CN108821980A - The rectification process of one kind 2,6- diethylaniline - Google Patents
The rectification process of one kind 2,6- diethylaniline Download PDFInfo
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- CN108821980A CN108821980A CN201811016945.7A CN201811016945A CN108821980A CN 108821980 A CN108821980 A CN 108821980A CN 201811016945 A CN201811016945 A CN 201811016945A CN 108821980 A CN108821980 A CN 108821980A
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- diethylaniline
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/68—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/84—Purification
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Abstract
The invention discloses the rectification process of one kind 2,6- diethylaniline, include the following steps：S1：Raw material preparation：Aniline is alkylated with catalyst and ethylene and is reacted, the reactant based on 2,6- diethylaniline, S2 are obtained：Distillation：Reactant described in S1 is injected into distillation equipment and carries out distillation processing, the thick finished product of 2,6- diethylaniline, S3 is made through distilling：Filtering：Thick finished product described in S2 is injected into large trough and is filtered, and filtered 2,6- diethylaniline material is collected, waste liquid remaining after filtering is recycled, S4：Heating separation：Filtered 2,6- diethylaniline material described in S3 is imported into feed pump.The present invention reduces impurity content by the separation rectifying to 2,6- diethylaniline, improves the quality of 2,6- diethylaniline, and convenient for recycling to the product after separation, avoids the waste of resource, reduce waste discharge.
Description
Technical field
The present invention relates to 2,6- diethylaniline technical field of rectification, more particularly to the rectifying of one kind 2,6- diethylaniline
Technique.
Background technique
2,6- diethylanilines, molecular formula：C10H15N 3-4 DEG C of fusing point, boils to be faint yellow to red, transparent oily liquids
243 DEG C of point, relative molecular weight 149.23 is slightly dissolved in water, is soluble in the organic solvents such as ethyl alcohol, ether, and 2,6- diethylanilines are
One of most important amine substance, the product are important organic synthesis intermediate, for manufacturing dyestuff, medicine, fragrance and pesticide,
Itself can replace lead tetraethide to make gasoline anti-knock agent, be also important pesticide, dyestuff and medicine intermediate, be amide-type herbiciding
The raw material of agent alachlor and butachlor, 2,6- diethylanilines need to carry out after producing rectification process, remove 2,6-
Impurity in diethylaniline improves purity, and through retrieving, the patent document of publication number CN1903832A discloses a kind of 3-
The preparation method of chloro-2,6-diethyl aniline, includes the following steps：Metal or its salt heat instead in aniline or alkyl benzene amine
Aniline or alkyl benzene amine metal complex catalyst should be generated, m-chloroaniline is added in obtained complex compound catalyst,
150 DEG C~400 DEG C, ethylene is passed through under the conditions of 10MPa~25MPa, aniline or alkyl benzene amine metal complex catalyst generate second
Base complex compound, m-chloroaniline displaces 3- chloro-2,6-diethyl aniline from ethylization complex compound, and urges complex compound
Agent is regenerated, and such ethylization/displacement reaction cycle carries out.Add water in the product reacted to ethylization/displacement, and
Heating hydrolysis, generates aniline or alkyl benzene amine, ethylating aniline or alkyl benzene amine and 3- chloro-2,6-diethyl aniline.It will
Organic phase after hydrolysate separation carries out rectification under vacuum, isolated 3- chloro-2,6-diethyl aniline.
But this method is not easy to carry out rectification process to 2,6- diethylaniline, causes miscellaneous in 2,6- diethylaniline
Matter is more, quality is reduced, therefore we have proposed the rectification process of one kind 2,6- diethylaniline, for solving above-mentioned ask
Topic.
Summary of the invention
Technical problems based on background technology, the invention proposes the rectification process of one kind 2,6- diethylaniline.
A kind of rectification process of 2,6- diethylaniline proposed by the present invention, includes the following steps：
S1：Raw material preparation：Aniline is alkylated with catalyst and ethylene and is reacted, is obtained based on 2,6- diethylaniline
Reactant；
S2：Distillation：Reactant described in S1 is injected into distillation equipment and carries out distillation processing, 2,6- diethyl is made through distilling
The thick finished product of base aniline；
S3：Filtering：Thick finished product described in S2 is injected into large trough and is filtered, and to filtered 2,6- diethylaniline
Material is collected, and is recycled to waste liquid remaining after filtering；
S4：Heating separation：Filtered 2,6- diethylaniline material described in S3 is imported into feed pump, then passes through preheating
Device is preheated, and 2, the 6- diethylaniline material after preheating is imported into lightness-removing column, is separated；
S5：Separation product processing：After the mask work described in the S4, by 2, the 6- diethylaniline object of lightness-removing column tower top
Material imported into pan tank, and lightness-removing column kettle material is squeezed into weight-removing column through pump, and lightness-removing column kettle material, will after weight-removing column separates
Weight-removing column tower top material imported into pan tank, and weight-removing column kettle material squeezes into heavy constituent slot through pump；
S6：The processing of weight-removing column material：Material in heavy constituent slot described in S5 is sucked in recovery tower by vacuum pump, is carried out
The material for recycling column overhead after material is separated by recovery tower, is imported into pan tank, the material of recovery tower tower reactor imports by separation
Tar slot, is recycled；
S7：Rectifying：2,6- diethylaniline material in pan tank described in S5 and S6 is put into rectifying device and carries out essence
Processing is evaporated, the rectifying to 2,6- diethylaniline can be completed；
S8：Storage：2,6- diethylaniline after rectifying described in S7 is put into container and is stored.
Preferably, in the S1, aniline be alkylated with catalyst and ethylene react should 320 DEG C of high temperature, high pressure≤
It is carried out under conditions of 6.0Mpa.
Preferably, in the S2, distillation equipment is destilling tower, and reactant is imported in destilling tower, and heating makes reactant vapour
Change, then make the reactant liquefaction of gasification, removes impurity therein.
Preferably, in the S3, when being filtered to thick finished product, the thick finished product of 2,6- diethylaniline is being imported into large trough
During, the thick finished product of 2,6- diethylanilines can first pass through the filter screen in large trough, again to 2,6- diethylaniline slightly at
Impurity in product is filtered, and the impurity being obtained by filtration is imported into garbage collection bucket, is recycled.
Preferably, in the S4, after filtered 2,6- diethylaniline material enters lightness-removing column, by lightness-removing column
Reboiler material is heated so that light component material from tower top be discharged, into overhead condenser condense.
Preferably, in the S5, when lightness-removing column kettle material enters in weight-removing column, weight-removing column can be taken off in material
Extra heavy constituent recycles remaining material.
Preferably, in the S7, rectifying device is rectifying column, is had not using each component in 2,6- diethylaniline material
With volatility, i.e. this different property of the vapour pressure of each component at the same temperature makes the light component in liquid phase be transferred to gas
Xiang Zhong, and the heavy constituent in gas phase is transferred in liquid phase, carries out rectifying separation to 2,6- diethylaniline material.
Preferably, in the S8, when being stored to 2,6- diethylaniline, 2,6- diethylaniline is put into container
It is interior, it is sealed processing, is avoided and skin contact, heat, flame, Mars and other ignition sources is avoided, avoids contact with incompatible object
Matter.
Beneficial effects of the present invention：By the separation rectifying to 2,6- diethylaniline, impurity content is reduced, is improved
The quality of 2,6- diethylanilines, and convenient for being recycled to the product after separation, the waste of resource is avoided, is reduced
Waste discharge.
Specific embodiment
Combined with specific embodiments below the present invention is made further to explain.
Embodiment
The rectification process of one kind 2,6- diethylaniline is proposed in the present embodiment, is included the following steps：
S1：Raw material preparation：Aniline is alkylated with catalyst and ethylene and is reacted, is obtained based on 2,6- diethylaniline
Reactant；
S2：Distillation：Reactant described in S1 is injected into distillation equipment and carries out distillation processing, 2,6- diethyl is made through distilling
The thick finished product of base aniline；
S3：Filtering：Thick finished product described in S2 is injected into large trough and is filtered, and to filtered 2,6- diethylaniline
Material is collected, and is recycled to waste liquid remaining after filtering；
S4：Heating separation：Filtered 2,6- diethylaniline material described in S3 is imported into feed pump, then passes through preheating
Device is preheated, and 2, the 6- diethylaniline material after preheating is imported into lightness-removing column, is separated；
S5：Separation product processing：After the mask work described in the S4, by 2, the 6- diethylaniline object of lightness-removing column tower top
Material imported into pan tank, and lightness-removing column kettle material is squeezed into weight-removing column through pump, and lightness-removing column kettle material, will after weight-removing column separates
Weight-removing column tower top material imported into pan tank, and weight-removing column kettle material squeezes into heavy constituent slot through pump；
S6：The processing of weight-removing column material：Material in heavy constituent slot described in S5 is sucked in recovery tower by vacuum pump, is carried out
The material for recycling column overhead after material is separated by recovery tower, is imported into pan tank, the material of recovery tower tower reactor imports by separation
Tar slot, is recycled；
S7：Rectifying：2,6- diethylaniline material in pan tank described in S5 and S6 is put into rectifying device and carries out essence
Processing is evaporated, the rectifying to 2,6- diethylaniline can be completed；
S8：Storage：2,6- diethylaniline after rectifying described in S7 is put into container and is stored, of the invention is beneficial
Effect is to reduce impurity content by the separation rectifying to 2,6- diethylaniline, improve the matter of 2,6- diethylaniline
Amount, and convenient for being recycled to the product after separation, the waste of resource is avoided, waste discharge is reduced.
In the present embodiment, in S1, aniline be alkylated with catalyst and ethylene react should 320 DEG C of high temperature, high pressure≤
It is carried out under conditions of 6.0Mpa, in S2, distillation equipment is destilling tower, and reactant is imported in destilling tower, and heating makes reactant vapour
Change, then make the reactant liquefaction of gasification, remove impurity therein, in S3, when being filtered to thick finished product, by 2,6- diethyl
During the thick finished product of base aniline imports large trough, the thick finished product of 2,6- diethylanilines can first pass through the filter screen in large trough, again
Impurity in the thick finished product of 2,6- diethylaniline is filtered, the impurity being obtained by filtration is imported into garbage collection bucket, into
Row is recycled, and in S4, after filtered 2,6- diethylaniline material enters lightness-removing column, passes through the reboiler in lightness-removing column
Material is heated, so that light component material is discharged from tower top, is condensed into overhead condenser, in S5, when lightness-removing column tower reactor
When material is entered in weight-removing column, weight-removing column can take off the extra heavy constituent in material, and remaining material is recycled,
In S7, rectifying device is rectifying column, has different volatility using each component in 2,6- diethylaniline material, i.e., same
At a temperature of each component this different property of vapour pressure, be transferred to the light component in liquid phase in gas phase, and the recombination in gas phase
It point is transferred in liquid phase, rectifying separation is carried out to 2,6- diethylaniline material, in S8, is deposited to 2,6- diethylaniline
Chu Shi puts 2,6- diethylaniline in container into, is sealed processing, avoids and skin contact, avoids heat, flame, Mars
With other ignition sources, incompatible substance is avoided contact with, the beneficial effects of the invention are as follows pass through the separation to 2,6- diethylaniline
Rectifying reduces impurity content, improves the quality of 2,6- diethylaniline, and convenient for carrying out circulation benefit to the product after separation
With avoiding the waste of resource, reduce waste discharge.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. one kind 2, the rectification process of 6- diethylaniline, which is characterized in that include the following steps：
S1：Raw material preparation：Aniline is alkylated with catalyst and ethylene and is reacted, is obtained based on 2,6- diethylaniline
Reactant；
S2：Distillation：Reactant described in S1 is injected into distillation equipment and carries out distillation processing, 2,6- diethyl is made through distilling
The thick finished product of base aniline；
S3：Filtering：Thick finished product described in S2 is injected into large trough and is filtered, and to filtered 2,6- diethylaniline
Material is collected, and is recycled to waste liquid remaining after filtering；
S4：Heating separation：Filtered 2,6- diethylaniline material described in S3 is imported into feed pump, then passes through preheating
Device is preheated, and 2, the 6- diethylaniline material after preheating is imported into lightness-removing column, is separated；
S5：Separation product processing：After the mask work described in the S4, by 2, the 6- diethylaniline object of lightness-removing column tower top
Material imported into pan tank, and lightness-removing column kettle material is squeezed into weight-removing column through pump, and lightness-removing column kettle material, will after weight-removing column separates
Weight-removing column tower top material imported into pan tank, and weight-removing column kettle material squeezes into heavy constituent slot through pump；
S6：The processing of weight-removing column material：Material in heavy constituent slot described in S5 is sucked in recovery tower by vacuum pump, is carried out
The material for recycling column overhead after material is separated by recovery tower, is imported into pan tank, the material of recovery tower tower reactor imports by separation
Tar slot, is recycled；
S7：Rectifying：2,6- diethylaniline material in pan tank described in S5 and S6 is put into rectifying device and carries out essence
Processing is evaporated, the rectifying to 2,6- diethylaniline can be completed；
S8：Storage：2,6- diethylaniline after rectifying described in S7 is put into container and is stored.
2. a kind of rectification process of 2,6- diethylaniline according to claim 1, which is characterized in that in the S1, benzene
Amine is alkylated with catalyst and ethylene to react and should carry out under conditions of 320 DEG C of high temperature, high pressure≤6.0Mpa.
3. a kind of rectification process of 2,6- diethylaniline according to claim 1, which is characterized in that in the S2, steam
Evaporating equipment is destilling tower, and reactant is imported in destilling tower, and heating vaporizes reactant, then makes the reactant liquefaction of gasification, is removed
Remove impurity therein.
4. a kind of rectification process of 2,6- diethylaniline according to claim 1, which is characterized in that in the S3,
When being filtered to thick finished product, during the thick finished product of 2,6- diethylaniline is imported large trough, 2,6- diethylanilines are thick
Finished product can first pass through the filter screen in large trough, be filtered, will be filtered to the impurity in the thick finished product of 2,6- diethylaniline again
Obtained impurity is imported into garbage collection bucket, is recycled.
5. a kind of rectification process of 2,6- diethylaniline according to claim 1, which is characterized in that in the S4, when
After filtered 2,6- diethylaniline material enters lightness-removing column, material is heated by the reboiler in lightness-removing column, is made
It obtains light component material to be discharged from tower top, be condensed into overhead condenser.
6. a kind of rectification process of 2,6- diethylaniline according to claim 1, which is characterized in that in the S5, when
When lightness-removing column kettle material is entered in weight-removing column, weight-removing column can take off the extra heavy constituent in material, by remaining material into
Row recycles.
7. a kind of rectification process of 2,6- diethylaniline according to claim 1, which is characterized in that in the S7, essence
Evaporating equipment is rectifying column, has different volatility using each component in 2,6- diethylaniline material, i.e., at the same temperature
This different property of the vapour pressure of each component, is transferred to the light component in liquid phase in gas phase, and the heavy constituent transfer in gas phase
Into liquid phase, rectifying separation is carried out to 2,6- diethylaniline material.
8. a kind of rectification process of 2,6- diethylaniline according to claim 1, which is characterized in that in the S8,
When being stored to 2,6- diethylaniline, 2,6- diethylaniline is put into container, is sealed processing, is avoided and skin
Contact, avoids heat, flame, Mars and other ignition sources, avoids contact with incompatible substance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811016945.7A CN108821980B (en) | 2018-09-03 | 2018-09-03 | Rectification process of 2, 6-diethylaniline |
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| CN201811016945.7A CN108821980B (en) | 2018-09-03 | 2018-09-03 | Rectification process of 2, 6-diethylaniline |
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| CN108821980A true CN108821980A (en) | 2018-11-16 |
| CN108821980B CN108821980B (en) | 2021-02-26 |
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| CN107793319A (en) * | 2017-09-06 | 2018-03-13 | 双阳化工淮安有限公司 | A kind of preparation technology of 2,6 diethylaniline |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107793319A (en) * | 2017-09-06 | 2018-03-13 | 双阳化工淮安有限公司 | A kind of preparation technology of 2,6 diethylaniline |
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