CN105884649A - Recycling technology of beta-aminopropionitrile - Google Patents
Recycling technology of beta-aminopropionitrile Download PDFInfo
- Publication number
- CN105884649A CN105884649A CN201610368269.4A CN201610368269A CN105884649A CN 105884649 A CN105884649 A CN 105884649A CN 201610368269 A CN201610368269 A CN 201610368269A CN 105884649 A CN105884649 A CN 105884649A
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- aminopropionitrile
- autoclave
- ammonia
- recovery process
- temperature
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/30—Preparation of carboxylic acid nitriles by reactions not involving the formation of cyano groups
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a recycling technology of beta-aminopropionitrile. A by-product beta in beta-aminopropionitrile production and beta-iminodipropionitrile continue to be recycled and react to generate beta-aminopropionitrile. The adopted recycling technology improves the beta-aminopropionitrile yield to a larger extent, improves recycling of raw materials in liquid waste, lowers liquid waste disposal, lowers the production cost, and reduces environmental influences.
Description
Technical field
The present invention relates to the synthesis technique of a kind of organic compound, especially in regard to the recovery work of a kind of β-aminopropionitrile
Skill.
Background technology
β-aminopropionitrile is a kind of important organic chemical industry's intermediate, and its preparation method more commonly used is to pass through ammonia
Reaction with acrylonitrile generates and prepares.But owing to the amino of β-aminopropionitrile has higher alkalescence compared with ammonia,
Still can produce more by-product with acrylonitrile generation side reaction, not only affect the yield of product, and by-product
Thing also cannot directly recycle, and processes only as harmful influence.
Summary of the invention
It is an object of the invention to provide one and can improve product yield, reduce liquid waste processing, reduce and produce into
The recovery process of this β-aminopropionitrile.
For reaching above-mentioned purpose, the present invention adopts the following technical scheme that the recovery process of a kind of β-aminopropionitrile,
It comprises the following steps that
One, raw material propylene nitrile and ammonia are put in reactor react, generate β-aminopropionitrile, beta-amino
Propionitrile and acrylonitrile reactor generate by-product β, β-iminobis-propanenitrile；
Two, the reaction solution in step one is delivered in there-necked flask, after Distillation recovery β-aminopropionitrile, useless
Liquid is sent in autoclave；
Three, in autoclave, add ammonia, be warming up to after uniform temperature be incubated, allow β, β-iminobis-propanenitrile
A period of time is reacted with ammonia；
Four, after having reacted, the temperature in autoclave is down to room temperature, reclaims the ammonia in autoclave；
Five, by liquids recovery in autoclave to there-necked flask, Distillation recovery β-aminopropionitrile, waste liquid continues to send
To autoclave, carry out reaction together with other waste liquid and reclaim β-aminopropionitrile.
Further, the concentration of the described ammonia in step 3 is 30%～40%.
Further, the described ammonia in step 3 is 4:1～6:1 with the mass ratio of waste liquid in step 2.
Further, described ammonia is 5:1 with the optimum quality ratio of waste liquid.
Further, the temperature in step 3 rises to 120 DEG C～150 DEG C.
Further, in step 3, optimal reaction temperature is 150 DEG C.
Further, in step 3, temperature retention time is 2～3 hours.
Further, in step 3, optimal temperature retention time is 3 hours.
Further, in step 3 when insulation reaction, the Stress control in autoclave is 4～5MPa.
Compared with prior art, recovery process of the present invention improves β-aminopropionitrile to a greater degree
Yield, adds the recycling of raw material in waste liquid, decreases liquid waste processing, reduce production cost,
Decrease the impact on environment.
Detailed description of the invention
For the technology used in the present invention means and the technique effect that reach being expanded on further, below in conjunction with enforcement
The present invention is described in detail by example.
The recovery process of the β-aminopropionitrile that the present invention provides, it comprises the following steps that
One, raw material propylene nitrile and ammonia are put in reactor react, generate β-aminopropionitrile, beta-amino
Propionitrile and acrylonitrile reactor generate by-product β, β-iminobis-propanenitrile；
Two, the reaction solution in step one is delivered in there-necked flask, after Distillation recovery β-aminopropionitrile, useless
Liquid is sent in autoclave；
Three, in autoclave, add ammonia, be warming up to 120 DEG C～150 DEG C, be incubated 2～3 hours, pressure in still
Control 4～5MPa, allow β, β-iminobis-propanenitrile and ammonia react；
Four, after having reacted, the temperature in autoclave is down to room temperature, reclaims the ammonia in autoclave；
Five, by liquids recovery in autoclave to there-necked flask, Distillation recovery β-aminopropionitrile, waste liquid continues to send
To autoclave, carry out reaction together with other waste liquid and reclaim β-aminopropionitrile.
In step 3, the concentration of ammonia is 30%～40%.The quality of the waste liquid in ammonia and step 2 in step 3
Ratio is 4:1～6:1, and its optimum quality ratio is 5:1.In step 3, optimal reaction temperature is 150 DEG C, optimum response
Time is 3 hours.
The reaction equation generating by-product in step one is:
The reaction equation of β-aminopropionitrile of reducing in step 3 is
Embodiment 1
β-aminopropionitrile slops 50g (wherein β, β iminobis-propanenitrile content is added in autoclave
80%), add 35% concentration ammonia 200g, after airtight good autoclave, be warmed up to 120 DEG C, Stress control at 4MPa,
It is incubated 2 hours.After insulation terminates, cool to room temperature, in taking-up reactant liquor to there-necked flask, first reclaim ammonia
Water, redistillation β-aminopropionitrile, distill out aminopropionitrile 42g, an addition yield 61.7%.
Embodiment 2
β-aminopropionitrile slops 50g (wherein β, β iminobis-propanenitrile content is added in autoclave
80%), add 35% concentration ammonia 200g, after airtight good autoclave, be warmed up to 150 DEG C, Stress control at 4MPa,
It is incubated 3 hours.After insulation terminates, cool to room temperature, in taking-up reactant liquor to there-necked flask, first reclaim ammonia
Water, redistillation β-aminopropionitrile, distill out aminopropionitrile 45g, an addition yield 68%.
Embodiment 3
β-aminopropionitrile slops 50g (wherein β, β iminobis-propanenitrile content is added in autoclave
80%), add 35% concentration ammonia 250g, after airtight good autoclave, be warmed up to 120 DEG C, Stress control at 4MPa,
It is incubated 2 hours, after insulation terminates, cools to room temperature, in taking-up reactant liquor to there-necked flask, first reclaim ammonia
Water, redistillation β-aminopropionitrile, distill out aminopropionitrile 46.7g, an addition yield 68.7%.
Embodiment 4
β-aminopropionitrile slops 50g (wherein β, β iminobis-propanenitrile content is added in autoclave
80%), add 35% concentration ammonia 250g, after airtight good autoclave, be warmed up to 150 DEG C, Stress control at 4MPa,
It is incubated 3 hours, after insulation terminates, cools to room temperature, in taking-up reactant liquor to there-necked flask, first reclaim ammonia
Water, redistillation β-aminopropionitrile, distill out aminopropionitrile 47.2g, an addition yield 69.4%.
Embodiment 5
β-aminopropionitrile slops 50g (wherein β, β iminobis-propanenitrile content is added in autoclave
80%), add 35% concentration ammonia 300g, after airtight good autoclave, be warmed up to 120 DEG C, Stress control at 4MPa,
It is incubated 2 hours, after insulation terminates, cools to room temperature, in taking-up reactant liquor to there-necked flask, first reclaim ammonia
Water, redistillation β-aminopropionitrile, distill out aminopropionitrile 42.5g, an addition yield 62.5%.
Embodiment 6
β-aminopropionitrile slops 50g (wherein β, β iminobis-propanenitrile content is added in autoclave
80%), add 35% concentration ammonia 300g, after airtight good autoclave, be warmed up to 150 DEG C, Stress control at 4MPa,
It is incubated 3 hours, after insulation terminates, cools to room temperature, in taking-up reactant liquor to there-necked flask, first reclaim ammonia
Water, redistillation β-aminopropionitrile, distill out aminopropionitrile 43.7g, an addition yield 64.3%.
Above the present invention has been carried out the most detailed description with certain particularity.General in art
Logical it is to be understood by the skilled artisans that what description in embodiment was merely exemplary, true without departing from the present invention
Make being changed on the premise of real spirit and scope and all should belong to protection scope of the present invention.Institute of the present invention
Claimed scope be defined by described claims rather than above-mentioned by embodiment
Description limits.
Claims (9)
1. the recovery process of a β-aminopropionitrile, it is characterised in that: it comprises the following steps that
One, raw material propylene nitrile and ammonia are put in reactor react, generate β-aminopropionitrile, beta-amino
Propionitrile and acrylonitrile reactor generate by-product β, β-iminobis-propanenitrile；
Two, the reaction solution in step one is delivered in there-necked flask, after Distillation recovery β-aminopropionitrile, useless
Liquid is sent in autoclave；
Three, in autoclave, add ammonia, be warming up to after uniform temperature be incubated, allow β, β-iminobis-propanenitrile
A period of time is reacted with ammonia；
Four, after having reacted, the temperature in autoclave is down to room temperature, reclaims the ammonia in autoclave；
Five, by liquids recovery in autoclave to there-necked flask, Distillation recovery β-aminopropionitrile, waste liquid continues to send
To autoclave, carry out reaction together with other waste liquid again and reclaim β-aminopropionitrile.
The recovery process of β-aminopropionitrile the most according to claim 1, it is characterised in that: in step 3
The concentration of described ammonia is 30%～40%.
The recovery process of β-aminopropionitrile the most according to claim 1, it is characterised in that: in step 3
Described ammonia is 4:1～6:1 with the mass ratio of waste liquid in step 2.
The recovery process of β-aminopropionitrile the most according to claim 3, it is characterised in that: described ammonia with
The optimum quality ratio of waste liquid is 5:1.
The recovery process of β-aminopropionitrile the most according to claim 1, it is characterised in that: in step 3
Temperature rises to 120 DEG C～150 DEG C.
The recovery process of β-aminopropionitrile the most according to claim 5, it is characterised in that: in step 3
Good reaction temperature is 150 DEG C.
The recovery process of β-aminopropionitrile the most according to claim 1, it is characterised in that: step 3 is protected
The temperature time is 2～3 hours.
The recovery process of β-aminopropionitrile the most according to claim 7, it is characterised in that: in step 3
Good temperature retention time is 3 hours.
The recovery process of β-aminopropionitrile the most according to claim 1, it is characterised in that: in step 3
During insulation reaction, the Stress control in autoclave is 4～5MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610368269.4A CN105884649A (en) | 2016-05-27 | 2016-05-27 | Recycling technology of beta-aminopropionitrile |
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| CN201610368269.4A CN105884649A (en) | 2016-05-27 | 2016-05-27 | Recycling technology of beta-aminopropionitrile |
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| CN201610368269.4A Pending CN105884649A (en) | 2016-05-27 | 2016-05-27 | Recycling technology of beta-aminopropionitrile |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107473986A (en) * | 2017-08-07 | 2017-12-15 | 杭州鑫富科技有限公司 | A kind of β aminopropionitriles recovery method |
| CN109438283A (en) * | 2018-12-25 | 2019-03-08 | 江苏兄弟维生素有限公司 | A kind of synthetic method and device of β-aminopropionitrile |
| CN112679382A (en) * | 2020-12-26 | 2021-04-20 | 杭州鑫富科技有限公司 | Method for preparing 3-aminopropionitrile from waste liquid containing 3, 3-iminodipropionitrile |
| CN112830883A (en) * | 2020-12-31 | 2021-05-25 | 江苏兄弟维生素有限公司 | Method for recycling beta, beta-iminodipropionitrile and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3914280A (en) * | 1973-07-30 | 1975-10-21 | Daiichi Seiyaku Co | Process for producing {62 -aminopropionitrile |
| EP0391349A2 (en) * | 1989-04-07 | 1990-10-10 | Air Products And Chemicals, Inc. | Coproduction of propanediamine and alkylated aminopropylamines |
| JPH04110626A (en) * | 1990-08-30 | 1992-04-13 | Nippon Seiko Kk | Torque sensor |
| CN101397266A (en) * | 2008-10-30 | 2009-04-01 | 浙江大学 | Synthetic method of 3-aminopropionitrile and reaction-rectification coupling apparatus used therefor |
-
2016
- 2016-05-27 CN CN201610368269.4A patent/CN105884649A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3914280A (en) * | 1973-07-30 | 1975-10-21 | Daiichi Seiyaku Co | Process for producing {62 -aminopropionitrile |
| EP0391349A2 (en) * | 1989-04-07 | 1990-10-10 | Air Products And Chemicals, Inc. | Coproduction of propanediamine and alkylated aminopropylamines |
| JPH04110626A (en) * | 1990-08-30 | 1992-04-13 | Nippon Seiko Kk | Torque sensor |
| CN101397266A (en) * | 2008-10-30 | 2009-04-01 | 浙江大学 | Synthetic method of 3-aminopropionitrile and reaction-rectification coupling apparatus used therefor |
Non-Patent Citations (1)
| Title |
|---|
| MUROHASHI, SUSUMU: "Amination of acrylonitrile in liquid ammonia", 《NAGAOKA KOGYO TANKI DAIGAKU KOTO SEMMON GAKKO KENKYU KIYO》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107473986A (en) * | 2017-08-07 | 2017-12-15 | 杭州鑫富科技有限公司 | A kind of β aminopropionitriles recovery method |
| CN107473986B (en) * | 2017-08-07 | 2019-09-10 | 杭州鑫富科技有限公司 | A kind of β-aminopropionitrile recovery method |
| CN109438283A (en) * | 2018-12-25 | 2019-03-08 | 江苏兄弟维生素有限公司 | A kind of synthetic method and device of β-aminopropionitrile |
| CN109438283B (en) * | 2018-12-25 | 2021-08-20 | 江苏兄弟维生素有限公司 | Synthesis method and device of beta-aminopropionitrile |
| CN112679382A (en) * | 2020-12-26 | 2021-04-20 | 杭州鑫富科技有限公司 | Method for preparing 3-aminopropionitrile from waste liquid containing 3, 3-iminodipropionitrile |
| CN112830883A (en) * | 2020-12-31 | 2021-05-25 | 江苏兄弟维生素有限公司 | Method for recycling beta, beta-iminodipropionitrile and application |
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Application publication date: 20160824 |