CN108558694A - A kind of process and device of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester - Google Patents
A kind of process and device of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester Download PDFInfo
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- CN108558694A CN108558694A CN201810643229.5A CN201810643229A CN108558694A CN 108558694 A CN108558694 A CN 108558694A CN 201810643229 A CN201810643229 A CN 201810643229A CN 108558694 A CN108558694 A CN 108558694A
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- benzene
- distillation column
- reactive distillation
- reaction
- oxalyl
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- 238000000034 method Methods 0.000 title claims abstract description 50
- 230000008569 process Effects 0.000 title claims abstract description 45
- 238000010924 continuous production Methods 0.000 title claims abstract description 36
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 258
- 238000000066 reactive distillation Methods 0.000 claims abstract description 75
- 238000006243 chemical reaction Methods 0.000 claims abstract description 67
- 239000002994 raw material Substances 0.000 claims abstract description 47
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000012024 dehydrating agents Substances 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- 235000019441 ethanol Nutrition 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 11
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000605 extraction Methods 0.000 claims abstract description 6
- 238000009833 condensation Methods 0.000 claims abstract description 5
- 230000005494 condensation Effects 0.000 claims abstract description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 64
- 235000006408 oxalic acid Nutrition 0.000 claims description 19
- 230000018044 dehydration Effects 0.000 claims description 12
- 238000006297 dehydration reaction Methods 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 10
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 9
- 238000004581 coalescence Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 7
- 230000000391 smoking effect Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 description 4
- LXNHXLLTXMVWPM-UHFFFAOYSA-N pyridoxine Chemical compound CC1=NC=C(CO)C(CO)=C1O LXNHXLLTXMVWPM-UHFFFAOYSA-N 0.000 description 4
- KATRFCCKXHEDJB-BYPYZUCNSA-N 2-[[(2S)-1-ethoxy-1-oxopropan-2-yl]amino]-2-oxoacetic acid Chemical compound C(C)OC([C@@H](NC(C(=O)O)=O)C)=O KATRFCCKXHEDJB-BYPYZUCNSA-N 0.000 description 3
- 125000004494 ethyl ester group Chemical group 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- RADKZDMFGJYCBB-UHFFFAOYSA-N pyridoxal hydrochloride Natural products CC1=NC=C(CO)C(C=O)=C1O RADKZDMFGJYCBB-UHFFFAOYSA-N 0.000 description 2
- 239000011726 vitamin B6 Substances 0.000 description 2
- 235000019158 vitamin B6 Nutrition 0.000 description 2
- 229940011671 vitamin b6 Drugs 0.000 description 2
- QNAYBMKLOCPYGJ-UHFFFAOYSA-N D-alpha-Ala Natural products CC([NH3+])C([O-])=O QNAYBMKLOCPYGJ-UHFFFAOYSA-N 0.000 description 1
- QNAYBMKLOCPYGJ-UWTATZPHSA-N L-Alanine Natural products C[C@@H](N)C(O)=O QNAYBMKLOCPYGJ-UWTATZPHSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229960003767 alanine Drugs 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a kind of process and device of continuous production N ethoxies oxalyl L alanine ethyl esters, and using benzene as dehydrating agent, preparation raw material mixed liquor is dissolved in batching kettle；The raw material mixed liquor of preparation is transported to preheater to preheat；Material is heated to 70 DEG C to 85 DEG C successive reactions by reboiler；Benzene is inputted into reactive distillation column, and the moisture that reaction generates continuously is sloughed using benzene as dehydrating agent；The water that reaction is generated, it is steamed from the tower top of reactive distillation column in the form of benzene, ethyl alcohol, water ternary azeotrope, after condensed device condensation, it is automatically subjected to phase splitting again by coalescing phase-splitter, benzene of the upper layer containing a small amount of water, ethyl alcohol is mutually back to reactive distillation column after split-phase, and ethanol water phase extraction of the lower layer containing a small amount of benzene goes subsequently to be dehydrated workshop section；It continuously goes to the reaction was complete in reactive distillation column and has removed the kettle liquid of water follow-up workshop section and carries out product separation.Present device is few, and floor space is small；Reaction efficiency is high；Full-automatic save manually can be achieved；It is at low cost.
Description
Technical field
The present invention relates to a kind of processes and device of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, belong to N-
Ethoxy oxalyl-l-Alanine ethyl ester production technical field.
Background technology
Vitamin B6 is found in the 1930s, belonging to water soluble vitamin, and N- ethoxies oxalyl-l-Alanine ethyl ester is also known as
N- oxalyl objects are the important intermediates for synthesizing vitamin B6.At present in the production process of N- ethoxies oxalyl-l-Alanine ethyl ester
In, traditional handicraft is reacted and is dehydrated using one or more batch reactors, produces material again after complete dehydration to follow-up point
From workshop section, the reaction kettle that this traditional handicraft needs under same treatment amount is more, and equipment investment is huge, takes up a large area, and efficiency is low,
Energy consumption, operating cost and labour cost are high.
The Chinese patent of Publication No. CN1193006C discloses a kind of preparation side of N- ethoxies oxalyl-alanine ethyl ester
Method is in molar ratio：α-alanine: oxalic acid: ethyl alcohol: diethy-aceto oxalate: benzene=1: 1~2: 3~6: 0.5~1.5: 1~4 body
In system, the moisture in continuously sloughing system under the reaction condition for being heated to 70 DEG C~85 DEG C a, step completes the ester of α-alanine
Change, is acylated, generating N- ethoxies oxalyl-alanine ethyl ester.Although the technical solution discloses N- ethoxies oxalyl-alanine ethyl ester system
A standby formula, but there is no the specific technical solutions of open industrial manufacturing processes.
Invention content
The present invention is in view of the deficienciess of the prior art, provide a kind of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester
Process and device all individually feed intake, heat up without every kettle compared with traditional reaction kettle intermittent reaction dewatering process
Process, simplify technological process, reduce equipment, reduce occupation area of equipment, improve reaction efficiency, reduce investment at
This.
The technical solution that the present invention solves above-mentioned technical problem is as follows：A kind of continuous production N- ethoxies oxalyl-l-Alanine
The process of ethyl ester, the process include the following steps：
(1) raw material is prepared：Using benzene as dehydrating agent, dissolving preparation l-Alanine, oxalic acid, ethyl alcohol and oxalic acid two in batching kettle
Ethyl ester reaction raw materials mixed liquor；
(2) raw material preheating：The raw material mixed liquor of preparation is transported to preheater to preheat, raw material mixed liquor is made to be preheating to
50 to 70 DEG C；
(3) heating reaction：Raw material mixed liquor after preheating is transported to reactive distillation column, is heated material by reboiler
To 70 DEG C to 85 DEG C successive reactions；
(4) reaction dehydration：Benzene is inputted into reactive distillation column, and the water that reaction generates continuously is sloughed using benzene as dehydrating agent
Point；
(5) split-phase is condensed：The water that reaction is generated, from reactive distillation column in the form of benzene, ethyl alcohol, water ternary azeotrope
Tower top steams, and after the condensation of condensed device, then is automatically subjected to phase splitting by coalescing phase-splitter, benzene of the upper layer containing a small amount of water, ethyl alcohol after split-phase
It is mutually back to reactive distillation column, ethanol water phase extraction of the lower layer containing a small amount of benzene goes subsequently to be dehydrated workshop section；
(6) product detaches：By the reaction was complete in reactive distillation column and removed water kettle liquid continuously go to follow-up workshop section into
Row product detaches.
A kind of process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester as described above, the step (1)
In, it is prepared the stage in raw material, the feed postition of dehydrating agent benzene is to be added at one time, and the addition of benzene is the 1 to 2 of oxalic acid addition
Times.Benzene can reduce the moisture in material or remove the crystallization water in compound molecule, the stage is prepared in raw material as dehydrating agent
It is first added at one time the benzene of 1 to 2 times of oxalic acid amount, to be dehydrated for the first time in the preparation stage.
A kind of process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester as described above, the step (3)
In, the moisture generated to reactive distillation column in reaction process is detected, and judges whether the moisture that reaction generates removes completely.It is logical
The water content detection to generation is crossed, on the one hand judges whether the water that reaction generates removes completely, on the other hand can also judge to react
Carry out degree.
A kind of process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester as described above, the step (3)
In, according to the length of reaction time T, residence time t of the increase and decrease raw material mixed liquor in reactive distillation column, the residence time, t was more than
Reaction time T.Reaction time T is judged according to the amount, mixability and reaction temperature etc. of the reaction raw materials of addition, makes stop
Time t is more than reaction time T, to ensure that raw material mixed liquor adequately reacts in reactive distillation column.
A kind of process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester as described above, the step (4)
In, in the reaction water smoking, the amount that benzene is inputted into reactive distillation column is 2 to 3 times of the oxalic acid addition in step (1), to
It inputs the mode of benzene in reactive distillation column to feed for continuity, the rate of continuity charging is to input benzene into reactive distillation column
The residence time t of amount divided by raw material mixed liquor in reactive distillation column.In the reaction water smoking according to the amount and raw material of input benzene
Residence time t of the mixed liquor in reactive distillation column, continuously inputs benzene into reactive distillation column, in combination with preparation rank
The benzene that is added at one time of section continuously sloughs the moisture that reaction generates collectively as dehydrating agent, using being added at one time and duration
The mode combined is added, benzene can be made adequately to be dehydrated as dehydrating agent.
The present invention also provides a kind of process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, the technique dress
It sets including batching kettle, preheater, reactive distillation column, reboiler, condenser and coalescence phase-splitter；The batching kettle is connected with first
The bottom of defeated benzene pipeline, liquid addition pipeline and solid feed feed pot, the batching kettle is connected to the preheater；It is described pre-
Hot device connects in the middle part of the reactive distillation column；The reactive distillation column lower part is connected with the second defeated benzene pipeline；The reboiler connects
Connect the reactive distillation column tower reactor；The condenser connects the tower top of the reactive distillation column；The coalescence phase-splitter is connected to
Between the condenser and reactive distillation column top.
A kind of process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester as described above, the batching kettle bottom
It is connected with transfering material pump between portion and the preheater.The raw material mixed liquor of preparation in batching kettle is transported to preheater by transfering material pump
In, so that raw material mixed liquor is preheating to 50 to 70 DEG C in preheater.
A kind of process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester as described above, the coalescence split-phase
Device is connected with follow-up dehydration pipeline.Follow-up dehydration pipeline will coalesce ethanol water phase of the phase-splitter lower layer containing a small amount of benzene and produce and convey
To follow-up dehydration workshop section.
A kind of process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester as described above, the reactive distillation
The bottom of tower is connected with later separation pipeline.Later separation pipeline is by the reaction was complete in reactive distillation column and has removed the kettle liquid of water
It continuously goes to follow-up workshop section and carries out product separation.
A kind of process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester as described above, the first defeated benzene
Conveying has the dehydrating agent benzene of preparation in pipeline；Conveying has the dehydrating agent benzene of reaction in the second defeated benzene pipeline；The liquid
Conveying has oxalic acid, ethyl alcohol and diethy-aceto oxalate in body charge line；L-Alanine is added in the solid feed feed pot.
The beneficial effects of the invention are as follows：Using benzene as dehydrating agent, dissolving preparation l-Alanine, oxalic acid, ethyl alcohol in batching kettle
With diethy-aceto oxalate reaction raw materials mixed liquor, the raw material mixed liquor of preparation is transported to preheater and is preheated, after preheating
Raw material mixed liquor is transported to reactive distillation column, and benzene is inputted into reactive distillation column, and reaction production is continuously sloughed using benzene as dehydrating agent
Raw moisture；The water that reaction is generated, is steamed in the form of benzene, ethyl alcohol, water ternary azeotrope from the tower top of reactive distillation column, is passed through
Condenser condensation after, then by coalesce phase-splitter be automatically subjected to phase splitting, benzene of the upper layer containing a small amount of water, ethyl alcohol is mutually back to reaction after split-phase
Rectifying column, ethanol water phase extraction of the lower layer containing a small amount of benzene go subsequently to be dehydrated workshop section；By the reaction was complete in reactive distillation column and removes
The kettle liquid of complete water continuously goes to follow-up workshop section and carries out product separation.Present invention process appliance arrangement is few, and floor space is small；Reaction effect
Rate is high；Full-automatic save manually can be achieved；It is energy saving, save operating cost；Equipment and place investment cost are few.
Description of the drawings
Fig. 1 is the process method flow chart of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester；
Fig. 2 is the process unit schematic diagram of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester；
Wherein, 1：Batching kettle；2：Preheater；3：Reactive distillation column；4：Reboiler；5：Condenser；6：Coalesce phase-splitter；7：
First defeated benzene pipeline；8：Liquid addition pipeline；9：Solid feed feed pot；10：Second defeated benzene pipeline；11：Transfering material pump；12：Afterwards
Continuous dehydration pipeline；13：Later separation pipeline.
Specific implementation mode
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below in conjunction with the accompanying drawings to the present invention
Specific implementation mode be described in detail.Many details are elaborated in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case of violating intension of the present invention, therefore the present invention is not limited by following public specific embodiment.
Unless otherwise defined, all of technologies and scientific terms used here by the article and belong to the technical field of the present invention
The normally understood meaning of technical staff is identical.Used term is intended merely to description tool in the description of the invention herein
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more
Any and all combinations of relevant Listed Items.
As depicted in figs. 1 and 2, a kind of process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, the technique
Method includes the following steps：
S1：Raw material is prepared：Using benzene as dehydrating agent, dissolving preparation l-Alanine, oxalic acid, ethyl alcohol and oxalic acid two in batching kettle
Ethyl ester reaction raw materials mixed liquor；
S2：Raw material preheating：The raw material mixed liquor of preparation is transported to preheater to preheat, raw material mixed liquor is made to be preheating to
50 to 70 DEG C；
S3：Heating reaction：Raw material mixed liquor after preheating is transported to reactive distillation column, is heated material by reboiler
To 70 DEG C to 85 DEG C successive reactions；
S4：Reaction dehydration：Benzene is inputted into reactive distillation column, and the water that reaction generates continuously is sloughed using benzene as dehydrating agent
Point；
S5：Condense split-phase：The water that reaction is generated, from reactive distillation column in the form of benzene, ethyl alcohol, water ternary azeotrope
Tower top steams, and after the condensation of condensed device, then is automatically subjected to phase splitting by coalescing phase-splitter, benzene of the upper layer containing a small amount of water, ethyl alcohol after split-phase
It is mutually back to reactive distillation column, ethanol water phase extraction of the lower layer containing a small amount of benzene goes subsequently to be dehydrated workshop section；
S6：Product detaches：By the reaction was complete in reactive distillation column and removed water kettle liquid continuously go to follow-up workshop section into
Row product detaches.
In one embodiment of the process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, the step (1)
In, it is prepared the stage in raw material, the feed postition of dehydrating agent benzene is to be added at one time, and the addition of benzene is the 1 to 2 of oxalic acid addition
Times.Benzene can reduce the moisture in material or remove the crystallization water in compound molecule, the stage is prepared in raw material as dehydrating agent
It is first added at one time the benzene of 1 to 2 times of oxalic acid amount, to be dehydrated for the first time in the preparation stage.
In one embodiment of the process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, the step (3)
In, the moisture generated to reactive distillation column in reaction process is detected, and judges whether the moisture that reaction generates removes completely.It is logical
The water content detection to generation is crossed, on the one hand judges whether the water that reaction generates removes completely, on the other hand can also judge to react
Carry out degree.In the step (3), according to the length of reaction time T, increase and decrease raw material mixed liquor stops in reactive distillation column
Time t, residence time t is stayed to be more than reaction time T.Reaction time T is according to the amount, mixability and reaction of the reaction raw materials of addition
Temperature etc. is judged, residence time t is made to be more than reaction time T, to ensure raw material mixed liquor in reactive distillation column fully
Reaction.
In one embodiment of the process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, the step (4)
In, in the reaction water smoking, the amount that benzene is inputted into reactive distillation column is 2 to 3 times of the oxalic acid addition in step (1), to
It inputs the mode of benzene in reactive distillation column to feed for continuity, the rate of continuity charging is to input benzene into reactive distillation column
The residence time t of amount divided by raw material mixed liquor in reactive distillation column.In the reaction water smoking according to the amount and raw material of input benzene
Residence time t of the mixed liquor in reactive distillation column, continuously inputs benzene into reactive distillation column, in combination with preparation rank
The benzene that is added at one time of section continuously sloughs the moisture that reaction generates collectively as dehydrating agent, using being added at one time and duration
The mode combined is added, benzene can be made adequately to be dehydrated as dehydrating agent.
Referring to Fig. 2, the present invention also provides a kind of process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, institutes
It includes batching kettle 1, preheater 2, reactive distillation column 3, reboiler 4, condenser 5 and coalescence phase-splitter 6 to state process unit；It is described to match
Material kettle 1 is connected with the first defeated benzene pipeline 7, liquid addition pipeline 8 and solid feed feed pot 9, the bottom connection of the batching kettle 1
To the preheater 2；The preheater 2 connects 3 middle part of the reactive distillation column；3 lower part of the reactive distillation column is connected with
Two defeated benzene pipelines 10；The reboiler 4 connects 3 tower reactor of the reactive distillation column；The condenser 5 connects the reactive distillation column
3 tower top；The coalescence phase-splitter 6 is connected between 3 top of the condenser 5 and reactive distillation column.
In one embodiment of the process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, 1 bottom of the batching kettle
Transfering material pump 11 is connected between portion and the preheater 2.The raw material mixed liquor of preparation in batching kettle 1 is transported to by transfering material pump 11
In preheater 2, raw material mixed liquor is made to be preheating to 50 to 70 DEG C in preheater 2.
In one embodiment of the process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, the coalescence split-phase
Device 6 is connected with follow-up dehydration pipeline 12.Follow-up dehydration pipeline 12 will coalesce ethanol water phase of 6 lower layer of phase-splitter containing a small amount of benzene and produce
And it is transported to follow-up dehydration workshop section.
In one embodiment of the process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, the reactive distillation
The bottom of tower 3 is connected with later separation pipeline 13.Later separation pipeline 13 is by the reaction was complete and has removed water in reactive distillation column 3
Kettle liquid continuously go to follow-up workshop section and carry out product separation.
In one embodiment of the process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, the first defeated benzene
Conveying has the dehydrating agent benzene of preparation in pipeline 7；Conveying has the dehydrating agent benzene of reaction in the second defeated benzene pipeline 10；It is described
Conveying has oxalic acid, ethyl alcohol and diethy-aceto oxalate in liquid addition pipeline 8；The third ammonia of L- is added in the solid feed feed pot 9
Acid.
The present invention is using benzene as dehydrating agent, dissolving preparation l-Alanine, oxalic acid, ethyl alcohol and diethy-aceto oxalate in batching kettle 1
The raw material mixed liquor of preparation is transported to preheater 2 and preheated by reaction raw materials mixed liquor, and the raw material mixed liquor after preheating is defeated
It is sent to reactive distillation column 3, benzene is inputted into reactive distillation column 3, the moisture that reaction generates continuously is sloughed using benzene as dehydrating agent；It will
The water generated is reacted, is steamed from the tower top of reactive distillation column 3 in the form of benzene, ethyl alcohol, water ternary azeotrope, condensed device 5 is cold
It after solidifying, then is automatically subjected to phase splitting by coalescing phase-splitter 6, benzene of the upper layer containing a small amount of water, ethyl alcohol is mutually back to reactive distillation column after split-phase
3, ethanol water phase extraction of the lower layer containing a small amount of benzene goes subsequently to be dehydrated workshop section；By the reaction was complete and has removed water in reactive distillation column 3
Kettle liquid continuously go to follow-up workshop section and carry out product separation.Present invention process appliance arrangement is few, and floor space is small；Reaction efficiency
It is high；Full-automatic save manually can be achieved；It is energy saving, save operating cost；Equipment and place investment cost are few.
Each technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, it is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, it is characterised in that：The process packet
Include following steps：
(1) raw material is prepared：Using benzene as dehydrating agent, dissolving preparation l-Alanine, oxalic acid, ethyl alcohol and diethy-aceto oxalate in batching kettle
Reaction raw materials mixed liquor；
(2) raw material preheating：The raw material mixed liquor of preparation is transported to preheater to preheat, make raw material mixed liquor be preheating to 50 to
70℃；
(3) heating reaction：Raw material mixed liquor after preheating is transported to reactive distillation column, material is heated to 70 by reboiler
DEG C to 85 DEG C of successive reactions；
(4) reaction dehydration：Benzene is inputted into reactive distillation column, and the moisture that reaction generates continuously is sloughed using benzene as dehydrating agent；
(5) split-phase is condensed：The water that reaction is generated, from the tower top of reactive distillation column in the form of benzene, ethyl alcohol, water ternary azeotrope
It steams, after the condensation of condensed device, then is automatically subjected to phase splitting by coalescing phase-splitter, benzene phase of the upper layer containing a small amount of water, ethyl alcohol is returned after split-phase
Reactive distillation column is flowed back to, ethanol water phase extraction of the lower layer containing a small amount of benzene goes subsequently to be dehydrated workshop section；
(6) product detaches：It continuously goes to the reaction was complete in reactive distillation column and has removed the kettle liquid of water follow-up workshop section and produces
Product detach.
2. a kind of process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester according to claim 1, feature
It is：It in the step (1), is prepared the stage in raw material, the feed postition of dehydrating agent benzene is to be added at one time, and the addition of benzene is
1 to 2 times of oxalic acid addition.
3. a kind of process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester according to claim 1, feature
It is：In the step (3), the moisture generated to reactive distillation column in reaction process is detected, and judges the water that reaction generates
Divide and removes whether completely.
4. a kind of process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester according to claim 1, feature
It is：In the step (3), according to the length of reaction time T, residence time of the increase and decrease raw material mixed liquor in reactive distillation column
T, residence time t are more than reaction time T.
5. a kind of process of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester according to claim 1, feature
It is：In the step (4), in the reaction water smoking, the amount of benzene is inputted into reactive distillation column and is added for the oxalic acid in step (1)
Enter 2 to 3 times of amount, the mode of benzene is inputted into reactive distillation column and is fed for continuity, the rate of continuity charging is to reaction
The residence time t of the amount divided by raw material mixed liquor of benzene in reactive distillation column is inputted in rectifying column.
6. a kind of process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester, it is characterised in that：The process unit packet
Include batching kettle, preheater, reactive distillation column, reboiler, condenser and coalescence phase-splitter；The batching kettle is connected with the first defeated benzene
The bottom of pipeline, liquid addition pipeline and solid feed feed pot, the batching kettle is connected to the preheater；The preheater
It connects in the middle part of the reactive distillation column；The reactive distillation column lower part is connected with the second defeated benzene pipeline；The reboiler connects institute
State reactive distillation column tower reactor；The condenser connects the tower top of the reactive distillation column；The coalescence phase-splitter is connected to described
Between condenser and reactive distillation column top.
7. a kind of process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester according to claim 6, feature
It is：It is connected with transfering material pump between the batching kettle bottom and the preheater.
8. a kind of process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester according to claim 6, feature
It is：The coalescence phase-splitter is connected with follow-up dehydration pipeline.
9. a kind of process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester according to claim 6, feature
It is：The bottom of the reactive distillation column is connected with later separation pipeline.
10. a kind of process unit of continuous production N- ethoxies oxalyl-l-Alanine ethyl ester according to claim 6, special
Sign is：Conveying has the dehydrating agent benzene of preparation in the first defeated benzene pipeline；Conveying has reaction in the second defeated benzene pipeline
Dehydrating agent benzene；Conveying has oxalic acid, ethyl alcohol and diethy-aceto oxalate in the liquid addition pipeline；The solid feed feed pot
It is interior to be added with l-Alanine.
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| CN201810643229.5A CN108558694B (en) | 2018-06-21 | Technological method and device for continuously producing N-ethoxyoxalyl-L-alanine ethyl ester |
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| CN201810643229.5A CN108558694B (en) | 2018-06-21 | Technological method and device for continuously producing N-ethoxyoxalyl-L-alanine ethyl ester |
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| Publication Number | Publication Date |
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| CN108558694B CN108558694B (en) | 2024-05-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109293525A (en) * | 2018-09-26 | 2019-02-01 | 山东新和成精化科技有限公司 | A kind of micro passage reaction and the method for preparing N- alkyloxy oxalyl alanine ester using the micro passage reaction |
| CN116332783A (en) * | 2021-12-23 | 2023-06-27 | 杭州鑫富科技有限公司 | Continuous preparation method of N-ethoxyoxalyl alanine ethyl ester |
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| CN102311360A (en) * | 2011-07-11 | 2012-01-11 | 湖北惠生药业有限公司 | Method for preparing N-ethoxy oxalyl alanine ethyl ester |
| CN104725262A (en) * | 2013-12-23 | 2015-06-24 | 大丰海嘉诺药业有限公司 | Method for continuously preparing N-ethyloxyl oxalyl alanine ethyl ester |
| CN107827779A (en) * | 2017-10-30 | 2018-03-23 | 烟台国邦化工机械科技有限公司 | Batch reactive distillation production cyanoacetate compound, malonate compound device and its production technology |
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| CN104725262A (en) * | 2013-12-23 | 2015-06-24 | 大丰海嘉诺药业有限公司 | Method for continuously preparing N-ethyloxyl oxalyl alanine ethyl ester |
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| CN109293525A (en) * | 2018-09-26 | 2019-02-01 | 山东新和成精化科技有限公司 | A kind of micro passage reaction and the method for preparing N- alkyloxy oxalyl alanine ester using the micro passage reaction |
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