；Lightness-removing column (4) tower reactor is connected with caprolactam Distallation systm (5), the condenser of caprolactam Distallation systm (5) is connected with vacuum system, the liquid-phase outlet of condenser is connected with essence caprolactam product tank, and caprolactam Distallation systm (5) bottom has residual liquid to export.
Caprolactam refining device the most according to claim 1, it is characterised in that lightness-removing column (4) is connected to vacuum system.
Caprolactam refining device the most according to claim 1, it is characterised in that rectifying column (2) is connected to vacuum system.
Caprolactam refining device the most according to claim 1, it is characterised in that hydrogenation reactor (3) is fixed bed hydrogenation reactor.
5. according to the caprolactam refining device described in claim 1 or 4, it is characterised in that the bottom of hydrogenation reactor (3) connects knockout drum.
Caprolactam refining device the most according to claim 1, it is characterised in that rectifying column is the distillation system of cascade towers.
Caprolactam refining device the most according to claim 1, it is characterised in that rectifying column is the distillation system of parallel two towers.
Caprolactam refining device the most according to claim 1, it is characterised in that caprolactam Distallation systm is the Distallation systm of three set series connection.
Caprolactam refining device the most according to claim 1, it is characterised in that be connected to caustic washing system at extraction tower.
Caprolactam refining device the most according to claim 1, it is characterised in that the connection between equipment is to be connected with each other by pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620239506.2U CN205575970U (en) | 2016-03-28 | 2016-03-28 | Caprolactam refining plant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620239506.2U CN205575970U (en) | 2016-03-28 | 2016-03-28 | Caprolactam refining plant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN205575970U true CN205575970U (en) | 2016-09-14 |
Family
ID=56866846
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201620239506.2U Active CN205575970U (en) | 2016-03-28 | 2016-03-28 | Caprolactam refining plant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN205575970U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106316955A (en) * | 2016-10-28 | 2017-01-11 | 湖北三宁化工股份有限公司 | Refining device for high-purity caprolactam and purifying method |
| CN107556241A (en) * | 2017-01-19 | 2018-01-09 | 沧州旭阳化工有限公司 | The method and apparatus that caprolactam is prepared by trifluoroacetic acid catalysis of pimelinketone oxime Beckmann rearrangement |
| CN111635348A (en) * | 2020-06-22 | 2020-09-08 | 聊城鲁西聚酰胺新材料科技有限公司 | Application and system of screw vacuum pump in caprolactam refining process production |
-
2016
- 2016-03-28 CN CN201620239506.2U patent/CN205575970U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106316955A (en) * | 2016-10-28 | 2017-01-11 | 湖北三宁化工股份有限公司 | Refining device for high-purity caprolactam and purifying method |
| CN107556241A (en) * | 2017-01-19 | 2018-01-09 | 沧州旭阳化工有限公司 | The method and apparatus that caprolactam is prepared by trifluoroacetic acid catalysis of pimelinketone oxime Beckmann rearrangement |
| CN111635348A (en) * | 2020-06-22 | 2020-09-08 | 聊城鲁西聚酰胺新材料科技有限公司 | Application and system of screw vacuum pump in caprolactam refining process production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104098441B (en) | Commercial syngas mesohigh carbonylation produces dimethyl oxalate and the technique of Hydrogenation ethylene glycol and apparatus system | |
| CN106588536B (en) | Preparation method and system of cyclohexanone | |
| CN205575970U (en) | Caprolactam refining plant | |
| CN106810455B (en) | A kind of production method of high-quality essence hexamethylene diamine | |
| CN206232628U (en) | A kind of production system of cyclohexanone | |
| CN109384666A (en) | A method of organic acid in linkage recycling aqueous solutions of organic acids | |
| CN105111079A (en) | Method and device for separating acetic acid sec-butyl ester and sec-butyl alcohol | |
| CN109503410A (en) | The method of solvent DMF recycling in a kind of production of Sucralose | |
| CN104098495A (en) | Method for improving caprolactam refining process | |
| CN101367724A (en) | Method and apparatus for synthesis of isopropyl acetate | |
| CN104998689A (en) | Anion resin-carried peroxyphosphotungstic acid, its preparation method and use, and epoxycycloparaffin synthesis method | |
| CN108341741A (en) | A kind of synthesis gas prepares the purification technique and device of ethylene glycol | |
| CN108002995A (en) | A kind of method and its equipment of acetone two-step method synthesizing methyl isobutyl ketone | |
| CN109134217B (en) | Oxidation device and oxidation process improvement method in cyclohexanone production process by cyclohexane oxidation method | |
| CN110981721A (en) | Method for continuously producing n-propyl acetate | |
| CN112898120B (en) | Device and method for producing ethylene glycol | |
| WO2020015321A1 (en) | Method and device for separating isopropanol | |
| CN104119225A (en) | New technology for producing ethyl acetate through reactive distillation by taking mixed ionic liquid as catalyst | |
| CN102219641B (en) | Method for purifying ethylene glycol | |
| CN102372598A (en) | Method for separating glycol from butanediol | |
| CN110483282B (en) | Device and method for producing high-concentration ethylene glycol diacetate | |
| CN105037233A (en) | Process for refining caprolactam | |
| CN107722033A (en) | The method for adding hydrophobic ionic liquid to be evaporated under reduced pressure separation dehydration of sugar alcohols reaction product | |
| CN102372599A (en) | Method for separating glycol and butylene glycol | |
| CN106588597A (en) | Method for purifying polyoxyethene dimethyl ether |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |