CN211636491U - M-methyl anisole circulation micro-reaction device - Google Patents
M-methyl anisole circulation micro-reaction device Download PDFInfo
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- CN211636491U CN211636491U CN201922180476.9U CN201922180476U CN211636491U CN 211636491 U CN211636491 U CN 211636491U CN 201922180476 U CN201922180476 U CN 201922180476U CN 211636491 U CN211636491 U CN 211636491U
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Abstract
The utility model discloses a meta-methyl anisole circulation micro-reaction device, which comprises a reaction kettle; the material inlet of the reaction kettle is respectively communicated with a metacresol feeding pipe, a dimethyl sulfate feeding pipe and a sodium hydroxide feeding pipe; the material inlet of the reaction kettle is also provided with a micro mixer; the bottom outlet of the reaction kettle is respectively communicated with a finished product conveying pipe and an external circulation pipeline; the external circulation pipeline is communicated with the micro mixer; and the external circulation pipeline is provided with a circulation pump and a heat exchanger. The utility model is used for methyl anisole circulation microreaction between adopts the form of circulation reaction, disperses into the micron order liquid drop of high dispersion with sodium hydroxide solution through micromixer, has increased the area of contact of sodium hydroxide and metacresol, the effectual concentration that has reduced sodium hydroxide among the reaction system to the alkaline decomposition of dimethyl sulfate has been restrained, has improved conversion rate and reaction rate.
Description
Technical Field
The utility model relates to a chemical synthesis technical field, concretely relates to synthesizer of methyl anisole.
Background
The m-methyl anisole is an organic synthesis intermediate, can be used for synthesizing medicines and pesticides, is also an important raw material of pressure-sensitive and thermosensitive dyes, and is widely applied to the synthesis of fine chemicals. As one of the oxyalkylation reactions of the phenolic hydroxyl group, it can be obtained by reacting it with a corresponding alkylating agent, such as dimethyl sulfate method, halogenated methane method, dimethyl carbonate method, etc. The halogen (chlorine, bromine and iodine) methyl alkane as a classical alkylating reagent has high reaction activity, but has a low boiling point, and the synthesis operation conditions are harsh and expensive. The dimethyl carbonate method is a novel methylating agent, has the characteristics of environmental protection and the like, but has low activity and can react only at high reaction temperature. Dimethyl sulfate has the advantages of high boiling point and high activity, and is a widely used methylating agent.
Two typical process routes are provided for synthesizing m-methyl anisole by using dimethyl sulfate as a methylating agent, wherein a sodium hydroxide solution is slowly dripped into a mixed solution of m-cresol and dimethyl sulfate. In order to prevent the excessive alkaline hydrolysis of the dimethyl sulfate, the reaction needs to be carried out at a low temperature of about 5 ℃, so the process energy consumption and the unit consumption of the dimethyl sulfate are high; secondly, m-cresol firstly reacts with a proper amount of sodium hydroxide to be converted into m-cresol sodium salt, and then dimethyl sulfate is dripped into the sodium salt water solution to react. Compared with the former, the reaction system has high pH and strong alkalinity, and is easy to cause the alkaline hydrolysis of dimethyl sulfate, so that the utilization rate of the dimethyl sulfate is reduced.
Disclosure of Invention
The utility model discloses the technical problem that will solve is: aiming at the defects in the prior art, the m-methyl anisole circulation micro-reaction device with low energy consumption, low consumption and high yield is provided.
In order to solve the technical problem, the technical scheme of the utility model is that:
an m-methyl anisole circulation micro-reaction device:
the reaction device comprises a reaction kettle;
the material inlet of the reaction kettle is respectively communicated with a metacresol feeding pipe, a dimethyl sulfate feeding pipe and a sodium hydroxide feeding pipe;
the material inlet of the reaction kettle is also provided with a micro mixer;
the bottom outlet of the reaction kettle is respectively communicated with a finished product conveying pipe and an external circulation pipeline; the external circulation pipeline is communicated with the micro mixer;
and the external circulation pipeline is provided with a circulation pump and a heat exchanger.
As an improved technical scheme, the finished product conveying pipe is sequentially communicated with a mixed clarifying tank and a finished product storage tank; the upper part of the mixing and clarifying tank is also communicated with a waste water storage tank.
As an improved technical scheme, a first metering pump, a second metering pump and a third metering pump are respectively arranged on the m-cresol feeding pipe, the dimethyl sulfate feeding pipe and the sodium hydroxide feeding pipe; and the m-cresol feeding pipe, the dimethyl sulfate feeding pipe and the sodium hydroxide feeding pipe are respectively provided with a first electric valve, a second electric valve and a third electric valve.
As an improved technical scheme, a circulation electric valve and a conveying electric valve are respectively arranged on the finished product conveying pipe and the external circulation pipeline.
As an improved technical scheme, the micro mixer is a micro-sieve-hole dispersing mixer, or a cross micro-channel mixer of any one or two of a T-shaped micro-channel mixer and a Y-shaped micro-channel mixer.
As an optimized technical scheme, the diameter of a microchannel of the T-shaped microchannel mixer is 200-500 um, and the number of the microchannels is one or more.
As an optimized technical scheme, the number of the micro-channels of the Y-shaped micro-channel mixer is 200-1000 um, and the number of the micro-channels is one or more than one.
As a preferred technical scheme, the m-cresol feeding pipe, the dimethyl sulfate feeding pipe and the sodium hydroxide feeding pipe are respectively communicated with an m-cresol charging bucket, a dimethyl sulfate charging bucket and a sodium hydroxide charging bucket.
As an improved technical scheme, the reaction kettle is provided with a stirring device.
As a further preferable technical scheme, the stirring device comprises a stirring shaft arranged in the reaction kettle and a stirring motor electrically connected with the stirring shaft; and the stirring shaft is provided with a stirring paddle.
Since the technical scheme is used, the beneficial effects of the utility model are that:
in the meta-methyl anisole circulation micro-reaction device of the utility model, the material inlet of the reaction kettle is respectively communicated with a meta-cresol feeding pipe, a dimethyl sulfate feeding pipe and a sodium hydroxide feeding pipe; the material inlet of the reaction kettle is also provided with a micro mixer; the bottom outlet of the reaction kettle is respectively communicated with a finished product conveying pipe and an external circulation pipeline; the external circulation pipeline is communicated with the micro mixer; a circulating pump and a heat exchanger are arranged on the external circulating pipeline; the utility model is used for among methyl anisole circulation micro reaction, can adopt the form of circulation reaction, introduce metacresol and dimethyl sulfate into the reation kettle first and mix and form the circulating solution, circulate the sodium hydroxide solution with the circulating solution through the outer circulation pipeline and flow through the micromixer simultaneously, get into the reation kettle after fully mixing with the sodium hydroxide solution in the micromixer; the sodium hydroxide solution is dispersed into highly dispersed micron-sized liquid drops through the micro mixer, so that the contact area of the sodium hydroxide and the m-cresol is increased, the sodium hydroxide added into a reaction system and the m-cresol are subjected to acid-base reaction rapidly to form m-cresol sodium salt, the concentration of the sodium hydroxide in the reaction system is effectively reduced, and the alkaline decomposition of dimethyl sulfate is inhibited. On the other hand, the generated m-cresol sodium salt can quickly react with dimethyl sulfate around the m-cresol sodium salt to form a target product, so that the reaction rate is further improved.
The utility model discloses a reaction unit, moreover, the steam generator is simple in structure, and reasonable in design, the combination of micromixer and extrinsic cycle has both realized the high dispersion and the abundant contact of sodium hydroxide solution in raw materials mixed solution, can make the reaction system be in lower pH value state all the time again, consequently showing the probability of hydrolysising that has reduced dimethyl sulfate, make full use of reaction heat simultaneously, make the reaction system be in relatively higher reaction temperature, meta-cresol and dimethyl sulfate's reaction rate has been improved, the raw materials conversion rate has been improved, the energy consumption of the reaction has been reduced.
Drawings
The present invention will be further explained with reference to the drawings and examples.
FIG. 1 is a schematic structural view of a reaction apparatus of the present invention;
in the figure, 1, a reaction kettle; 11. a stirring device; 12. a material inlet; 13. a bottom outlet; 14. an external circulation line; 15. a heat exchanger; 16. a micro mixer; 17. a circulating electric valve; 18. a circulation pump; 2. a metacresol feeding pipe; 21. a first metering pump; 22. a first electrically operated valve; 23. a meta-cresol bucket; 3. a dimethyl sulfate feeding pipe; 31. a second metering pump; 32. a second electrically operated valve; 33. a dimethyl sulfate tank; 4. a sodium hydroxide feeding pipe; 41. a third metering pump; 42. a third electrically operated valve; 43. a sodium hydroxide tank; 5. a finished product conveying pipe; 51. a delivery electric valve; 52. a delivery pump; 6. a mixing and clarifying tank; 7. a finished product storage tank; 8. a waste water storage tank.
Detailed Description
The invention is further explained below with reference to the drawings and examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes and modifications of the present invention may be made by those skilled in the art after reading the teachings of the present invention, and these equivalents also fall within the scope of the appended claims.
As shown in the attached drawings, the utility model discloses a circulation micro reaction unit of m-methyl anisole: the reaction device comprises a reaction kettle 1, and the reaction kettle 1 is provided with a stirring device 11; a material inlet 12 of the reaction kettle 1 is respectively communicated with a metacresol feeding pipe 2, a dimethyl sulfate feeding pipe 3 and a sodium hydroxide feeding pipe 4; the m-cresol feeding pipe 2, the dimethyl sulfate feeding pipe 3 and the sodium hydroxide feeding pipe 4 are respectively provided with a first metering pump 21, a second metering pump 31 and a third metering pump 41; and a first, second and third electrically operated valves 22, 32, 42; the metacresol feeding pipe 2, the dimethyl sulfate feeding pipe 3 and the sodium hydroxide feeding pipe 4 are respectively communicated with a metacresol charging bucket 23, a dimethyl sulfate charging bucket 33 and a sodium hydroxide charging bucket 43. The bottom outlet 13 of the reaction kettle 1 is respectively communicated with a finished product conveying pipe 5 and an external circulation pipeline 14; a heat exchanger 15 and a micro mixer 16 are arranged on the external circulation pipeline 14; a circulation electric valve 17 and a circulation pump 18 are also provided. The metacresol feeding pipe 2, the dimethyl sulfate feeding pipe 3 and the sodium hydroxide feeding pipe 4 are respectively communicated with the micro mixer 16 and are communicated with the material inlet 12 of the reaction kettle 1 through the micro mixer 16. The finished product conveying pipe 5 is sequentially communicated with a mixed clarifying tank 6 and a finished product storage tank 7; the upper part of the mixing and clarifying tank 6 is also communicated with a waste water storage tank 8. The finished product delivery pipe 5 is also provided with a delivery electric valve 51 and a delivery pump 52.
In a preferred embodiment, the micromixer is a T-type microchannel mixer. The diameter of the micro-channel of the T-shaped micro-channel mixer is 400um, and the number of the micro-channels is one.
In another preferred embodiment, the micromixer is a Y-type microchannel mixer. The diameter of the micro-channel of the Y-shaped micro-channel mixer is 500um, and the number of the micro-channels is one.
Claims (9)
1. An m-methyl anisole circulation micro-reaction device is characterized in that:
the reaction device comprises a reaction kettle;
the material inlet of the reaction kettle is respectively communicated with a metacresol feeding pipe, a dimethyl sulfate feeding pipe and a sodium hydroxide feeding pipe;
the material inlet of the reaction kettle is also provided with a micro mixer;
the bottom outlet of the reaction kettle is respectively communicated with a finished product conveying pipe and an external circulation pipeline; the external circulation pipeline is communicated with the micro mixer;
and the external circulation pipeline is provided with a circulation pump and a heat exchanger.
2. The m-methylanisole loop micro-reaction device as claimed in claim 1, characterized in that: the finished product conveying pipe is sequentially communicated with a mixed clarifying tank and a finished product storage tank; the upper part of the mixing and clarifying tank is also communicated with a waste water storage tank.
3. The m-methylanisole loop micro-reaction device as claimed in claim 1, characterized in that: a first metering pump, a second metering pump and a third metering pump are respectively arranged on the m-cresol feeding pipe, the dimethyl sulfate feeding pipe and the sodium hydroxide feeding pipe; and the m-cresol feeding pipe, the dimethyl sulfate feeding pipe and the sodium hydroxide feeding pipe are respectively provided with a first electric valve, a second electric valve and a third electric valve.
4. The m-methylanisole loop micro-reaction device as claimed in claim 1, characterized in that: and the finished product conveying pipe and the external circulating pipeline are respectively provided with a circulating electric valve and a conveying electric valve.
5. The m-methylanisole loop micro-reaction device as claimed in claim 1, characterized in that: the micro mixer is a micro-sieve-hole dispersing mixer, or a cross micro-channel mixer of any one or two of a T-shaped micro-channel mixer and a Y-shaped micro-channel mixer.
6. The m-methylanisole loop micro-reaction device as defined in claim 5, wherein: the diameter of the micro-channel of the T-shaped micro-channel mixer is 200-500 um, and the number of the micro-channels is one or more than one.
7. The m-methylanisole loop micro-reaction device as defined in claim 5, wherein: the microchannel of the Y-shaped microchannel mixer is 200-1000 um, and the number of the microchannels is one or more than one.
8. The m-methylanisole loop micro-reaction device as claimed in claim 1, characterized in that: the metacresol feeding pipe, the dimethyl sulfate feeding pipe and the sodium hydroxide feeding pipe are respectively communicated with a metacresol charging bucket, a dimethyl sulfate charging bucket and a sodium hydroxide charging bucket.
9. The m-methylanisole loop micro-reaction device as claimed in claim 1, characterized in that: the reaction kettle is provided with a stirring device.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201922180476.9U CN211636491U (en) | 2019-12-06 | 2019-12-06 | M-methyl anisole circulation micro-reaction device |
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| CN201922180476.9U CN211636491U (en) | 2019-12-06 | 2019-12-06 | M-methyl anisole circulation micro-reaction device |
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| CN211636491U true CN211636491U (en) | 2020-10-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114797737A (en) * | 2022-04-09 | 2022-07-29 | 河北利仕化学科技有限公司 | Clean synthesizer of dibromo hydantoin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114797737A (en) * | 2022-04-09 | 2022-07-29 | 河北利仕化学科技有限公司 | Clean synthesizer of dibromo hydantoin |
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