CN101434569B - Method and equipment for preparing caprolactam from cyclohexanone oxime - Google Patents
Method and equipment for preparing caprolactam from cyclohexanone oxime Download PDFInfo
- Publication number
- CN101434569B CN101434569B CN2007101774067A CN200710177406A CN101434569B CN 101434569 B CN101434569 B CN 101434569B CN 2007101774067 A CN2007101774067 A CN 2007101774067A CN 200710177406 A CN200710177406 A CN 200710177406A CN 101434569 B CN101434569 B CN 101434569B
- Authority
- CN
- China
- Prior art keywords
- oxime
- carrier gas
- cyclohexanone
- reactor
- solvent
- 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
Images
Abstract
The invention relates to a method for preparing caprolactam with cyclohexanone-oxime, and a device used in the method. The method includes the steps as follows: after being heated, inert supporting gas containing a solvent is continuously put into a supporting gas intake of a first-class reactor of a multi-stage series reactor provided with a catalyst. Cyclohexanone- oxime is directly divided into two parts which then enter all stages of the multi-stage series reactor, thereby ensuring that reaction effluents are cooled. The supporting gas is separated and recycled to the supporting gas intake of the first-class reactor, and then products from a liquid phase reaction are separated and purified.
Description
Technical field
The present invention relates to a kind of method and employed equipment of this method by preparing caprolactam with cyclohexanone-oxime.More specifically, the present invention relates to method and the employed equipment of this method that a kind of Cyclohexanone-Oxime Gas Phase Beckmann Rearrangement prepares hexanolactam.
Background technology
It is the at present industrial technology of generally using that cyclohexanone-oxime is converted into hexanolactam through the liquid phase Beckmann rearrangement, and catalyzer mostly is the vitriol oil or oleum.This method can reach more than 98.5% the selectivity of hexanolactam.The hexanolactam that adopts this method to produce accounts for about 90% of world's hexanolactam output.The shortcoming of this method maximum is a large amount of low value ammonium sulfate of by-product, secondly is that equipment corrosion and environmental pollution are serious.
Shortcoming at present liquid phase method existence, Chinese patent CN1269360A has disclosed the method that hexanolactam is produced in a kind of vapor phase rearrangement, it is catalyzer that this method adopts the MFI structure molecular screen, adopt fluidized-bed process, uninterrupted cyclic regeneration by catalyzer overcomes catalyst carbon deposit inactivation defective, the cyclohexanone-oxime transformation efficiency is 99.6%, hexanolactam selectivity 95.7%.This method is not used sulfuric acid, has solved the problem of equipment corrosion and producing ammonium sulfate byproduct.But there are shortcomings such as flow process and equipment complexity, investment and process cost height in the employing fluidized-bed process.
Chinese patent CN1621405 discloses a kind of Fixed Bed Gas Phase and has reset technology, and it adopts conventional fixed-bed process, and atmospheric operation is a catalyzer with the MFI structure molecular screen, at 250～500 ℃, normal pressure, cyclohexanone-oxime weight space velocity 1-8h
-1Under carry out vapor phase rearrangement reaction, the cyclohexanone-oxime transformation efficiency is 99.5%, the hexanolactam selectivity is 97.5%, the catalyzer one way life-span reaches 1200 hours.There are shortcomings such as reaction temperature rising is big, bed temperature is uneven, easy coking, operational cycle weak point, running cost height in this method, and is difficult to carry out industrial.
Summary of the invention
The purpose of this invention is to provide a kind of method by preparing caprolactam with cyclohexanone-oxime, this method has the high temperature on-catalytic side reaction that suppresses oxime, improve reaction preference, avoid well heater and heat-exchange equipment coking, prolong advantages such as catalyzer life cycle.
Method provided by the invention is: after will containing the inert carrier gas heating of solvent, feed the carrier gas inlet of the first step reactor of the plural serial stage reactor that catalyzer is housed continuously, cyclohexanone-oxime is divided at least two parts of each stage reactors that enters described plural serial stage reactor respectively, the cooling reaction effluent, isolate carrier gas and be circulated to the carrier gas inlet of described first step reactor, liquid-phase reaction product is separated, purifies.
Equipment provided by the invention comprises following a few part:
The plural serial stage reactor is to be made up of at least two reactors that are cascaded, or comprises the single reactor of at least two beds, which is provided with mixing raw material inlet, carrier gas inlet and reaction effluent outlet;
Separator is used for reaction effluent is carried out gas-liquid separation, which is provided with reaction effluent inlet, carrier gas outlet and discharge channel;
Solvent recovery tower is used for separating and the recovery solvent from the liquid-phase reaction product that separator is told, and which is provided with liquid-phase reaction product inlet, solvent outlet and crude product outlet;
Be used for well heater with the carrier gas heating; Be used for reaction effluent refrigerative water cooler;
Be used to carry out the interchanger of heat exchange between reaction effluent and the carrier gas;
Be used to connect between the carrier gas inlet of the carrier gas outlet of separator and plural serial stage reactor, between the reaction effluent inlet of the reaction effluent outlet of plural serial stage reactor and separator, the parting liquid of the discharge channel of separator and the solvent recovery tower pipeline between entering the mouth, and will be from the solvent and the circulation carrier gas blended pipeline of solvent recovery tower solvent outlet.
Each bed that has the single reaction vessel of a plurality of beds in the described plural serial stage reactor, each reactor in perhaps a plurality of tandem reactors is called as A reactor.That A reactor that wherein is in the upstream of carrier gas mobile direction is called first step reactor.
Adopt feed process provided by the invention, can be under lower total rare gas element/cyclohexanone-oxime mol ratio, obtain to use higher rare gas element/cyclohexanone-oxime mol ratio in each stage reactor, thereby side reactions such as minimizing cyclohexanone-oxime pyrocondensation coking prolong the catalyzer life cycle.Total rare gas element/cyclohexanone-oxime mol ratio is low, means reducing of full scale plant energy consumption and equipment scale.In addition, because the raising of rare gas element in each stage reactor/cyclohexanone-oxime mol ratio, the rare gas element relative content increases, and has therefore significantly reduced the intensification that beds brings because of exothermic heat of reaction, helps improving the selectivity of hexanolactam and the service efficiency of catalyzer.The another one advantage of the inventive method is that cyclohexanone-oxime need not heat, enter each stage reactor in the low-temperature receiver mode, the heat-obtaining of each inter-stage of realization response device, thereby avoided the high-temperature heating process of cyclohexanone-oxime in well heater or interchanger, eliminated the problem of coking in well heater or interchanger, and reduced the generation of side reactions such as cyclohexanone-oxime on-catalytic thermal condensation, can improve the purpose product selectivity.
Description of drawings
Fig. 1 is the synoptic diagram of a specific embodiments of the inventive method and equipment.
Fig. 2 is the idiographic flow synoptic diagram of another specific embodiments embodiment 1,2 method therefors of the inventive method and equipment.
Fig. 3 is the synoptic diagram of the continuous fixed-bed reactor of single hop.
Embodiment
Method of the present invention is the continuous carrier gas inlet that feeds the first step reactor of the plural serial stage reactor that catalyzer is housed in inert carrier gas heating back that will contain solvent, cyclohexanone-oxime is divided at least two parts of each levels that enter described plural serial stage reactor respectively, make the reaction effluent cooling, isolate carrier gas and be circulated to the carrier gas inlet of described first step reactor, liquid-phase reaction product is separated, purifies.Preferably the mixture with cyclohexanone-oxime and solvent is divided into and the corresponding umber of the progression of described plural serial stage reactor, and preferably each part is five equilibrium.
Plural serial stage reactor described in the inventive method is preferably insulation fix bed reactor, for example can be axial and radial reactor.The plural serial stage reactor can be formed by a plurality of independent reactors in series, also can be a reactor with a plurality of beds.Material in reactor flow pattern can be upstriker or downstriker.
Plural serial stage reactor described in the inventive method is divided into 2 grades at least.Do not make reactive system too under the complicated situation, the high more effect of progression is good more.The progression of the plural serial stage reactor that the inventive method is used is generally the 2-10 level, preferred 3-6 level.
Any medium of inert carrier gas in the inventive method for not reacting with cyclohexanone-oxime, hexanolactam includes but not limited to that nitrogen, hydrogen, argon gas, ammonia, boiling point are not higher than 180 ℃ stable hydrocarbon and halohydrocarbon or their mixture.
Total mol ratio of inert carrier gas and cyclohexanone-oxime is 6-50 in the inventive method, and inert carrier gas and cyclohexanone-oxime are 12-300 in the mol ratio of every stage reactor, are preferably 20-200.Total mol ratio of inert carrier gas and cyclohexanone-oxime is meant, when system stable operation, enters the carrier gas mole number of whole plural serial stage reactor and the ratio of total cyclohexanone-oxime mole number in the unit time.Inert carrier gas and cyclohexanone-oxime are meant in the mol ratio of every stage reactor, when system stable operation, enter the carrier gas mole number of plural serial stage reactor one-level and the ratio of this grade cyclohexanone-oxime mole number in the unit time.The inert carrier gas of each stage reactor and cyclohexanone-oxime mol ratio can be identical or different.
Catalyzer in the inventive method can be any MFI structural molecule sieve catalyst that is used for the cyclohexanone-oxime vapor phase rearrangement.Described MFI structure molecular screen catalyzer comprises the ZSM-5 molecular sieve of the disclosed HTS of prior art, total silicon molecular sieve and silicon/aluminum ratio 〉=500.These molecular sieves can be directly used in the inventive method, also can handle through the alkaline aqueous solution of nitrogenous compound in advance.
Solvent in the inventive method is selected from C
1-C
6The straight or branched Fatty Alcohol(C12-C14 and C12-C18) or their mixture, particular methanol, ethanol or propyl alcohol or their mixture.The weight ratio of solvent and cyclohexanone-oxime is 10-80: 90-20, is preferably 20-70: 80-30.
Temperature of reaction in the inventive method is 200-500 ℃, preferred 300-450 ℃.
Pressure in the inventive method is 0.11-2.5MPa, preferred 0.15-1.2MPa.When pressure during greater than normal pressure, equipment of the present invention also comprises the compressor with the carrier gas pressurization.
The weight space velocity of cyclohexanone-oxime is 0.2-8h in the method for the present invention
-1, be preferably 0.5-6h
-1
Contain suitable quantity of water in the reaction system and help to improve activity of such catalysts, but too high water will cause the increase of side reactions such as cyclohexanone-oxime hydrolysis, influence the selectivity of hexanolactam.The mol ratio of water and cyclohexanone-oxime is 0.03-1.0, is preferably 0.05-0.35.Water can be brought into by the reactor inlet injection or from recovered solvent in the inventive method.
The present invention is described in detail with reference to the accompanying drawings.
Fig. 1 is the synoptic diagram of an embodiment of the inventive method and equipment.In this embodiment, described plural serial stage reactor is the single reaction vessel that the flow direction along reactant is provided with a plurality of beds.Circulation carrier gas and recovery solvent are after the interchanger heat exchange enters the carrier gas inlet of reactor, and cyclohexanone-oxime is divided into and the corresponding umber of bed number, enter into different catalysts bed inlet respectively.The cyclohexanone-oxime that enters first bed begins the vapor phase rearrangement reaction under the rearrangement reaction condition, originally react completely to this bed exit cyclohexanone-oxime hexyl.Owing to the exothermic heat of reaction reason, the first bed outlet material temperature will rise.Second part of cyclohexanone-oxime is admitted to second bed inlet, and the rest may be inferred, and to the last a cyclohexanone-oxime enters last bed and finishes reaction, reaction effluent and the circulation carrier gas heat exchange cooling that contains solvent.Through gas-liquid separation, isolated carrier gas is circulated to the carrier gas inlet of reactor, and isolated liquid product obtains crude caprolactam behind solvent recovery tower recovery solvent wherein, and recovered solvent can be mixed and fed into reactor once more with the circulation carrier gas.
Fig. 2 is the synoptic diagram of another embodiment of the inventive method and equipment.In this embodiment, the plural serial stage reactor is formed by a plurality of independent reactors in series.Enter the carrier gas inlet of first step reactor after circulation carrier gas and the heat exchange of recovery solvent process interchanger, cyclohexanone-oxime is divided into and the corresponding umber of bed number, enters the inlet of each stage reactor respectively.The cyclohexanone-oxime that enters first step reactor begins the vapor phase rearrangement reaction under the rearrangement reaction condition, the cyclohexanone-oxime hexyl originally reacts completely during to this stage reactor exit.Owing to the exothermic heat of reaction reason, first step reactor outlet material temperature will rise.Second part of cyclohexanone-oxime is admitted to second stage reactor inlet, and the rest may be inferred, and to the last a cyclohexanone-oxime enters the last step reactor and finishes reaction.Reaction effluent and the circulation carrier gas heat exchange cooling that contains solvent, through gas-liquid separation, be circulated to the carrier gas inlet of first step reactor after the compressed machine compression of isolated carrier gas, liquid product obtains to treat the purified crude caprolactam after solvent recovery tower reclaims solvent.Recovered solvent and circulation carrier gas are mixed and fed into reactor once more.
The invention will be further described below by embodiment, but the present invention is not limited to the content of following embodiment.
Catalyzer:
Employed catalyzer is the total silicon molecular sieve catalyst that makes according to the method described in the Chinese patent CN1338427 among the embodiment.The content of this patent is all included in this specification sheets by reference.
Reactor:
Among the embodiment, the vapor phase rearrangement reaction process is to carry out in the reactive system that a cover is composed in series by three fixed-bed reactor, and every reactor volume is 220L.
Chromatographic instrument:
Reaction product adopts Trace GC-MS to carry out qualitative analysis.The GC8000 chromatographic instrument is adopted in quantitative analysis, and FID detects, OV-1 capillary column φ 0.25mm * 30m, and 248 ℃ of temperature of vaporization chamber, 240 ℃ of sensing chamber's temperature, column temperature is temperature programming, 110 ℃ of constant temperature 8 minutes, 15 ℃/min are raised to 230 ℃ of constant temperature 14 minutes again.
Calculation of parameter:
Reaction after in the crude caprolactam cut after the solvent recuperation rearrangement product content such as hexanolactam, pimelinketone, cyclohexanone-oxime, cyclonene adopt area normalization methods to calculate, solvent does not participate in integration.Each relevant reaction evaluating parameter-definition is as follows among the embodiment:
Cyclohexanone-oxime transformation efficiency (mol%)=[(cyclohexanone-oxime molar content in the 100-crude caprolactam)/100] * 100%
Hexanolactam selectivity (mol%)=[molar content of hexanolactam in the crude caprolactam/(molar content of cyclohexanone-oxime in the 100-crude caprolactam)] * 100%
Weight space velocity (h
-1The mass rate of)=cyclohexanone-oxime (kg/h)/layer bed catalyst quality (kg)
Embodiment 1
Three fixed-bed reactor series connection backs as the plural serial stage reactor, are respectively charged into φ 10, φ 3 inert ceramic balls and 25kg catalyzer from top to bottom, and the catalyzer inventory is 75kg.With nitrogen is carrier gas, and carrier gas and reaction raw materials flow to and be downstriker.With the nitrogen purging system to oxygen level less than 0.3
%, and pressurising starts circulation carrier gas compressor to reaction pressure 0.28MPa (g), the circulating nitrogen gas total flux that control enters reactor is 410Nm
3/ h.Behind the system stability, start the carrier gas well heater carrier gas is heated to 380-400 ℃.Flow with 75kg/h adds the recycle methanol solvent in the circulation carrier gas, inject the 0.63L/h deionized water continuously from first reactor inlet, cyclohexanone-oxime is under flow is controlled automatically, flow with 75kg/h is divided into 3 parts, enter three reactor inlet pipelines respectively, bed reacts with entering separately after the next mixing of materials in upstream.The 3rd reactor outlet material is cooled to about 40 ℃ through heat exchange, enter separator and tell carrier gas, carrier gas loops back reactor inlet through the recycle compressor supercharging, and the separator liquid phase product is delivered to solvent recovery tower, solvent methanol steams from cat head and loops back reactive system, and the tower still is a crude caprolactam.The device steady running after 48 hours the sampling analysis crude caprolactam form and calculate transformation efficiency and selectivity, detailed process condition and the results are summarized in table 1.
Embodiment 2
According to the identical method of embodiment 1, the feed rate of cyclohexanone-oxime is increased to 150Kg/h by 75kg/h, water injection rate is brought up to 1.2L/h by 0.63L/h, and other condition is identical with embodiment 1, and the variation and the reaction result of corresponding air speed, total nitrogen oxime ratio, pure oxime ratio are summarized in table 1.
Embodiment 3
According to the identical method of embodiment 1, the feed rate of cyclohexanone-oxime is reduced to 45Kg/h by 75Kg/h, other condition is identical with embodiment 1, and corresponding air speed, total nitrogen oxime are summarized in table 1 than the variation and the reaction result of, pure oxime ratio.
Embodiment 4
According to the identical method of embodiment 1, reaction pressure is adjusted to 0.5Mpa by 0.28Mpa, other condition is with identical with embodiment 1, and reaction result is summarized in table 1.
The comparative example 1
This comparative example 1 explanation is only used the single hop fixed bed, the reaction effect when not adopting the direct sectional feeding of cyclohexanone-oxime.
Comparison example is carried out on the continuous fixed-bed reactor of single hop, enter reactor inlet after the heating of circulation carrier gas heater via, cyclohexanone-oxime mixes by a certain percentage with the circulating solvent and the carrier gas that partly circulates, vaporize at low temperatures through vaporizer earlier, after interchanger and the heat exchange of reactor outlet product, enter reactor again and carry out the vapor phase rearrangement reaction, reaction product is carried out vapor-liquid separation after heat exchange, cooling, the compressed machine of gaseous phase materials boosts and loops back reactor, and liquid product obtains to treat the purified crude caprolactam after solvent recovery tower reclaims solvent.Recovered solvent and raw material cyclohexanone-oxime are mixed and fed into reactor once more.Exemplary flow is seen accompanying drawing 3.
The fixed-bed reactor volume is 220L, is respectively charged into φ 10, φ 3 inert ceramic balls and 45kg catalyzer from top to bottom, with the nitrogen replacement system to oxygen level less than 0.3
%, and pressurising starts circulation carrier gas compressor to reaction pressure 0.28MPa (g), the circulating nitrogen gas flow that control enters well heater is 410Nm
3/ h enters the circulating nitrogen gas flow 300Nm of vaporizer
3/ h.Behind the system stability, start the carrier gas well heater carrier gas is heated to 380-400 ℃.Flow with 45kg/h adds the recycle methanol solvent in the circulation carrier gas, inject the 0.18L/h deionized water continuously from first reactor inlet, cyclohexanone-oxime is at flow automatically under the control, enters the reactor inlet pipeline with the flow of 45kg/h, enters the bed reaction after the mixing of materials of coming with the upstream.Reactor outlet material is cooled to about 40 ℃ through heat exchange, enter vapour liquid separator and tell carrier gas, carrier gas loops back reactor inlet through the recycle compressor supercharging, and the separator liquid phase product is delivered to solvent recovery tower, solvent methanol steams from cat head and loops back reactive system, and the tower still is a crude caprolactam.The device steady running after 48 hours the sampling analysis crude caprolactam form and calculate transformation efficiency and selectivity, detailed process condition and the results are summarized in table 1.It should be noted that in the accumulation running vaporizer causes the heat exchange deleterious because of coking after 300 hours, temperature out drops to 158 ℃ by 167 ℃.
By table 1 as seen, adopt method of the present invention, under the lower situation of total carrier gas/oxime mol ratio, the method that hexanolactam selectivity (mol%) adopts apparently higher than Comparative Examples, consequently present method has low energy consumption and raw material consumption, has also avoided cyclohexanone-oxime at engineering problems such as heat-exchange equipment and pipeline cokings simultaneously.
Table 1 processing condition and result gather
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative Examples 1 |
| Reactor inlet pressure (MPa (g)) | 0.28 | 0.28 | 0.28 | 0.5 | 0.28 |
| The bed medial temperature (℃) | 375 | 382 | 373 | 367 | 376 |
| The vaporizer temperature out (℃) | -- | -- | -- | -- | 167-158 |
| Oxime weight space velocity (h -1) | 1.0 | 2.0 | 0.6 | 1.0 | 1.0 |
| Methyl alcohol/oxime (w/w) | 50/50 | 33/67 | 63/37 | 50/50 | 50/50 |
| Feed water/oxime (mol/mol) | 0.053 | 0.053 | 0.088 | 0.053 | 0.053 |
| Total nitrogen/oxime (mol/mol) | 25.1 | 12.6 | 41.8 | 25.1 | 55.2 |
| Nitrogen/oxime (mol/mol) in the beds | 75.2 | 37.8 | 125 | 75.2 | 55.2 |
| Cyclohexanone-oxime transformation efficiency (mol%) | 99.8 | 99.8 | 99.9 | 99.9 | 99.8 |
| Hexanolactam selectivity (mol%) | 97.5 | 97.5 | 97.4 | 97.4 | 96.2 |
Claims (21)
1. method by preparing caprolactam with cyclohexanone-oxime, comprise that the inert carrier gas heating back that will contain solvent feeds the carrier gas inlet of the first step reactor of the plural serial stage reactor that catalyzer is housed continuously, cyclohexanone-oxime is divided at least two parts of each levels that enter described plural serial stage reactor respectively, reaction effluent is cooled off, isolate carrier gas and be circulated to the carrier gas inlet of described first step reactor, liquid-phase reaction product is separated, purifies
Wherein
Described plural serial stage reactor is an insulation fix bed reactor,
Described plural serial stage reactor is made up of at least two reactors that are cascaded, and perhaps is the single reactor with at least two beds,
Described catalyzer is handle or the untreated MFI structural molecule sieve catalyst of the alkaline aqueous solution of process nitrogenous compound in advance.
2. the method for claim 1, the flow pattern that it is characterized in that material in the described plural serial stage reactor is upstriker or downstriker.
3. the process of claim 1 wherein that described inert carrier gas is the medium that do not react with cyclohexanone-oxime and hexanolactam or the mixture of described medium.
4. the method for claim 3, wherein inert carrier gas is selected from stable hydrocarbon and halohydrocarbon or their mixture that nitrogen, hydrogen, argon gas, ammonia, boiling point are not higher than 180 ℃.
5. the method for claim 1 is characterized in that described MFI structural molecule sieve catalyst is selected from the ZSM-5 molecular sieve of HTS, total silicon molecular sieve and silicon/aluminum ratio 〉=500.
6. the process of claim 1 wherein that described solvent is selected from C
1-C
6The straight or branched Fatty Alcohol(C12-C14 and C12-C18) or their mixture.
7. the method for claim 6, wherein said solvent is selected from methyl alcohol, ethanol, propyl alcohol and their mixture.
8. the process of claim 1 wherein that total mol ratio of inert carrier gas and cyclohexanone-oxime is 6-50.
9. the process of claim 1 wherein that inert carrier gas and cyclohexanone-oxime are 12-300 in the mol ratio of every stage reactor.
10. the method for claim 9, wherein inert carrier gas and cyclohexanone-oxime are 20-200 in the mol ratio of every stage reactor.
11. the process of claim 1 wherein that temperature of reaction is 200-500 ℃, pressure is 0.11-2.5MPa.
12. the method for claim 11, wherein temperature of reaction is 300-450 ℃, and pressure is 0.15-1.2MPa.
13. the process of claim 1 wherein that the weight space velocity of cyclohexanone-oxime is 0.2-8h
-1
14. the method for claim 13, wherein the weight space velocity of cyclohexanone-oxime is 0.5-6h
-1
15. the process of claim 1 wherein that the weight ratio of solvent and cyclohexanone-oxime is at 10-80: in the 90-20 scope.
16. the method for claim 15, wherein the weight ratio of solvent and cyclohexanone-oxime is at 20-70: in the 80-30 scope.
17. the process of claim 1 wherein and contain water in the reaction system, the mol ratio of water and cyclohexanone-oxime is 0.03-1.0.
18. the described method of claim 17, wherein the mol ratio of water and cyclohexanone-oxime is 0.05-0.35.
19. the method for claim 17, wherein water can be brought into by the reactor inlet injection or from recovered solvent.
20. the equipment by preparing caprolactam with cyclohexanone-oxime, this equipment comprises:
The plural serial stage reactor, the reactor that is cascaded of serving as reasons at least two is formed, and perhaps is the single reactor that comprises at least two beds, which is provided with feed(raw material)inlet, carrier gas inlet and reaction effluent outlet;
Separator is used for reaction effluent is carried out gas-liquid separation, which is provided with reaction effluent inlet, carrier gas outlet and discharge channel;
Solvent recovery tower is used for separating and the recovery solvent from the liquid-phase reaction product that separator is told, and which is provided with liquid-phase reaction product inlet, solvent outlet and crude product outlet;
Be used for well heater with the carrier gas heating;
Be used for reaction effluent refrigerative water cooler;
Be used to carry out the interchanger of reaction effluent and carrier gas heat exchange;
Be used to connect between the carrier gas inlet of the carrier gas outlet of separator and plural serial stage reactor, between the reaction effluent inlet of the reaction effluent outlet of plural serial stage reactor and separator, the parting liquid of the discharge channel of separator and the solvent recovery tower pipeline between entering the mouth, and will mix and provide pipeline with the circulation carrier gas from the solvent of solvent recovery tower solvent outlet to multistage tandem reactor.
21. the described equipment of claim 20 is characterized in that also comprising the carrier gas compressor for compressing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101774067A CN101434569B (en) | 2007-11-15 | 2007-11-15 | Method and equipment for preparing caprolactam from cyclohexanone oxime |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101774067A CN101434569B (en) | 2007-11-15 | 2007-11-15 | Method and equipment for preparing caprolactam from cyclohexanone oxime |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101434569A CN101434569A (en) | 2009-05-20 |
| CN101434569B true CN101434569B (en) | 2011-07-20 |
Family
ID=40709224
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101774067A Active CN101434569B (en) | 2007-11-15 | 2007-11-15 | Method and equipment for preparing caprolactam from cyclohexanone oxime |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101434569B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311386B (en) * | 2010-07-02 | 2013-05-15 | 天华化工机械及自动化研究设计院有限公司 | Caprolactam suspension filtering and washing method |
| CN102229553B (en) * | 2011-05-06 | 2012-10-10 | 清华大学 | Multistage rearrangement system and method for preparation of caprolactam from cyclohexanone oxime |
| CN102875469B (en) * | 2011-07-14 | 2015-01-14 | 中国石油化工股份有限公司 | Method for preparing caprolactam through adopting radial moving bed reactor |
| CN104513202B (en) * | 2013-09-29 | 2017-05-24 | 中国石油化工股份有限公司 | Cyclohexanone oxime conversion method |
| CN104876782B (en) * | 2014-02-27 | 2017-01-04 | 中国石油化工股份有限公司 | The method of the organic solvent of a kind of processing cycle and the preparation method of caprolactam |
| CN109400532B (en) * | 2018-12-29 | 2020-08-21 | 清华大学 | Method and device for preparing caprolactam from cyclohexanone oxime |
| CN110394134B (en) * | 2019-08-28 | 2024-04-19 | 沧州旭阳化工有限公司 | Cooling system |
| CN111848482A (en) * | 2020-08-11 | 2020-10-30 | 湖南百利工程科技股份有限公司 | Separation method of cyclohexanone oxime gas phase reaction rearrangement product |
| CN114507171A (en) * | 2022-02-24 | 2022-05-17 | 江苏扬农化工集团有限公司 | Preparation method of caprolactam |
| CN114507170A (en) * | 2022-02-24 | 2022-05-17 | 江苏扬农化工集团有限公司 | Process for preparing caprolactam |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1269360A (en) * | 1999-02-09 | 2000-10-11 | 住友化学工业株式会社 | Process for producing epsilon-hexanolactam |
| CN1273971A (en) * | 1999-03-16 | 2000-11-22 | 住友化学工业株式会社 | Method and equipment for prodn. of epsilon-hexanolactam |
-
2007
- 2007-11-15 CN CN2007101774067A patent/CN101434569B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1269360A (en) * | 1999-02-09 | 2000-10-11 | 住友化学工业株式会社 | Process for producing epsilon-hexanolactam |
| CN1273971A (en) * | 1999-03-16 | 2000-11-22 | 住友化学工业株式会社 | Method and equipment for prodn. of epsilon-hexanolactam |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101434569A (en) | 2009-05-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101434569B (en) | Method and equipment for preparing caprolactam from cyclohexanone oxime | |
| CN102875469B (en) | Method for preparing caprolactam through adopting radial moving bed reactor | |
| CN106518608B (en) | The continuous preparation method and device of cyclohexanedimethanol | |
| CN111574400B (en) | Separation method of ammoniated and dehydrated product of caprolactam and synthesis method of hexamethylene diamine | |
| CN101918357A (en) | Process and plant for urea production | |
| CN102317251B (en) | Process for the manufacturing of vinyl acetate | |
| CN101830807B (en) | Synthesizing device and process for alkyl nitrite | |
| CN113501770A (en) | Acetonitrile refining method | |
| CN109608340A (en) | The preparation method of N, N- dimethyl cyclohexyl amine | |
| CN114702375A (en) | Separation system and method for ethanol-to-acetaldehyde product | |
| CN113087641B (en) | Method for preparing 6-aminocapronitrile from cyclohexanone oxime | |
| CN103420776A (en) | Preparation method for methyl cyclopentene | |
| CN107082732A (en) | The method and apparatus that alkene is produced by dimethyl ether | |
| CN111848482A (en) | Separation method of cyclohexanone oxime gas phase reaction rearrangement product | |
| JP2008031155A (en) | Method for producing xylylenediamine | |
| CN1054366C (en) | Process for producing isopropyl amine | |
| JP2022534527A (en) | Enhanced Method for Dialkyl Ether Synthesis Using a Stepped Cone Reactor | |
| KR100566450B1 (en) | Continuous Method for Producing Aromatic Amines | |
| CN111253213A (en) | Process method and system for preparing ethanol by acetate hydrogenation | |
| CN102311323B (en) | Method for preparing butaldehyde by synthesizing propene and carbonyl syngas | |
| CN217757302U (en) | Separation system for catalyst and oxo-product in oxo-synthesis | |
| CN215975599U (en) | Acrylonitrile and acetonitrile coproduction device | |
| WO2022073525A1 (en) | Method for integrating ammoximation reaction and separation and device thereof | |
| CN113277924B (en) | Heat exchange system for propylene preparation | |
| CN107513016B (en) | Method for preparing methyl acetate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |