CN110343071A - A kind of purifying process of 1- methylimidazole - Google Patents
A kind of purifying process of 1- methylimidazole Download PDFInfo
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- CN110343071A CN110343071A CN201910719177.XA CN201910719177A CN110343071A CN 110343071 A CN110343071 A CN 110343071A CN 201910719177 A CN201910719177 A CN 201910719177A CN 110343071 A CN110343071 A CN 110343071A
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- methyl imidazole
- imidazole solution
- purifying process
- methylimidazole
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D233/56—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms
- C07D233/58—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring nitrogen atoms
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of purifying process of 1- methylimidazole, purification step is as follows: reactant imidazoles and methanol are put into reaction unit by a. first, then are added catalyst into reaction unit and reacted, and 1- methyl imidazole solution is made；B. after the completion of step a, then 1- methyl imidazole solution obtained is put into distilling apparatus and is purified；C. it after the completion of step b, reuses purity detecting device and the 1- methyl imidazole solution obtained after distillation is detected, when 1- methyl imidazole solution purity is not achieved 99%, places into and continue to distill in distilling apparatus；D. after the completion of step c, then will be obtained after distillation pure 1- methyl imidazole solution be encased in filling in be packaged.The present invention has many advantages, such as that purification procedures are few, is easy to get without concentration, raw material, simple process, easy to accomplish, consume energy low and high income, and the purifying process in the invention can recycle progress, improve the purity of 1- methylimidazole after purification.
Description
Technical field
The present invention relates to purifying process technical field, specially a kind of purifying process of 1- methylimidazole.
Background technique
Currently, there is also the places of some shortcomings for the purifying process of existing 1- methylimidazole, such as；Existing 1- first
The process of the purifying process of base imidazoles is relatively more, needs concentration, complex process, be not easily accomplished, the high and yield that consumes energy compares
It is low, and the purifying process of existing 1- methylimidazole cannot recycle progress, reduce the purity of 1- methylimidazole after purification.
Summary of the invention
The purpose of the present invention is to provide a kind of purifying process of 1- methylimidazole, solve proposed in background technique
Problem.
To achieve the above object, the invention provides the following technical scheme: a kind of purifying process of 1- methylimidazole, purifying step
It is rapid as follows:
A. reactant imidazoles and methanol are put into reaction unit first, then add catalyst into reaction unit and carries out
1- methyl imidazole solution is made in reaction；
B. after the completion of step a, then 1- methyl imidazole solution obtained is put into distilling apparatus and is purified；
C. it after the completion of step b, reuses purity detecting device and the 1- methyl imidazole solution obtained after distillation is examined
It surveys, when 1- methyl imidazole solution purity is not achieved 99%, places into and continue to distill in distilling apparatus；
D. after the completion of step c, then will be obtained after distillation pure 1- methyl imidazole solution be encased in filling in be packaged.
As a kind of preferred embodiment of the invention, reaction unit is continuously flowed instead using fixed bed in the step a
Device is answered, the catalyst is with ammonium metatungstate pillared hydrotalcite.
As a kind of preferred embodiment of the invention, the molar ratio of imidazoles and methanol is 1:1~10 in the step a.
Pressure as a kind of preferred embodiment of the invention, in the continuous flow reactor use process of fixed bed
Power is 0.1~1MPa, and temperature is 0.05~0.6/h of reaction solution feedstock quality air speed at 250~400 DEG C.
As a kind of preferred embodiment of the invention, pressure when distilling apparatus uses in the step b is 4.0-
5.0kPa, temperature are 100~110 DEG C.
As a kind of preferred embodiment of the invention, the step c moderate purity detection device is using portable electric
Sub- detector.
As a kind of preferred embodiment of the invention, pure 1- methyl imidazole solution is encased in filling in the step d
In be packaged, the jar using brown glass make.
Compared with prior art, beneficial effects of the present invention are as follows:
The present invention have that purification procedures are few, be easy to get without concentration, raw material, simple process, easy to accomplish, energy consumption are low and
The advantages that high income, and the purifying process in the invention can recycle progress, improve the purity of 1- methylimidazole after purification.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is a kind of flow chart of the purifying process of 1- methylimidazole of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Referring to Fig. 1, the present invention provides a kind of technical solution: a kind of purifying process of 1- methylimidazole, purification step is such as
Under:
A. reactant imidazoles and methanol are put into reaction unit first, then add catalyst into reaction unit and carries out
1- methyl imidazole solution is made in reaction；
B. after the completion of step a, then 1- methyl imidazole solution obtained is put into distilling apparatus and is purified；
C. it after the completion of step b, reuses purity detecting device and the 1- methyl imidazole solution obtained after distillation is examined
It surveys, when 1- methyl imidazole solution purity is not achieved 99%, places into and continue to distill in distilling apparatus；
D. after the completion of step c, then will be obtained after distillation pure 1- methyl imidazole solution be encased in filling in be packaged.
Further, reaction unit uses the continuous flow reactor of fixed bed in the step a, and the catalyst is with inclined
Ammonium tungstate pillared hydrotalcite.
Further, the molar ratio of imidazoles and methanol is 1:1~10 in the step a.
Further, the pressure in the continuous flow reactor use process of the fixed bed is 0.1~1MPa, and temperature is
At 250~400 DEG C, 0.05~0.6/h of reaction solution feedstock quality air speed.
Further, pressure when distilling apparatus uses in the step b is 4.0-5.0kPa, and temperature is 100~110 DEG C.
Further, the step c moderate purity detection device is using portable electronic detector.
Further, 1- methyl imidazole solution pure in the step d is encased in filling and is packaged, and the jar uses
The glass of brown makes.
Embodiment one
A kind of purifying process of 1- methylimidazole, purification step are as follows:
A. reactant imidazoles and methanol are put into reaction unit first, then add catalyst into reaction unit and carries out
1- methyl imidazole solution is made in reaction；
B. after the completion of step a, then 1- methyl imidazole solution obtained is put into distilling apparatus and is purified；
C. it after the completion of step b, reuses purity detecting device and the 1- methyl imidazole solution obtained after distillation is examined
It surveys, when 1- methyl imidazole solution purity is not achieved 99%, places into and continue to distill in distilling apparatus；
D. after the completion of step c, then will be obtained after distillation pure 1- methyl imidazole solution be encased in filling in be packaged.
The pressure when distilling apparatus uses is 4.0kPa, and temperature is 100 DEG C.
Embodiment two
A kind of purifying process of 1- methylimidazole, purification step are as follows:
A. reactant imidazoles and methanol are put into reaction unit first, then add catalyst into reaction unit and carries out
1- methyl imidazole solution is made in reaction；
B. after the completion of step a, then 1- methyl imidazole solution obtained is put into distilling apparatus and is purified；
C. it after the completion of step b, reuses purity detecting device and the 1- methyl imidazole solution obtained after distillation is examined
It surveys, when 1- methyl imidazole solution purity is not achieved 99%, places into and continue to distill in distilling apparatus；
D. after the completion of step c, then will be obtained after distillation pure 1- methyl imidazole solution be encased in filling in be packaged.
The pressure when distilling apparatus uses is 5.0kPa, and temperature is 110 DEG C.
Traditional purification process data parameters table 1 is as follows:
| Test item | High income | Technique process | Energy consumption | Purity after purification |
| Parameter index | It is low | It is more | It is high | It is lower |
One purifying process data parameters table 2 of embodiment is as follows:
| Test item | High income | Technique process | Energy consumption | Purity after purification |
| Parameter index | Generally | It is more | Generally | Generally |
Two purifying process data parameters table 3 of embodiment is as follows:
| Test item | High income | Technique process | Energy consumption | Purity after purification |
| Parameter index | It is high | It is few | It is low | It is high |
It to sum up states, is obtained referring to the data comparison of table 1, table 2 and table 3, the present invention is few with purification procedures, is not necessarily at concentration
The advantages that reason, raw material be easy to get, simple process, easy to accomplish, the low and high income that consumes energy, and the purifying process in the invention can be with
Circulation carries out, and improves the purity of 1- methylimidazole after purification.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention, for this field skill
For art personnel, it is clear that invention is not limited to the details of the above exemplary embodiments, and without departing substantially from spirit of the invention or
In the case where essential characteristic, the present invention can be realized in other specific forms.Therefore, in all respects, should all incite somebody to action
Embodiment regards exemplary as, and is non-limiting, the scope of the present invention by appended claims rather than on state
Bright restriction, it is intended that including all changes that fall within the meaning and scope of the equivalent elements of the claims in the present invention
It is interior.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (7)
1. a kind of purifying process of 1- methylimidazole, it is characterised in that: purification step is as follows:
A. reactant imidazoles and methanol are put into reaction unit first, then add catalyst into reaction unit and carries out instead
It answers, 1- methyl imidazole solution is made；
B. after the completion of step a, then 1- methyl imidazole solution obtained is put into distilling apparatus and is purified；
C. it after the completion of step b, reuses purity detecting device and the 1- methyl imidazole solution obtained after distillation is detected, 1-
When methyl imidazole solution purity is not achieved 99%, places into and continue to distill in distilling apparatus；
D. after the completion of step c, then will be obtained after distillation pure 1- methyl imidazole solution be encased in filling in be packaged.
2. a kind of purifying process of 1- methylimidazole according to claim 1, it is characterised in that: reacted in the step a
Device uses the continuous flow reactor of fixed bed, and the catalyst is with ammonium metatungstate pillared hydrotalcite.
3. a kind of purifying process of 1- methylimidazole according to claim 1, it is characterised in that: imidazoles in the step a
Molar ratio with methanol is 1:1~10.
4. a kind of purifying process of 1- methylimidazole according to claim 2, it is characterised in that: the fixed bed continuous flow
Pressure in dynamic reaction unit use process is 0.1~1MPa, and temperature is reaction solution feedstock quality air speed at 250~400 DEG C
0.05~0.6/h.
5. a kind of purifying process of 1- methylimidazole according to claim 1, it is characterised in that: distilled in the step b
Pressure when device uses is 4.0-5.0kPa, and temperature is 100~110 DEG C.
6. a kind of purifying process of 1- methylimidazole according to claim 1, it is characterised in that: the step c moderate purity
Detection device is using portable electronic detector.
7. a kind of purifying process of 1- methylimidazole according to claim 1, it is characterised in that: pure in the step d
1- methyl imidazole solution be encased in filling in be packaged, the jar using brown glass make.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111410634A (en) * | 2020-05-19 | 2020-07-14 | 郑州中科新兴产业技术研究院 | Novel efficient dynamic N-methylimidazole synthesis and purification technology |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086978A (en) * | 2013-02-06 | 2013-05-08 | 江苏康乐新材料科技有限公司 | 1-methylimidazole preparation method |
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2019
- 2019-08-05 CN CN201910719177.XA patent/CN110343071A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086978A (en) * | 2013-02-06 | 2013-05-08 | 江苏康乐新材料科技有限公司 | 1-methylimidazole preparation method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111410634A (en) * | 2020-05-19 | 2020-07-14 | 郑州中科新兴产业技术研究院 | Novel efficient dynamic N-methylimidazole synthesis and purification technology |
| CN111410634B (en) * | 2020-05-19 | 2022-03-29 | 郑州中科新兴产业技术研究院 | Novel efficient dynamic N-methylimidazole synthesis and purification technology |
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