CN107793329A - A kind of isolation and purification method of cyanoacetic acid - Google Patents

A kind of isolation and purification method of cyanoacetic acid Download PDF

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Publication number
CN107793329A
CN107793329A CN201711033865.8A CN201711033865A CN107793329A CN 107793329 A CN107793329 A CN 107793329A CN 201711033865 A CN201711033865 A CN 201711033865A CN 107793329 A CN107793329 A CN 107793329A
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China
Prior art keywords
tower
cyanoacetic acid
dehydration
column
dehydrating
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CN201711033865.8A
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Inventor
张燕
毛学峰
赵帅
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YANTAI GUOBANG CHEMICAL MACHINE TECHNOLOGY Co Ltd
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YANTAI GUOBANG CHEMICAL MACHINE TECHNOLOGY Co Ltd
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Priority to CN201711033865.8A priority Critical patent/CN107793329A/en
Publication of CN107793329A publication Critical patent/CN107793329A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C253/00Preparation of carboxylic acid nitriles
    • C07C253/32Separation; Purification; Stabilisation; Use of additives
    • C07C253/34Separation; Purification

Abstract

A kind of isolation and purification method of cyanoacetic acid, including material treatment process and crude product refining process, step include:Material treatment process and crude product refining process.Material treatment process is dehydrated using triple effect, and crude product refining process is refined using single-action or economic benefits and social benefits refine.In the present invention, (1) many places make full use of energy, energy consumption is low using the coupling of vapours and reboiler;(2) cyanoacetic acid content is low in the water isolated, and is refined using triple effect dehydration and single-action, cyanoacetic acid content can drop to below 500ppm in water;Refined using triple effect dehydration and economic benefits and social benefits, cyanoacetic acid content can drop to 300 below 400ppm in water;Reduce waste water subsequent treatment expense so that cyanoacetic acid loss is small;(3) cyanoacetic acid high income, 95% 99.5% can be reached.

Description

A kind of isolation and purification method of cyanoacetic acid
Technical field
The present invention relates to a kind of isolation and purification method of cyanoacetic acid, belong to material separation technology field.
Background technology
Cyanoacetic acid is using monoxone, sodium carbonate, Cymag as raw material, and neutralized, cyaniding, hydrochloric acid are acidified and obtained.Its reclaimed water Point content and salt content are higher, need to be further purified during use.Because cyanoacetic acid concentration is low in cyanoacetic acid mixed solution, water It is high with the content of salt, therefore concentration process need to consume substantial amounts of steam, and after evaporation the phase largely separate out because of sodium chloride, conduct heat Difference, easily decompose cyanoacetic acid.
CN200810052135.7 discloses a kind of preparation method of high purity solid cyanoacetic acid, with esters solvent to obtaining To cyanoacetic acid and the mixture of sodium chloride extracted, extract is evaporated under reduced pressure and is concentrated to give high-purity solid cyanoacetic acid.But Organic solvent amount used is big, and (ratio of solvent and mixed liquor is 1-5:1), extraction times 4-8 times, it is cumbersome, cost is high.
CN201510810110.9 discloses a kind of preparation method of cyanoacetic acid and its derivative, by obtained cyanoacetic acid and The mixed solution of sodium chloride is separated into cyanoacetic acid solution and sodium chloride solution with continuous chromatography, avoids traditional distillation and concentration point The shortcomings that cyanoacetic acid from caused by largely decomposes, yield is low, but it is only suitable for small-scale production.
The content of the invention
The present invention is in view of the deficienciess of the prior art, provide a kind of isolation and purification method of cyanoacetic acid.
The technical scheme that the present invention solves above-mentioned technical problem is as follows:A kind of isolation and purification method of cyanoacetic acid, including original Expect that handling process and crude product refining process, step are as follows:
(1) material treatment process
By mainly contain cyanoacetic acid, NaCl, water raw material inputted from the first dehydrating tower tower reactor, the thing of the first dehydrating tower tower reactor Material is heated by the first dehydration column reboiler, and main component rises to the first dehydration column overhead for the steam of water, stays in the first dehydration The material of tower tower reactor is delivered to the second dehydrating tower, and the material of the second dehydrating tower tower reactor is heated by the second dehydration column reboiler, mainly Composition rises to the second dehydration column overhead for the steam of water, and the material for staying in the second dehydrating tower tower reactor is delivered to the 3rd dehydrating tower, The material of 3rd dehydrating tower tower reactor is heated by the 3rd dehydration column reboiler, and main component rises to the 3rd dehydrating tower for the steam of water Tower top, enter after staying in the material progress desalting processing of the 3rd dehydrating tower tower reactor from the middle part of the first treating column;
(2) crude product refining process
The material of first treating column tower reactor vaporizes after being heated by the first treating column reboiler to be risen, and main component is the steaming of water Vapour rises to the first refined column overhead, and the first treating column kettle material is cooled down, desalting processing obtains cyanoacetic acid product.
The beneficial effects of the invention are as follows:By triple effect dehydrating tower dehydration and desalting processing after, can obtain content 70% with On cyanoacetic acid solution, after single-action treating column is refined, obtain more than 99% cyanoacetic acid solution.
On the basis of above-mentioned technical proposal, the present invention can also do following improvement.
Before first treating column kettle material carries out desalting processing, it is introduced into the second treating column and carries out with the first treating column process The same distillation process, the second treating column kettle material carry out desalting processing and obtain cyanoacetic acid product.Economic benefits and social benefits treating column can be more thorough The moisture of sloughing at bottom the purity for not improving cyanoacetic acid, obtains more than 99% cyanoacetic acid solution.
Further, the second refined thermal source of the column overhead vapours as the first treating column reboiler, the second refined column overhead Vapours enters the second treating column return tank being connected with the second refined column overhead after being condensed by the first treating column reboiler, and second Technique water section in treating column return tank returns to the second treating column, and remaining is gone outside battery limit (BL), and fixed gas is through the cold of vacuum trap Discharged after solidifying through vacuum system.Second refined column overhead heat is steamed to be coupled with the first treating column reboiler, is efficiently utilized The heat of device in itself, the loss of recirculated water is reduced, has reduced energy consumption and reduce discharge, energy-conserving and environment-protective.
Further, it is refined to enter first after the condensation of the first treating column overhead condenser for the first refined column overhead vapours Tower return tank, the technique water section in the first treating column return tank return to the first treating column, and remaining is gone outside battery limit (BL), and fixed gas is through true Discharged after the condensation of empty trap through vacuum system.
Further, desalting processing device is provided with the first dehydrating tower tower reactor and the second dehydrating tower tower reactor at least one, Next stage dehydrating tower is entered back into after desalting processing, salinity is sloughed as far as possible using multiple desalting processing device.
Further, after raw material first passes through the heat exchange of the 3rd dehydration column overhead heat exchanger before being transported to the first dehydrating tower, then Feed preheater by being arranged on the first dehydrating tower tower reactor enters the first dehydrating tower after preheating;The first dehydration column overhead heat Thermal source of the steam as the second dehydration column reboiler, the second dehydration column overhead vapours is as the 3rd dehydration column reboiler Thermal source.Raw material is heated by the 3rd dehydration column overhead heat exchanger, equally cools the vapours of the 3rd dehydration column overhead, the first dehydration Column overhead vapours is coupled with the second dehydration column reboiler, the second dehydration column overhead vapours and the 3rd dehydration column reboiler Coupled.Such design efficiently utilizes the heat of device in itself, reduces the loss of recirculated water again, and reducing can depletion Few discharge, energy-conserving and environment-protective.
Further, the 3rd dehydration column overhead heat exchanger is connected to the 3rd dehydration column overhead condenser, and the described 3rd is de- Water tower overhead condenser is connected to the 3rd return tank, and the 3rd return tank is connected to the 3rd dehydration column overhead;3rd dehydration column overhead Vapours condenses by the 3rd dehydration column overhead condenser again after the heat exchange of the 3rd dehydration column overhead heat exchanger, the 3rd dehydration Enter the 3rd return tank after the condensation of tower reboiler, technique water section the 3rd dehydrating tower of return in the 3rd return tank, remaining goes to boundary Outside area, fixed gas is discharged after the condensation of vacuum trap through vacuum system.
Further, first dehydration column overhead is provided with the first return tank, the first return tank and the second dehydration column reboiler Connection, for the first dehydration column overhead vapours after the condensation of the second dehydration column reboiler, technique water section returns to the first dehydrating tower, Remaining is gone outside battery limit (BL), and fixed gas is discharged after the condensation of vacuum trap through vacuum system;Second dehydration column overhead is provided with Second return tank, the second return tank are connected with the second dehydration column reboiler, and the second dehydration column overhead vapours is by the 3rd dehydration Enter the second return tank after the condensation of tower reboiler, technique water section the second dehydrating tower of return in the second return tank, remaining goes to boundary Outside area, fixed gas is discharged after the condensation of vacuum trap through vacuum system.
Further, the first dehydrating tower tower reactor liquidus temperature is 102-112 DEG C, and tower top temperature is 96-106 DEG C, tower top Pressure is 80-120kPa;The second dehydrating tower tower reactor liquidus temperature is 89-102 DEG C, and tower top temperature is 81-92 DEG C, tower top pressure Power is 45-60kPa;The 3rd dehydrating tower tower reactor liquidus temperature is 65-83 DEG C, and tower top temperature is 50-65 DEG C, and tower top pressure is 10-18kPa。
Further, the first treating column tower reactor liquidus temperature is 102-120 DEG C, and tower top temperature is 35-64 DEG C, tower top pressure Power is 6-15kPa.
Further, the first treating column tower reactor liquidus temperature is 48-55 DEG C, and tower top temperature is 35-45 DEG C, tower top pressure For 5-10kPa;The second treating column tower reactor liquidus temperature is 95-105 DEG C, and tower top temperature is 58-68 DEG C, and tower top pressure is 15-25kPa。
Above-mentioned reboiler, heating agent can be conduction oil, vapor etc., then the form boiled can be forced circulation, Heat siphon type heating, falling film evaporation or submergence reboiler etc..Desalting processing device includes cooling device, crystallization apparatus and centrifuge Or drying machine etc..
In summary, the invention has the advantages that (1) makes full use of energy, energy consumption is low, for example many places utilize vapours With the coupling of reboiler;The recycling of vapours, with greatly reducing vapours consumption;(2) cyanogen second in the water isolated Acid content is low, is refined using triple effect dehydration and single-action, cyanoacetic acid content can drop to below 500ppm in water;Using triple effect dehydration and Economic benefits and social benefits refine, and cyanoacetic acid content can drop to below 300-400ppm in water;Reduce waste water subsequent treatment expense so that cyanoacetic acid damages Lose small;(3) cyanoacetic acid high income, 95%-99.5% can be reached.
Brief description of the drawings
Fig. 1 is the structural representation of the embodiment of the present invention;
Fig. 2 is the structural representation of the embodiment of the present invention.
Wherein, the 1, first dehydrating tower;2nd, the second dehydrating tower;3rd, the 3rd dehydrating tower;4th, the first treating column;5th, second is refined Tower;6th, feed preheater;7th, the first dehydration column reboiler;8th, the second dehydration column reboiler;9th, the 3rd dehydration column reboiler;10、 First treating column reboiler;11st, the second treating column reboiler;12nd, the first return tank;13rd, the second return tank;14th, the 3rd backflow Tank;15th, the first treating column return tank;16th, the second treating column return tank;17th, the 3rd dehydration column overhead heat exchanger;18th, the 3rd is de- Water tower overhead condenser;19th, the first treating column overhead condenser;20th, vacuum trap;21st, desalting processing device;22nd, mother liquor Surge tank.
Embodiment
The principle and feature of the present invention are described below in conjunction with accompanying drawing, the given examples are served only to explain the present invention, and It is non-to be used to limit the scope of the present invention.
The method that the present invention isolates and purifies cyanoacetic acid includes two on the whole, and one is that triple effect dehydration and single-action refine, One is that triple effect dehydration and economic benefits and social benefits refine, and the quantity of the desalter in triple effect dehydration can be according to the salt content in actual raw material It is determined that more preferably select.The applicable raw material of the present invention, which forms, is:Cyanoacetic acid:5%-25%, sodium chloride:10%-35%, remaining as Water.
Embodiment 1
Referring to Fig. 2 structural representation, the isolation and purification method of cyanoacetic acid, triple effect dehydration and single-action refine, and step is as follows:
(1) material treatment process
By mainly contain cyanoacetic acid, NaCl, water raw material from the tower reactor of the first dehydrating tower 1 input, the tower reactor of the first dehydrating tower 1 Material is heated by the first dehydration column reboiler 7, and steam rises to the tower top of the first dehydrating tower 1, stays in the thing of the tower reactor of the first dehydrating tower 1 Material is delivered to the second dehydrating tower 2;The tower top vapours of first dehydrating tower 1 heats second as the thermal source of the second dehydration column reboiler 8 The kettle material of dehydrating tower 2, steam rise to the tower top of the second dehydrating tower 2, and the material for staying in the tower reactor of the second dehydrating tower 2 is delivered to the 3rd Dehydrating tower 3, the tower top vapours of the second dehydrating tower 2 heat the tower reactor thing of the 3rd dehydrating tower 3 as the thermal source of the 3rd dehydration column reboiler 9 Material, steam rises to the tower top of the 3rd dehydrating tower 3, and the material for staying in the tower reactor of the 3rd dehydrating tower 3 is carried out after desalting processing from the first essence The middle part of tower 4 processed enters.
The tower top of first dehydrating tower 4 is provided with the first return tank 12, and the first return tank 12 is connected with the second dehydration column reboiler 8, The tower top vapours of first dehydrating tower 1 is after the condensation of the second dehydration column reboiler 8, and process water is gone outside battery limit (BL), and fixed gas is through vacuum Discharged after the condensation of trap 20 through vacuum system;The tower top of second dehydrating tower 2 is provided with the second return tank 13, the second return tank 13 with Second dehydration column reboiler 8 connects, and the tower top vapours of the second dehydrating tower 2 enters the after the condensation of the 3rd dehydration column reboiler 9 Two return tanks 13, the process water in the second return tank 13 are gone outside battery limit (BL), and fixed gas is after the condensation of vacuum trap 20 through vacuum System is discharged.3rd dehydration column overhead heat exchanger 17 is connected to the 3rd dehydration column overhead condenser 18, and the 3rd dehydration column overhead is cold Condenser 18 is connected to the 3rd return tank 14, and the 3rd return tank 14 is connected to the tower top of the 3rd dehydrating tower 3;The tower top of 3rd dehydrating tower 3 heat Steam condenses by the 3rd dehydration column overhead condenser 18 again after the heat exchange of the 3rd dehydration column overhead heat exchanger 17, and the 3rd is de- Water tower reboiler 9 enters the 3rd return tank 14 after condensing, and the process water in the 3rd return tank 14 is gone outside battery limit (BL), and fixed gas is through vacuum Discharged after the condensation of trap 20 through vacuum system.
, can be at the tower reactor of the first dehydrating tower 1 and the tower reactor of the second dehydrating tower 2 at least one according to salt content in practical operation Provided with desalting processing device 21, next stage dehydrating tower is entered back into after desalting processing.
Operating condition in each tower:The tower reactor liquidus temperature of first dehydrating tower 1 is 102-112 DEG C, tower top temperature 96- 106 DEG C, tower top pressure 80-120kPa;The tower reactor liquidus temperature of second dehydrating tower 2 is 89-102 DEG C, tower top temperature 81-92 DEG C, tower top pressure 45-60kPa;The tower reactor liquidus temperature of 3rd dehydrating tower 3 is 65-83 DEG C, and tower top temperature is 50-65 DEG C, tower top Pressure is 10-18kPa.
(2) crude product refining process
The material of the tower reactor of first treating column 4 vaporizes after being heated by the first treating column reboiler 10 to be risen, and steam rises to the The tower top of one treating column 4, the first treating column return tank 15 is entered after the condensation of the first treating column overhead condenser 19, first is refined Process water in tower return tank 15 is gone outside battery limit (BL), and fixed gas is discharged after the condensation of vacuum trap 20 through vacuum system.First The kettle material for the treatment of column 4 is cooled down, desalting processing obtains cyanoacetic acid product.The tower reactor liquidus temperature of first treating column 4 is 102- 120 DEG C, tower top temperature is 35-64 DEG C, tower top pressure 6-15kPa.
As improved energy-saving scheme, raw material can be first after the heat exchange of the 3rd dehydration column overhead heat exchanger 17, then through first The feed preheater 6 of the tower reactor of dehydrating tower 1 enters the first dehydrating tower 1 after preheating.In addition, solution can be with advanced after desalting processing Enter mother liquor surge tank 22 as buffering, enter back into next stage processing unit.As shown in Figure 1.
Above-mentioned reboiler, heating agent can be conduction oil, vapor etc., then the form boiled can be forced circulation, Heat siphon type heating, falling film evaporation or submergence reboiler etc..Desalting processing device includes cooling device, crystallization apparatus and centrifuge Or drying machine etc..
Embodiment 2
As shown in Fig. 2 the isolation and purification method of cyanoacetic acid, triple effect dehydration and economic benefits and social benefits refine, the main difference with embodiment It is in step (2) crude product refining process:
The material of the tower reactor of first treating column 4 vaporizes after being heated by the first treating column reboiler 10 to be risen, and steam rises to the The tower top of one treating column 4, the first treating column return tank 15 is entered after the condensation of the first treating column overhead condenser 19, first is refined Process water in tower return tank 15 is gone outside battery limit (BL), and fixed gas is discharged after the condensation of vacuum trap 20 through vacuum system.First The kettle material for the treatment of column 4 enters the second treating column 5 and carries out the distillation process the same with the process of the first treating column 4, the second treating column 5 Kettle material carries out desalting processing and obtains cyanoacetic acid product.
As improved energy-saving scheme, the first treating column reboiler 10 can be used as using the tower top vapours of the second treating column 5 Thermal source.The tower top vapours of second treating column 5 enters after being condensed by the first treating column reboiler 10 and connected with the tower top of the second treating column 5 The the second treating column return tank 16 connect, the process water in the second treating column return tank 16 are gone outside battery limit (BL), and fixed gas traps through vacuum Discharged after the condensation of device 20 through vacuum system.Referring to Fig. 2.
During economic benefits and social benefits are refined, the tower reactor liquidus temperature of the first treating column 4 is 48-55 DEG C, and tower top temperature is 35-45 DEG C, tower top pressure Power is 5-10kPa;The tower reactor liquidus temperature of second treating column 5 is 95-105 DEG C, and tower top temperature is 58-68 DEG C, tower top pressure 15- 25kPa。
Specifically, carrying out the operation experiments of above-mentioned two embodiment with one group of raw material, parameter is as follows:Raw material forms:Cyanogen second Acid:15.6%, sodium chloride:21.4%, water:63%.Charging rate 100000kg/h.
Obtained test data is operated according to embodiment 1:
Triple effect is dehydrated:The overhead extraction of first dehydrating tower 1:18815kg/h, the reflux ratio 0.03-2.0 of the first dehydrating tower 1;Second The overhead extraction of dehydrating tower 2:18401kg/h, the reflux ratio 0.03-2.5 of the second dehydrating tower 2;The overhead extraction of 3rd dehydrating tower 3: 18814kg/h, the reflux ratio 0.03-3.5 of the 3rd dehydrating tower 3;The tower reactor of 3rd dehydrating tower 3 produces:Cyanoacetic acid 15579kg/h, water 2896kg/h, sodium chloride 2659kg/h.
Single-action refines:The overhead extraction of first treating column 4:6872kg/h, reflux ratio 0.03-3.8;Tower reactor forms cyanoacetic acid: 99.5%, sodium chloride:0.3%, water:0.2-0.3%.
Obtained test data is operated according to embodiment 2:
The parameter of triple effect dehydration is with embodiment 1, during economic benefits and social benefits are refined:The overhead extraction of first treating column 4:3497kg/h, backflow Compare 0.03-2.8;The overhead extraction of second treating column 5:3006kg/h, reflux ratio 0.03-3.8;Tower reactor forms cyanoacetic acid:96.9%, Sodium chloride:1%-2%, water:3.1%.
Presently preferred embodiments of the present invention is these are only, is not intended to limit the invention, it is all in the spirit and principles in the present invention Within, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.

Claims (11)

1. a kind of isolation and purification method of cyanoacetic acid, it is characterised in that including material treatment process and crude product refining process, step It is as follows:
(1) material treatment process
By mainly contain cyanoacetic acid, NaCl, water raw material inputted from the first dehydrating tower tower reactor, the material quilt of the first dehydrating tower tower reactor First dehydration column reboiler heats, and main component rises to the first dehydration column overhead for the steam of water, stays in the first dehydrating tower tower The material of kettle is delivered to the second dehydrating tower, and the material of the second dehydrating tower tower reactor is heated by the second dehydration column reboiler, main component The second dehydration column overhead is risen to for the steam of water, the material for staying in the second dehydrating tower tower reactor is delivered to the 3rd dehydrating tower, and the 3rd The material of dehydrating tower tower reactor is heated by the 3rd dehydration column reboiler, and main component rises to the 3rd dehydrating tower tower for the steam of water Top, enter after staying in the material progress desalting processing of the 3rd dehydrating tower tower reactor from the middle part of the first treating column;
(2) crude product refining process
The material of first treating column tower reactor vaporizes after being heated by the first treating column reboiler to be risen, and main component is on the steam of water The first refined column overhead is raised to, the first treating column kettle material is cooled down, desalting processing obtains cyanoacetic acid product.
2. the isolation and purification method of cyanoacetic acid according to claim 1, it is characterised in that the first treating column kettle material is entered Before row desalting processing, it is introduced into the second treating column and carries out with the same distillation process of the first treating column process, the second treating column tower Kettle material carries out desalting processing and obtains cyanoacetic acid product.
3. the isolation and purification method of cyanoacetic acid according to claim 2, it is characterised in that the second refined column overhead vapours As the thermal source of the first treating column reboiler, the second refined column overhead vapours enter after being condensed by the first treating column reboiler with Second treating column return tank of the second refined column overhead connection, the technique water section in the second treating column return tank return to the second essence Tower processed, remaining is gone outside battery limit (BL), and fixed gas is discharged after the condensation of vacuum trap through vacuum system.
4. the isolation and purification method of the cyanoacetic acid according to claim 1,2 or 3, it is characterised in that the first refined column overhead Vapours enters the first treating column return tank after the condensation of the first treating column overhead condenser, in the first treating column return tank Technique water section returns to the first treating column, and remaining is gone outside battery limit (BL), and fixed gas is arranged after the condensation of vacuum trap through vacuum system Go out.
5. the isolation and purification method of cyanoacetic acid according to claim 1, it is characterised in that in the first dehydrating tower tower reactor With desalting processing device is provided with the second dehydrating tower tower reactor at least one, next stage dehydrating tower is entered back into after desalting processing.
6. the isolation and purification method of cyanoacetic acid according to claim 1, it is characterised in that raw material is transported to the first dehydration After the heat exchange of the 3rd dehydration column overhead heat exchanger is first passed through before tower, then by being arranged on the feed preheater of the first dehydrating tower tower reactor Enter the first dehydrating tower after preheating;Thermal source of the first dehydration column overhead vapours as the second dehydration column reboiler, it is described Thermal source of the second dehydration column overhead vapours as the 3rd dehydration column reboiler.
7. the isolation and purification method of cyanoacetic acid according to claim 6, it is characterised in that the 3rd dehydration column overhead is changed Hot device is connected to the 3rd dehydration column overhead condenser, and the 3rd dehydration column overhead condenser is connected to the 3rd return tank, and the 3rd Return tank is connected to the 3rd dehydration column overhead;3rd dehydration column overhead vapours exchanges heat by the 3rd dehydration column overhead heat exchanger Afterwards, condensed again by the 3rd dehydration column overhead condenser, enter the 3rd return tank after the condensation of the 3rd dehydration column reboiler, the 3rd time The technique water section flowed in tank returns to the 3rd dehydrating tower, and remaining is gone outside battery limit (BL), and fixed gas is after the condensation of vacuum trap through true Empty set system discharge.
8. the isolation and purification method of the cyanoacetic acid according to claim 1 or 6, it is characterised in that the first dehydrating tower tower Top is provided with the first return tank, and the first return tank is connected with the second dehydration column reboiler, and the first dehydration column overhead vapours passes through the After the condensation of two dehydration column reboilers, technique water section returns to the first dehydrating tower, and remaining is gone outside battery limit (BL), and fixed gas is through vacuum trap Condensation after discharged through vacuum system;Second dehydration column overhead is provided with the second return tank, the second return tank and the second dehydration Tower reboiler connects, and the second dehydration column overhead vapours enters the second return tank after the condensation of the 3rd dehydration column reboiler, the Technique water section in two return tanks returns to the second dehydrating tower, and remaining is gone outside battery limit (BL), and fixed gas is after the condensation of vacuum trap Discharged through vacuum system.
9. the isolation and purification method of the cyanoacetic acid according to claim 1 or 6, it is characterised in that the first dehydrating tower tower Kettle liquidus temperature is 102-112 DEG C, and tower top temperature is 96-106 DEG C, tower top pressure 80-120kPa;The second dehydrating tower tower Kettle liquidus temperature is 89-102 DEG C, and tower top temperature is 81-92 DEG C, tower top pressure 45-60kPa;The 3rd dehydrating tower tower reactor Liquidus temperature is 65-83 DEG C, and tower top temperature is 50-65 DEG C, tower top pressure 10-18kPa.
10. the isolation and purification method of cyanoacetic acid according to claim 1, it is characterised in that the first treating column tower reactor Liquidus temperature is 102-120 DEG C, and tower top temperature is 35-64 DEG C, tower top pressure 6-15kPa.
11. the isolation and purification method of cyanoacetic acid according to claim 4, it is characterised in that the first treating column tower reactor Liquidus temperature is 48-55 DEG C, and tower top temperature is 35-45 DEG C, tower top pressure 5-10kPa;The second treating column tower reactor liquid phase Temperature is 95-105 DEG C, and tower top temperature is 58-68 DEG C, tower top pressure 15-25kPa.
CN201711033865.8A 2017-10-30 2017-10-30 A kind of isolation and purification method of cyanoacetic acid Pending CN107793329A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102336685A (en) * 2011-09-17 2012-02-01 潍坊柏立化学有限公司 Method for preparing cyanoacetic acid through continuous dehydration
US20150045594A1 (en) * 2013-08-09 2015-02-12 WB Technologies LLC Integrated ethanol and renewable diesel facility
CN105481717A (en) * 2015-11-20 2016-04-13 重庆紫光化工股份有限公司 Preparation method for cyanoacetic acid and derivatives thereof
CN105968028A (en) * 2016-05-06 2016-09-28 新乡瑞诚科技股份有限公司 Acetonitrile continuous negative pressure distillation extraction technology
CN106045879A (en) * 2016-08-15 2016-10-26 国药集团化学试剂有限公司 Preparation method for cyanoacetic acid
CN106349108A (en) * 2016-08-26 2017-01-25 重庆紫光化工股份有限公司 Cyanoacetic acid separation and purification method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102336685A (en) * 2011-09-17 2012-02-01 潍坊柏立化学有限公司 Method for preparing cyanoacetic acid through continuous dehydration
US20150045594A1 (en) * 2013-08-09 2015-02-12 WB Technologies LLC Integrated ethanol and renewable diesel facility
CN105481717A (en) * 2015-11-20 2016-04-13 重庆紫光化工股份有限公司 Preparation method for cyanoacetic acid and derivatives thereof
CN105968028A (en) * 2016-05-06 2016-09-28 新乡瑞诚科技股份有限公司 Acetonitrile continuous negative pressure distillation extraction technology
CN106045879A (en) * 2016-08-15 2016-10-26 国药集团化学试剂有限公司 Preparation method for cyanoacetic acid
CN106349108A (en) * 2016-08-26 2017-01-25 重庆紫光化工股份有限公司 Cyanoacetic acid separation and purification method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
朱平等编著, 山东大学出版社 *

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