CN106946778A - A kind of preparation method of caprolactam - Google Patents
A kind of preparation method of caprolactam Download PDFInfo
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- CN106946778A CN106946778A CN201610008354.XA CN201610008354A CN106946778A CN 106946778 A CN106946778 A CN 106946778A CN 201610008354 A CN201610008354 A CN 201610008354A CN 106946778 A CN106946778 A CN 106946778A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- 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
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Abstract
The invention discloses a kind of preparation method of caprolactam, belong to chemical production technical field.Based on nucleophilic addition principle, using one kettle way, using alkali metal salt or alkali metal hydroxide as catalyst, using acetylene and caprolactam as raw material LP synthesizing caprolactam；Again by way of polar solvent recrystallization and vacuum distillation, different purity caprolactam is obtained.A kind of preparation method for caprolactam that the present invention is provided, technique is simple, easy to operate, reaction condition is gently controllable, efficiently solves moisture in system and there are problems that brought catalyst decomposes inactivation, avoid side reaction, reaction conversion ratio and product yield are improved, production cost is reduced, it is to avoid pollution of the organic solvent to environment, and the product of crystalline solid and the different appearance forrns of two kinds of liquid and purity is obtained, more conducively pack, use.
Description
Technical field
The invention belongs to chemical production technical field, it is related to a kind of preparation method of caprolactam, and in particular to
A kind of crystalline product of the preparation method of caprolactam and resulting different shape.
Background technology
Caprolactam (N-Vinyl Caprolactam), CAS:2235-00-9, Chinese is called N- ethene
Base caprolactam, 1- vinyl hexahydro -2H-Y heptan are because of -2- ketone etc..English name is called vinyl caprolactam, 1-
Ethenylhexahydro-2H-Azrpin-2-one, vinyl-epsilon-caprolactam etc..Its structural formula is as follows：
Caprolactam is the important intermediate for synthesizing poly-N-vinylcaprolactam.Poly-N-vinylcaprolactam
(PNVCL) it is the temperature sensitivity high polymer with low critical phase transition temperature (LCST).Its serial high polymer is in biological medicine, day
Prospect is extremely widely applied with having in chemicals, petrochemical.Therefore, exploitation caprolactam monomer and its polymerization
Thing production technology is significant.
The caprolactam synthesis route of current document report is mainly acetylene liquid phase addition process, with acetylene and
Caprolactam is raw material, with alkali metal caprolactam salt etc. for catalyst, under a certain pressure, at a temperature of reacted (referring to：
Feng Shubo etc., fine chemistry industry, 2008,25 (6), 610-613).There are following problems in the synthesis route：(1) with acyl in oneself
Amine and alkali metal hydroxide prepare catalyst caprolactam sylvite, then sylvite is added in reaction system reacted, by
In catalyst sylvite meet water or air can fast hydrolyzing, only short life, the secondly presence of water also results in raw material acyl in oneself
Amine open loop, segmentation, which prepares catalyst caprolactam sylvite, can not solve the problem of catalyst easy in inactivation.(2) the tertiary fourth of document report
The problem of potassium alcoholate or co-catalyst crown ether are solved in (1), but because expensive, only rest on the experimental stage, it is impossible to realize scale
Chemical industry is produced.(3) document report is using convention stir formula reactor, reaction condition or is high pressure 4-12MPa, or is high temperature
170-300 DEG C, operational danger is big, and technical difficulty is high.Under high pressure, hot conditions, reactor transmission device and axle rotate close
Envelope easily leakage, particularly acetylene gas leakage can cause serious consequence and influence surrounding enviroment.(4) special reaction device such as circulation
Injection reactor, only rests on the experimental stage, there is no method to realize industrialized production.(5) the acetylene liquid phase addition that document is reported
Method prepares caprolactam process conditions and is still in the lab scale stage, and reaction condition is extreme, the sticky easy solidification of reaction system, production
Product yield is generally relatively low.
Meanwhile, the caprolactam product of current document report is mainly purified using rectifying column way of purification,
There are following problems in the purifying technique：(1) equipment investment cost is high.(2) rectifying is more difficult to obtain high-purity ethylene base in oneself
Acid amides.(3) in its molecule of caprolactam there is high temperature rectifying and easily polymerize in activated double bonds.(4) reaction solution is deposited simultaneously
In catalyst and the complete raw material caprolactam of unreacted, under high temperature, alkalescence condition, the easy ring-opening polymerisation of caprolactam causes
Side reaction is more in distillation process, easily occurs that reaction can be associated, influences product yield.(5) product obtained after rectifying, normal temperature is preserved
Larger block crystalline solid is easily formed, it is necessary to which 200 DEG C of high temperature above heating could be melted and used, melting process easily causes product polymerization change
Color, is unfavorable for drum package storage.
Therefore, it is necessary to which the preparation method to existing caprolactam carries out further research with improving.
The content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of system of caprolactam
Preparation Method, for solving problems of the prior art.
In order to achieve the above objects and other related objects, first aspect present invention provides a kind of system of caprolactam
Preparation Method, comprises the following steps：
1) add caprolactam (I) in reactor and the compound (II) of alkali metal ion is provided, under vacuum
Heating melting dehydration, obtains alkali metal caprolactamate (III), the alkali metal caprolactamate (III) and caprolactam (I)
Form nucleophilic addition system；
2) it is passed through acetylene (IV) and carries out addition reaction, alkali metal caprolactamate (III) is reacted with acetylene (IV) and obtain
Caprolactam alkali metal salt (V), the caprolactam alkali metal salt (V) is reacted with caprolactam (I) again
To caprolactam (VI) and alkali metal caprolactamate (III)；
3) caprolactam (VI) is subjected to crystallization purifying in reactor, obtains preliminary purification product；
4) preliminary purification product is subjected to distillation purifying again in reactor, obtains final purified product.
Step 1) and step 2) reaction scheme it is as follows：
Preferably, in step 1) in, the performance indications of the caprolactam (I) are：White crystal under normal temperature；Fusing point is
68-71℃；Boiling point is 268.5 DEG C；Density is 1.0135g/cm3 (80 DEG C)；Flash-point is 152 DEG C；Freezing point is 69.2 DEG C；CAS
Number：105-60-2；Crystalline temperature >=68.9 DEG C；Acidity≤0.05mol/kg；Fe contents≤0.20mg/kg；Potassium permanganate absorption value
≤5；Cyclohexanone oxime content (mg/kg)≤20.
Preferably, in step 1) in, the compound (II) for providing alkali metal ion is alkali metal salt or alkali metal hydrogen
Oxide.
It is highly preferred that any one of the alkali metal salt in inorganic potassium salt, potassium methoxide, potassium ethoxide, potassium tert-butoxide.
It is highly preferred that the alkali metal hydroxide is potassium hydroxide.
Preferably, in step 1) in, the caprolactam (I) with provide alkali metal ion compound (II) quality it
Than for 3-200：0.5-50.
Preferably, in step 1) in, the reactor is conventional use of stirring reactor.
It is highly preferred that the specification condition of the reactor is：Volume：2-2000L；Inventory：0.2-1000kg；Temperature model
Enclose：50-200℃；Pressure：- 0.01 to 4MPa；Material：304 stainless steels.
Preferably, in step 1) in, the condition of the melting dehydration of heating under vacuum is：Temperature：80-150℃；
Stir speed (S.S.)：100-150rpm；Mixing time：30-240min；Vacuum：- 0.01 to -0.005MPa；Reaction time：30-
90min.The preparation condition can slough polar compound in reaction system.
Preferably, in step 2) in, the acetylene intake controls meter to be controlled by gas flow.The gas stream
Amount control is calculated as conventional use of gas flow control meter.
Preferably, in step 2) in, the acetylene is passed through condition and is：Throughput：0.01-70m3；Draft speed：50-
50000ml/min；Duration of ventilation：10min-30h.
It is highly preferred that the draft speed of the acetylene is advisable with keeping reactor temperature to change between ± 5 DEG C.
Preferably, in step 2) in, the condition of the addition reaction is：Design temperature：90-120 DEG C (sets in reactor
Temperature change control is determined between ± 5 DEG C)；Vacuum (setting pressure) in reactor：- 0.01 to 0.025MPa；Stir speed (S.S.)
80-150rpm；Reaction time：5-30h.
It is highly preferred that dropping to critical value at a temperature of nucleophilic addition system, it is when system pressure is begun to ramp up
The reaction end of addition reaction.
It is further preferred that the temperature threshold value is the lower limit of the design temperature.
It is further preferred that the system pressure, which is begun to ramp up, refers to that system pressure is begun to ramp up beyond setup pressure value.
Preferably, in step 3) in, the crystallization purifying is step 2) reaction terminate after, cooling, add polar solvent fill
Point stirring, cools, separates out product, centrifugal drying material obtains preliminary purification product again, and the purity of the preliminary purification product >=
95%.
It is highly preferred that the temperature of the cooling is down to less than 50 DEG C.It is further preferred that the temperature of the cooling is in 10-
Between 50 DEG C.
It is highly preferred that any one of the polar solvent in water, alcohol, ketone.
It is highly preferred that the ratio between volume that the caprolactam (VI) adds with polar solvent is 1-100：10-
200。
It is highly preferred that the temperature cooled again is reduced to -5 to -15 DEG C.
It is highly preferred that the centrifugal condition is：Centrifuging temperature：- 5 to -15 DEG C；Centrifugation time：5-60min；Centrifugation rate：
800-1500rpm。
Preferably, in step 4) in, the distillation purifying, for by step 3) in obtained preliminary purification product heats melt
Afterwards, vacuum distillation, collects product of distillation, produces final purified product, purity >=99% of the final purified product.
It is highly preferred that the heating melting temperature is 40-120 DEG C.The heating frit reaction is in convention stir distillation still
Can carry out.
It is highly preferred that the condition of the vacuum distillation is：Vacuum≤- 0.075MPa；100-180 DEG C of temperature.
Second aspect present invention provides the caprolactam that above-mentioned preparation method is prepared.
Preferably, the caprolactam is preliminary purification product or final purified product.
It is highly preferred that the performance parameter of the preliminary purification product is：Product purity >=95%；34-38 DEG C of fusing point；Its shape
State is white or pale yellow needles crystallization.The preliminary purification product can be preserved under 25 DEG C.
It is highly preferred that the performance parameter of the final purified product is：Product purity >=99%；34-37 DEG C of fusing point；Its shape
State is colourless or light yellow transparent liquid.The final purified product can be stored on 35 DEG C.
A kind of preparation method of caprolactam can also be used to prepare vinyl-based product.It is described vinyl-based
Product includes vinyl and adjoins pyrrolidone, triethylene glycol vinyl ethers, cyclohexanol vinyl ethers etc..
As described above, a kind of preparation method of caprolactam of the present invention, based on nucleophilic addition principle, is adopted
(i.e. one kettle way) is prepared with the disposable completion of same conventional reactor, using alkali metal salt or alkali metal hydroxide as catalyst,
Caprolactam is obtained using acetylene and caprolactam as raw material LP synthesizing.In preparation process, absolute is established
Vacuum reaction system, acetylene throughput and draft speed are effectively controlled by reaction temperature, in low pressure, gentle reaction temperature
Under, prepare the caprolactam of high-purity.Have the advantages that：
(1) preparation method for the vinyl machine lactams that the present invention is provided, reaction conversion ratio reaches more than 95%, passes through one
The crystallization of secondary polar solvent, secondarily purified distillation can obtain the product of different Dimensions, product purity is respectively >=95%, >=
99%, outward appearance is respectively white or yellowish acicular crystals, white or weak yellow liquid, total recovery >=85%.
(2) preparation method of caprolactam that the present invention is provided, using convention stir formula reactor, raw material is in oneself
Acid amides and catalyst are once put into, and one kettle way is directly reacted raw material and catalyst heating melting vacuum dehydration, fully fast
Fast removing system moisture, simplifies preparation process condition, efficiently solves moisture in system and there is brought catalyst decomposition
The problem of inactivation.
(3) by controlling reaction temperature and acetylene gas Ventilation Rate, i.e., it is prison to react design temperature change no more than 5%
Index is controlled, acetylene flow is controlled using acetylene flowmeter, insisting on of continuing rising high and reaction temperature with kettle internal pressure the change such as persistently reduces
Reaction end is determined, the consecutive complex reaction of product double bond initiation is reduced, the security of reaction, controllability, reaction is improved
Mild condition, it is to avoid side reaction generation, effectively increases reaction conversion ratio.
(4) reaction can be achieved under the lower pressure, it is to avoid because of high pressure, high temperature the production peace that leakage is brought occurs for acetylene
Full hidden danger, improves production technology safely controllable property and stability, and reduce production cost.
(5) it is by directly carrying out purified crystals using polar solvent, catalyst in reaction system and unreacted is complete
Caprolactam is effectively removed in crystalline mother solution, crystalline product purity is improved, when crystalline product is purified with vacuum distillation again, it is to avoid
Because the presence of impurity produces side reaction, the production cost of single pass rectifying purified product is reduced, crystallization purifying is improved
Yield, while having obtained the product of crystalline solid and the different mode of appearance of two kinds of liquid.
(6) under cryogenic conditions, caprolactam is separated out with crystalline state, it is to avoid high temperature polymerization reaction occurs, and improves
Purifying yield, meanwhile, crystalline ethylene base caprolactam is i.e. fusible at a lower temperature, can meet the bag of special medical material
Fill storage requirements.
(7) caprolactam after crystallization purifying be evaporated in vacuo purifying when, it is not necessary to rectifying column, equipment into
This substantially reduction and yield raising, product preserves more than 35 DEG C, does not form bulk crystals, more conducively pack, use.
Embodiment
The present invention is expanded on further with reference to specific embodiment, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention.
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
It should be clear that in the following example not specifically dated process equipment or device using conventional equipment in the art or
Device；All pressure values and scope are all referring to relative pressure.The reagent not indicated specifically in the following example uses in the market
The conventional reagent that can be bought.
In addition, it is to be understood that the one or more method and steps mentioned in the present invention do not repel before and after the combination step
There can also be other method step or other method step can also be inserted between the step of these are specifically mentioned, unless separately
It is described；It should also be understood that the combination annexation between the one or more equipment/devices mentioned in the present invention is not repelled
Can also have other equipment/device before and after the unit equipment/device or two equipment/devices specifically mentioning at these it
Between can also insert other equipment/device, unless otherwise indicated.Moreover, unless otherwise indicated, the numbering of various method steps is only
Differentiate the convenient tool of various method steps, rather than ordering or restriction enforceable model of the invention for limitation various method steps
Enclose, being altered or modified for its relativeness is of the invention enforceable when being also considered as in the case of without essence change technology contents
Category.
Embodiment 1
It is provided with one in electric mixer vacuum distillation apparatus and thermometer, the 3000ml four-hole bottles of gas valve,
It is separately added into caprolactam 400g, potassium hydroxide 12g vacuum distillations, heating melting dehydration, 80-150 DEG C of dehydration temperaturre, time
30-90min, vacuum -0.01 to -0.085MPa, until dripless outflow, forms nucleophilic addition system.
Acetylene is continually fed into above system, vinylation addition reaction is carried out.It is 120 DEG C to react design temperature, and
Reactor internal control design temperature changes, and makes design temperature change control between 120 ± 5 DEG C, pressure is 0-0.01MPa.Second
Alkynes throughput is 0.0786m3, draft speed is 160ml/min.As Continuous aeration 20min, system temperature continuous decrease is less than 90
DEG C, when system pressure is persistently increased beyond 0.01MPa, as reaction end, the reaction time is about 8h, obtains vinyl acyl in oneself
Amine.Analyzed using gas chromatography, reaction conversion ratio is 97.8%.
After reaction terminates, first time purifying is carried out, system temperature is first down to less than 50 DEG C, 1000g water is added and is used as pole
Property solvent, is sufficiently stirred for after dissolving, is cooled to -15 DEG C again, low-temperature centrifugation, and centrifugation time is 30min, and centrifugation rate is
800rpm.Preliminary purification Product samples 1# is produced, product 440g is separated out, product purity is 95.2%, fusing point is 37.1 DEG C, outward appearance
For white crystals, storage temperature is less than 20 DEG C.
The preliminary purification Product samples 1# of acquisition is carried out into second in 3000mL there-necked flasks again to purify, 100 DEG C of heating
Melting, be warming up to 120 DEG C, vacuum≤- 0.085MPa when, vacuum distillation produces final purified product sample 1*, separates out product
418g.Product purity is 99.5%, and fusing point is 36.2 DEG C, and outward appearance is weak yellow liquid, and storage temperature is 35 DEG C, gross mass yield
For 85%.
Embodiment 2
It is provided with one in electric mixer vacuum distillation apparatus and thermometer, the 3000ml four-hole bottles of gas valve,
Add caprolactam 500g, potassium hydroxide 15g vacuum distillations, heating melting dehydration, 100-150 DEG C of dehydration temperaturre, time 60-
90min, vacuum -0.085 to -0.001MPa, until dripless outflow, forms nucleophilic addition system.
Acetylene is continually fed into above system, vinylation addition reaction is carried out.It is 100 DEG C to react design temperature, and
Reactor internal control design temperature changes, and makes design temperature change control between 100 ± 5 DEG C, pressure is 0-0.025MPa.Second
Alkynes throughput is 0.0983m3, draft speed is 102ml/min.As Continuous aeration 25min, system temperature continuous decrease is less than 90
DEG C, when system pressure is persistently increased beyond 0.025MPa, as reaction end, the reaction time is about 16h, obtains vinyl in oneself
Acid amides.Analyzed using gas chromatography, reaction conversion ratio is 97.0%.
After reaction terminates, first time purifying is carried out, system temperature is first down to less than 40 DEG C, 1000g water is added and is used as pole
Property solvent, is sufficiently stirred for after dissolving, is cooled to -5 DEG C again, low-temperature centrifugation, and centrifugation time is 60min, and centrifugation rate is
1500rpm.Preliminary purification Product samples 2# is produced, product 570g is separated out, product purity is 95.4%, fusing point is 37.3 DEG C, outside
See as white crystals, storage temperature is less than 20 DEG C.
The preliminary purification Product samples 2# of acquisition is carried out into second in 3000mL there-necked flasks again to purify, 110 DEG C of heating
Melting, be warming up to 120 DEG C, vacuum≤- 0.075MPa when, vacuum distillation produces final purified product sample 2*, separates out product
528g.Product purity is 99.6%, and fusing point is 36.3 DEG C, and outward appearance is weak yellow liquid, and storage temperature is 35 DEG C, gross mass yield
For 86%.
Comparative example 1
In 500mL reactor, 200g caprolactams and 15gKOH are added, heating is melted, and heating-up temperature is 150
DEG C, vacuum is decompression dehydration under -0.085MPa, and the time is 60min, prepares 40g active catalyst hexanolactam sylvites,
It is cooled to 50 DEG C.
Caprolactam 1500g is added in 3000mL reactors, active hexanolactam sylvite is continuously heating to 170 DEG C, filled
Divide stirring, mixing speed is 100rpm, mixing time 30min.Build to be formed and added using the nucleophilic of phthalein amine sylvite as catalyst in oneself
Into reaction system.Acetylene is continually fed into this system, vinylation reaction is carried out.Pressure is 4-7MPa in kettle.Acetylene throughput
For 0.295m3, reaction time 6-18h, reaction conversion ratio is 50%.
After reaction terminates, pressure release turns material, and material directly distillation obtains caprolactam sample 1△, separate out product
627g, mass yield is 34%, and product purity is 93.0%, and fusing point is 38.5 DEG C.
Embodiment 3
By the vinyl in preliminary purification Product samples 1#, final purified product sample 1* and comparative example 1 in embodiment 1 oneself
Lactams sample 1△, carry out correlated performance test.Specific data result is shown in Table 1.
The performance test results comparison sheet of table 1
As shown in Table 1, the preliminary purification Product samples and final purified product sample prepared in the present embodiment 1, its product
Purity difference >=95% and >=99%, better than the caprolactam sample prepared in comparative example 1.Meanwhile, in the present embodiment 1
The final purified product sample prepared is white or light yellow transparent liquid, prepares solid sample compared to comparative example 1, does not form block
Shape crystal, more conducively packs, stores, uses.Moreover, sample prepared by the present embodiment 1 compares comparative example 1, fusing point is relatively low, can expire
The package storage demand of sufficient special medical material.
So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of preparation method of caprolactam, comprises the following steps：
1) add caprolactam (I) in reactor and the compound (II) of alkali metal ion is provided, heat under vacuum
Melting dehydration, obtains alkali metal caprolactamate (III), the alkali metal caprolactamate (III) and caprolactam (I) formation
Nucleophilic addition system；
2) it is passed through acetylene (IV) and carries out addition reaction, alkali metal caprolactamate (III) is reacted with acetylene (IV) and obtain ethene
Base alkali metal caprolactamate (V), the caprolactam alkali metal salt (V) obtains second with caprolactam (I) reaction again
Alkenyl caprolactam (VI) and alkali metal caprolactamate (III)；
3) caprolactam (VI) is subjected to crystallization purifying in reactor, obtains preliminary purification product；
4) preliminary purification product is subjected to distillation purifying again in reactor, obtains final purified product；
Step 1) and step 2) reaction scheme it is as follows：
。
2. the preparation method of caprolactam according to claim 1, it is characterised in that in step 1) in, it is described
The compound (II) for providing alkali metal ion is alkali metal salt or alkali metal hydroxide；The caprolactam (I) is with providing alkali
The mass ratio of the compound (II) of metal ion is 3-200：0.5-50.
3. the preparation method of caprolactam according to claim 1, it is characterised in that in step 1) in, it is described
The condition of heating melting dehydration is under vacuum：Temperature：80-150℃；Stir speed (S.S.)：100-150rpm；Mixing time：
30-240min；Vacuum：- 0.01 to -0.005MPa；Reaction time：30-90min.
4. the preparation method of caprolactam according to claim 1, it is characterised in that in step 2) in, it is described
Acetylene is passed through condition：Throughput：0.01-70m3；Draft speed：50-50000ml/min；Duration of ventilation：10min-30h.
5. the preparation method of caprolactam according to claim 1, it is characterised in that in step 2) in, it is described
The condition of addition reaction is：Design temperature：90-120 DEG C, the design temperature changes control between ± 5 DEG C in reactor；
Vacuum in reactor：- 0.01 to 0.025MPa；Stir speed (S.S.) 80-150rpm；Reaction time：5-30h.
6. the preparation method of caprolactam according to claim 1, it is characterised in that in step 3) in, it is described
Crystallization purifying, is step 2) reaction terminate after, cooling, add polar solvent be sufficiently stirred for, cool again, separate out product, centrifugation
Material is got rid of, preliminary purification product, purity >=95% of the preliminary purification product is obtained.
7. the preparation method of caprolactam according to claim 6, it is characterised in that the crystallization purifying includes
Any one of following condition is multinomial：
A) temperature of the cooling is down to less than 50 DEG C；
B) any one of the polar solvent in water, alcohol, ketone；
C) the ratio between volume of the caprolactam (VI) and polar solvent is 1-100：10-200；
D) temperature cooled again is reduced to -5 to -15 DEG C；
E) centrifugal condition is：Centrifuging temperature：- 5 to -15 DEG C；Centrifugation time：5-60min；Centrifugation rate：800-
1500rpm。
8. the preparation method of caprolactam according to claim 1, it is characterised in that in step 4) in, it is described
Distillation purifying, for by step 3) in after obtained preliminary purification product heats melting, vacuum distillation is collected product of distillation, produced
Final purified product, purity >=99% of the final purified product.
9. the preparation method of caprolactam according to claim 8, it is characterised in that the distillation purifying includes
Any one of following condition is multinomial：
A) the heating melting temperature is 40-120 DEG C；
B) condition of the vacuum distillation is：Vacuum≤- 0.075MPa；100-180 DEG C of temperature.
10. a kind of caprolactam, according to the preparation method system of any described caprolactams of claim 1-9
.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106946778B (en) | 2018-10-09 |
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