CN110003048A - A kind of method that reactive distillation prepares high purity butylene dintrile - Google Patents
A kind of method that reactive distillation prepares high purity butylene dintrile Download PDFInfo
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- CN110003048A CN110003048A CN201910303597.XA CN201910303597A CN110003048A CN 110003048 A CN110003048 A CN 110003048A CN 201910303597 A CN201910303597 A CN 201910303597A CN 110003048 A CN110003048 A CN 110003048A
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- reactive distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/08—Preparation of carboxylic acid nitriles by addition of hydrogen cyanide or salts thereof to unsaturated compounds
- C07C253/10—Preparation of carboxylic acid nitriles by addition of hydrogen cyanide or salts thereof to unsaturated compounds to compounds containing carbon-to-carbon double bonds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
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- 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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of methods that reactive distillation prepares high purity butylene dintrile, using reaction and rectification device, its structure includes: reactive distillation kettle, the top efferent duct in reactive distillation kettle top portion is connect with condenser, condenser is connect with storage tank, return pipe on storage tank is connected to the intermediate region of reactive distillation kettle, and the bottom nozzles in reactive distillation bottom portion are connected with reboiler；Use acrylonitrile, hydrogen cyanide, triethylamine for reaction raw materials, temperature control is at 50 DEG C ~ 70 DEG C, and acrylonitrile and triethylamine are fed from the upper end of reactive distillation kettle, and hydrogen cyanide is fed from the lower end of reactive distillation kettle；Reactive distillation bottom portion is sampled, when the mass fraction that detection obtains the succinonitrile after deduction solvent is more than 97%, stops reaction, the material in reactive distillation bottom portion is discharged into reboiler, solvent is evaporated off and obtains target product succinonitrile.The invention has the advantages that reaction, rectifying are integrated in one, reaction efficiency is high, and selectivity is good.
Description
Technical field
The present invention relates to the technical fields of succinonitrile preparation.
Background technique
Succinonitrile has anti-inflatable, improves electrochemical stability perforation, changes as first generation lithium battery electrolytes additive
The advantages that kind cycle performance of battery.The purity of succinonitrile is affected to the performance of lithium ion battery.Currently, succinonitrile all uses
The production technology separated afterwards is first reacted, this process route energy consumption is high, equipment investment is big, yield is low, product purity is low, and purity is logical
Often it is lower than 85%, later separation is difficult, and separation requirement is high.
Summary of the invention
The object of the present invention is to provide a kind of method that reactive distillation prepares high purity butylene dintrile, high conversion rates, selection
Property is good, with high purity.
To achieve the above object, the technical solution adopted by the present invention is that: a kind of reactive distillation prepares high purity butylene dintrile
Method, using reaction and rectification device, structure includes: reactive distillation kettle, the top setting top efferent duct of reactive distillation kettle, top
Portion's efferent duct is connected with the input terminal of condenser, and the output end of condenser is connect with storage tank, and return pipe is provided on storage tank, returns
Flow tube is connected to the intermediate region of reactive distillation kettle, and the bottom of reactive distillation kettle is provided with the bottom nozzles with outlet valve, bottom
Adapter tube is connected with reboiler；Use acrylonitrile, hydrogen cyanide, triethylamine for reaction raw materials, reaction temperature is controlled 50 DEG C ~ 70
DEG C, wherein acrylonitrile and triethylamine are fed from the upper end of reactive distillation kettle, and hydrogen cyanide uses the form of organic solution from reaction
The lower end of rectifying still is fed；In reaction process, the top material in reactive distillation kettle is constantly from top efferent duct successively through cold
Condenser, storage tank, return pipe enter to the intermediate region in reactive distillation kettle, and reflux ratio is controlled in 1:1；To reactive distillation bottom portion
It is sampled, when the mass fraction of the succinonitrile after sample detection obtains deduction solvent is more than 97%, stops reaction, open bottom
Discharge valve on portion's adapter tube, so that the material in reactive distillation bottom portion is discharged by bottom nozzles into reboiler, material exists
Solvent is evaporated off in reboiler and obtains target product succinonitrile.
Further, the method that a kind of reactive distillation above-mentioned prepares high purity butylene dintrile, wherein the hydrogen cyanide with
The form of hydrogen cyanide toluene solution feeds intake, and the volume ratio of hydrogen cyanide and toluene is 1:1 in hydrogen cyanide toluene solution.
Further, the method that a kind of reactive distillation above-mentioned prepares high purity butylene dintrile, wherein hydrogen cyanide toluene is molten
In 60L/h ~ 80L/h, being passed through the time is 6h ~ 9h for flow control when liquid feeds intake.
Further, the method that a kind of reactive distillation above-mentioned prepares high purity butylene dintrile, wherein triethylamine mole is
The 0.1% ~ 0.5% of hydrogen cyanide mole.
Further, the method that a kind of reactive distillation above-mentioned prepares high purity butylene dintrile, wherein the output end of condenser
It is also connected with the exhaust emission tube of hot tail gas dump valve, the exhaust emission tube is connected to lye absorption tower, after reaction,
Tail gas in reactive distillation kettle enters in lye absorption tower after condenser is cooling from exhaust emission tube.
Further, the method that a kind of reactive distillation above-mentioned prepares high purity butylene dintrile, wherein the bottom of reactive distillation kettle
Portion is provided with the agitator arm for stirring material, in reaction process, the revolving speed control of agitator arm 500 r/min ~
800r/min。
Further, the method that a kind of reactive distillation above-mentioned prepares high purity butylene dintrile, wherein be connected on reboiler
Recycling can, the solvent steamed in reboiler are collected in recycling can.
Further, the method that a kind of reactive distillation above-mentioned prepares high purity butylene dintrile, wherein acrylonitrile and hydrogen cyanide
With molar ratio be 1.05 ~ 1.1:1.
The invention has the advantages that reaction, rectifying are integrated in one, raw material propylene nitrile is recycled, so that hydrogen cyanide is completely anti-
It answers, therefore the utilization rate height of raw material, high conversion rate, selectivity are good in the reaction, to reduce waste processing cost indirectly, drops
Low energy consumption, while decreasing cost of investment.
Detailed description of the invention
Fig. 1 is that a kind of reactive distillation of the present invention prepares the reactive distillation dress used in the method for high purity butylene dintrile
The structural schematic diagram set.
Specific embodiment
High purity butylene dintrile is prepared to a kind of reactive distillation below to elaborate.
A kind of method that reactive distillation prepares high purity butylene dintrile, using reaction and rectification device, using acrylonitrile, hydrogen cyanogen
Acid, triethylamine are reaction raw materials.
The reaction and rectification device, structure include: reactive distillation kettle 1, and reactive distillation kettle is collection reaction and rectifying is
The tower reactor of one, the top setting top efferent duct 11 of reactive distillation kettle 1, the input terminal phase of top efferent duct 11 and condenser 2
Connection, the output end of condenser 2 are connect with storage tank 3, return pipe 31 are provided on storage tank 3, return pipe 31 is connected to reactive distillation
The intermediate region of kettle 1, the bottom of reactive distillation kettle 1 are provided with the bottom nozzles 7 with outlet valve 71, bottom nozzles 7 and reboiler 4
It is connected, the top of reboiler 4 is connected with recycling can 6.In order to improve reaction efficiency, the bottom setting of reactive distillation kettle 1 is useful
In the agitator arm 12 of stirring material, reaction process, the revolving speed of agitator arm 12 is controlled in 500 r/min ~ 800r/min.
Simultaneously in order to preferably handle the tail gas in reactive distillation kettle 1 after reaction, the output end of condenser 2 is also connected with hot tail gas
The exhaust emission tube 8 of dump valve 81, the exhaust emission tube 8 are connected to lye absorption tower 7, after reaction, reactive distillation
Tail gas in kettle 1 enters in lye absorption tower 7 after condenser 2 is cooling from exhaust emission tube 8.
Reaction raw materials use acrylonitrile, hydrogen cyanide, triethylamine, reaction temperature control at 50 DEG C ~ 70 DEG C, wherein acrylonitrile and
Triethylamine is fed from the upper end of reactive distillation kettle 1, and the mole of triethylamine is the 0.1% ~ 0.5% of hydrogen cyanide mole.Propylene
Nitrile and hydrogen cyanide and molar ratio be 1.05 ~ 1.1:1.Hydrogen cyanide uses the form of organic solution from the lower end of reactive distillation kettle 1
Portion's charging.Preferably, using hydrogen cyanide toluene solution, wherein the volume ratio of hydrogen cyanide and toluene is 1:1.Hydrogen cyanide toluene solution
In 60L/h ~ 80L/h, being passed through the time is 6h ~ 9h for flow control when feeding intake.
In reaction process, the material of 1 inner top of reactive distillation kettle is constantly from top efferent duct 11 successively through condenser 2, storage
Tank 3, return pipe 31 enter to the intermediate region in reactive distillation kettle 1, and reflux ratio is controlled in 1:1.In reaction process, reactive distillation
The mixture containing acrylonitrile and triethylamine of 1 inner top of kettle enters storage tank 3 through condenser 2, then returns to reaction essence through return pipe 31
The reaction was continued for the intermediate region for evaporating in kettle 1, this can driving a reaction system more effectively forward direction prepares succinonitrile.To reactive distillation kettle
1 bottom is sampled, and when the mass fraction of the succinonitrile after sample detection obtains deduction solvent is more than or equal to 97%, is stopped anti-
It answers, opens the outlet valve 71 on bottom nozzles 7, so that the material of 1 bottom of reactive distillation kettle is discharged by bottom nozzles 7 to boiling again
In device 4.Solvent is evaporated off in reboiler 4 and obtains target product succinonitrile for material, and the solvent steamed in reboiler 4 is collected in recycling
In tank 6, logical be transferred in finished pot 5 of target product succinonitrile is stored.
A kind of method that reactive distillation prepares high purity butylene dintrile of the present invention is done below by specific embodiment
It further illustrates.
Embodiment 1.
By acrylonitrile (281 kg) and triethylamine (0.57 kg) from the upper end of the reactive distillation kettle 1 of 1000L put into
Material, hydrogen cyanide toluene solution (the volume ratio 1:1 of hydrogen cyanide and toluene) are lower end of the 60L/h by reactive distillation kettle 1 with flow
Investment is passed through 6.75h, and three comes into full contact with reaction, and the revolving speed of agitator arm 12 is controlled in 500 r/min ~ 800r/min, instead
Answer temperature 70 C, the mixed material of 1 inner top of reactive distillation kettle constantly from top efferent duct 11 successively through condenser 2, storage tank 3,
Return pipe 31 enters to the intermediate region in reactive distillation kettle 1, and reflux ratio is controlled in 1:1.After reacting 5h, reactive distillation kettle 1
Bottom sample detection, the mass fraction of the succinonitrile after deducting solvent toluene content are 98.1%, stop reaction.By reactive distillation
The bottom succinonitrile and solvent toluene of kettle 1 are collected into reboiler 4.Solvent is evaporated off in reboiler 4, obtains target product succinonitrile 400
Kg(succinonitrile mass fraction is that 98.1%), solvent is collected in recycling can 6, and target product succinonitrile is transferred to storage in finished pot 5
Deposit, further purify finished product 394kg(succinonitrile mass fraction be 99.5%), molar yield: 95.12%.
Embodiment 2
Acrylonitrile (327 kg) and triethylamine (0.69 kg) are put into charging, hydrogen from the upper end of the reactive distillation kettle 1 of 1000L
Cyanic acid toluene solution (the volume ratio 1:1 of hydrogen cyanide and toluene) is that 64L/h is put by the lower end of reactive distillation kettle 1 with flow,
It is passed through 7.4h, three comes into full contact with reaction, and the revolving speed of agitator arm 12 is controlled in 500 r/min ~ 800r/min, reaction temperature
68 DEG C, the material of 1 inner top of reactive distillation kettle constantly from top efferent duct 11 successively through condenser 2, storage tank 3, return pipe 31 into
Enter to the intermediate region in reactive distillation kettle 1, reflux ratio is controlled in 1:1.After reacting 5.5h, the bottom of reactive distillation kettle 1 is sampled
Detection, the mass fraction of the succinonitrile after deducting solvent toluene content are 98.2%, stop reaction.By 1 bottom of reactive distillation kettle
Succinonitrile and solvent toluene are collected into reboiler 4.Solvent is evaporated off in reboiler 4, obtains 464 kg(succinonitrile of target product succinonitrile
Mass fraction be that 98.3%), solvent is collected in recycling can 6, target product succinonitrile is transferred to storage in finished pot 5, into one
Step purify finished product 457kg(succinonitrile mass fraction be 99.6%), molar yield: 94.42%.
Embodiment 3
Acrylonitrile (355 kg) and triethylamine (0.77 kg) are put into charging, hydrogen from the upper end of the reactive distillation kettle 1 of 1000L
Cyanic acid toluene solution (the volume ratio 1:1 of hydrogen cyanide and toluene) is that 70L/h is put by the lower end of reactive distillation kettle 1 with flow,
It is passed through 7.5h, three's haptoreaction, the revolving speed control of agitator arm 12 is in 500 r/min ~ 800r/min, and 67 DEG C of reaction temperature,
The material of 1 inner top of reactive distillation kettle constantly successively enters to instead through condenser 2, storage tank 3, return pipe 31 from top efferent duct 11
The intermediate region in rectifying still 1 is answered, reflux ratio is controlled in 1:1.After reacting 6.5h, the bottom sample detection of reactive distillation kettle 1, button
Except the mass fraction of the succinonitrile after solvent toluene content is 98.0%, stop reaction.By the fourth two of the bottom of reactive distillation kettle 1
Nitrile and solvent toluene are collected into reboiler 4.Solvent is evaporated off in reboiler 4, obtains the matter of 500 kg(succinonitrile of target product succinonitrile
Measuring score is that 98.05%), solvent is collected in recycling can 6, and target product succinonitrile is transferred to storage in finished pot 5.Further
Purify finished product 491kg(succinonitrile mass fraction be 99.7%), molar yield: 94.11%.
Embodiment 4
Acrylonitrile (355 kg) and triethylamine (0.77 kg) are put into charging, hydrogen from the upper end of the reactive distillation kettle 1 of 1000L
Cyanic acid toluene solution (the volume ratio 1:1 of hydrogen cyanide and toluene) is that 75L/h is put by tower bottom with flow, is passed through 7.2h, San Zhechong
Point haptoreaction, the revolving speed control of agitator arm 12 is in 500 r/min ~ 800r/min, and 69 DEG C of reaction temperature, reactive distillation kettle 1
The material of inner top constantly successively enters in reactive distillation kettle 1 through condenser 2, storage tank 3, return pipe 31 from top efferent duct 11
Intermediate region, reflux ratio control in 1:1.After reacting 6h, the bottom sample detection of reactive distillation kettle 1 deducts solvent toluene and contains
The mass fraction of succinonitrile after amount is 98.1%, stops reaction.By the succinonitrile and solvent toluene of the bottom of reactive distillation kettle 1
It collects into reboiler 4.Solvent is evaporated off in reboiler 4, and the mass fraction for obtaining 529 kg(succinonitrile of target product succinonitrile is
98.2%), solvent is collected in recycling can 6, and target product succinonitrile is transferred to storage in finished pot 5, further purifies to obtain finished product
The mass fraction of 521kg(succinonitrile is 99.5%) molar yield: 94.30%.
From the foregoing, it will be observed that the invention has the advantages that the material of 1 inner top of reactive distillation kettle is constantly from top in reaction process
Efferent duct 11 successively enters to the intermediate region in reactive distillation kettle 1, raw material propylene nitrile through condenser 2, storage tank 3, return pipe 31
It being recycled, hydrogen cyanide can react completely, therefore the utilization rate height of raw material, high conversion rate, selectivity are good in the reaction, thus
Connecing reduces waste processing cost, reduces energy consumption, while decreasing cost of investment.
Claims (8)
1. a kind of method that reactive distillation prepares high purity butylene dintrile, it is characterised in that: use reaction and rectification device, structure packet
Include: reactive distillation kettle, the top setting top efferent duct of reactive distillation kettle, top efferent duct are connected with the input terminal of condenser
It connects, the output end of condenser is connect with storage tank, and return pipe is provided on storage tank, and return pipe is connected to the middle area of reactive distillation kettle
Domain, the bottom of reactive distillation kettle are provided with the bottom nozzles with outlet valve, and bottom nozzles are connected with reboiler；Using propylene
Nitrile, hydrogen cyanide, triethylamine are reaction raw materials, and reaction temperature is controlled at 50 DEG C ~ 70 DEG C, and wherein acrylonitrile and triethylamine are smart from reaction
The upper end charging of kettle is evaporated, hydrogen cyanide is fed using the form of organic solution from the lower end of reactive distillation kettle；In reaction process,
Top material in reactive distillation kettle constantly successively enters to reactive distillation through condenser, storage tank, return pipe from top efferent duct
Intermediate region in kettle, reflux ratio are controlled in 1:1；Reactive distillation bottom portion is sampled, when sample detection obtain deducting it is molten
When the mass fraction of succinonitrile after agent is more than 97%, stop reaction, open the discharge valve on bottom nozzles, so that reaction essence
The material for evaporating bottom portion is discharged by bottom nozzles into reboiler, and solvent is evaporated off in reboiler and obtains target product fourth two for material
Nitrile.
2. the method that a kind of reactive distillation according to claim 1 prepares high purity butylene dintrile, it is characterised in that: described
Hydrogen cyanide is fed intake in the form of hydrogen cyanide toluene solution, and the volume ratio of hydrogen cyanide and toluene is 1 in hydrogen cyanide toluene solution:
1。
3. the method that a kind of reactive distillation according to claim 2 prepares high purity butylene dintrile, it is characterised in that: hydrogen cyanide
In 60L/h ~ 80L/h, being passed through the time is 6h ~ 9h for flow control when toluene solution feeds intake.
4. the method that a kind of reactive distillation according to claim 1 prepares high purity butylene dintrile, it is characterised in that: triethylamine
Mole is the 0.1% ~ 0.5% of hydrogen cyanide mole.
5. the method that a kind of reactive distillation according to claim 1 prepares high purity butylene dintrile, it is characterised in that: condenser
Output end be also connected with the exhaust emission tube of hot tail gas dump valve, the exhaust emission tube is connected to lye absorption tower, instead
After answering, the tail gas in reactive distillation kettle is entered in lye absorption tower after condenser is cooling from exhaust emission tube.
6. the method that a kind of reactive distillation according to claim 1 prepares high purity butylene dintrile, it is characterised in that: reaction essence
The bottom for evaporating kettle is provided with agitator arm for stirring material, and in reaction process, the revolving speed of agitator arm is controlled in 500 r/
min ~800r/min。
7. the method that a kind of reactive distillation according to claim 1 prepares high purity butylene dintrile, it is characterised in that: reboiler
On be connected with recycling can, the solvent steamed in reboiler is collected in recycling can.
8. the method that a kind of reactive distillation according to claim 1 prepares high purity butylene dintrile, it is characterised in that: acrylonitrile
With hydrogen cyanide and molar ratio be 1.05 ~ 1.1:1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910303597.XA CN110003048A (en) | 2019-04-16 | 2019-04-16 | A kind of method that reactive distillation prepares high purity butylene dintrile |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910303597.XA CN110003048A (en) | 2019-04-16 | 2019-04-16 | A kind of method that reactive distillation prepares high purity butylene dintrile |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2842584A (en) * | 1956-12-11 | 1958-07-08 | Carbogen Corp | Production of succinonitrile |
| CN103521158A (en) * | 2013-10-29 | 2014-01-22 | 万华化学集团股份有限公司 | Method for continuously preparing butanedinitrile |
-
2019
- 2019-04-16 CN CN201910303597.XA patent/CN110003048A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2842584A (en) * | 1956-12-11 | 1958-07-08 | Carbogen Corp | Production of succinonitrile |
| CN103521158A (en) * | 2013-10-29 | 2014-01-22 | 万华化学集团股份有限公司 | Method for continuously preparing butanedinitrile |
Non-Patent Citations (2)
| Title |
|---|
| 王文强: "丁二腈制备与提纯工艺的研究", 《青岛科技大学硕士学位论文》 * |
| 王文强等: "高纯丁二腈制备方法的研究现状", 《化工科技》 * |
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