CN106966897A - One kind is used for methyl formate continuous esterification synthetic method and device - Google Patents
One kind is used for methyl formate continuous esterification synthetic method and device Download PDFInfo
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- CN106966897A CN106966897A CN201710195530.XA CN201710195530A CN106966897A CN 106966897 A CN106966897 A CN 106966897A CN 201710195530 A CN201710195530 A CN 201710195530A CN 106966897 A CN106966897 A CN 106966897A
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- esterification
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- methyl formate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a kind of methyl formate continuous esterification synthetic method and device, comprises the following steps：Using methanol and formic acid as raw material, esterification is carried out in the first high pass micro passage reaction, obtained reaction mass is continuously introduced into the first vapour liquid separator, and isolated gas phase feeding dehydrating tower epimere, isolated liquid phase is sent into the second high flux micro passage reaction；Methanol is continuously sent into the second high flux micro passage reaction and carries out esterification, obtained reaction mass is continuously introduced into the second vapour liquid separator, isolated gas phase feeding dehydrating tower epimere, isolated liquid phase enters dehydrating tower hypomere；The tower top discharging of dehydrating tower enters alcohol ester knockout tower, and control reflux ratio makes alcohol ester separate tower top methyl ester content and is more than 97%.The present invention realizes the continuous reaction of methyl formate；And reaction temperature is improved by high flux micro passage reaction, reaction efficiency is improved, the generation of side reaction is reduced, synthesis yield is more than 98%.
Description
Technical field
The invention belongs to continuous esterification synthetic method and its device, it is more particularly to a kind of for methyl formate continuous esterification
Synthetic method and device.
Background technology
The synthetic method of existing methyl formate is intermittent reaction.Synthetic method for intermittent reaction is less efficient
And the equipment of onsite application is more, the cost input of equipment is on the one hand added, on the other hand also make it that course of reaction is cumbersome
It is tediously long, add the input of human cost.And existing methyl formate uses enamel equipment, heat transfer effect is caused
Difference, the problem of energy consumption is big.
The content of the invention
It is used for methyl formate continuous esterification synthesis side it is an object of the invention to provide a kind of simple and easy to apply and higher efficiency
Method and device.
According to an aspect of the invention, there is provided a kind of methyl formate continuous esterification synthetic method, comprises the following steps：
1st step：Using methanol and formic acid as raw material, esterification is carried out in the first high pass micro passage reaction, is obtained
Reaction mass is continuously introduced into the first vapour liquid separator, isolated gas phase feeding dehydrating tower epimere, isolated liquid phase
Send into the second high flux micro passage reaction；
2nd step：Methanol is continuously sent into the second high flux micro passage reaction and carries out esterification, obtained reactant
Material is continuously introduced into the second vapour liquid separator, and isolated gas phase feeding dehydrating tower epimere, isolated liquid phase enters de-
Water tower hypomere；
3rd step：The tower top discharging of dehydrating tower enters alcohol ester knockout tower, and control reflux ratio makes alcohol ester separate tower top methyl ester content
More than 97%, return the 1st step after the bottom of towe methanol discharge of alcohol ester knockout tower and the 2nd step is applied mechanically.
In some embodiments, the mol ratio of the methanol and formic acid is 1.2~2.0:1.
In some embodiments, the esterification of the 1st step and the esterification of the 2nd step are added by steam
Heat heating, the reaction temperature of the 1st step is higher than the reaction temperature of the 2nd step.
In some embodiments, the reaction temperature of the esterification of the 1st step is 130 DEG C, the esterification of the 2nd step
The reaction temperature of reaction is 120 DEG C.
In some embodiments, the bottom of towe discharging of the dehydrating tower enters sewage disposal system.
According to another aspect of the present invention there is provided a kind of synthesizer for methyl formate continuous esterification, including
First high flux micro passage reaction, the first vapour liquid separator, the second high flux micro passage reaction, the second vapour liquid separator,
Dehydrating tower and alcohol ester knockout tower, the first high flux micro passage reaction, the first vapour liquid separator, the second high flux microchannel
Reactor and the second vapour liquid separator are sequentially connected, and first vapour liquid separator and the second vapour liquid separator take off with described respectively
Water tower is connected, and the dehydrating tower is connected with the alcohol ester knockout tower.
In some embodiments, the first high flux micro passage reaction and the second high flux micro passage reaction
Steam is entered by bottom is discharged by top.
In some embodiments, the first high flux micro passage reaction and the second high flux micro passage reaction
Material is glass or ceramics.
Its advantage is：The present invention realizes the continuous reaction of methyl formate；And pass through high flux microchannel plate
Answer device to improve reaction temperature, improve reaction efficiency, reduce the generation of side reaction, synthesis yield is more than 98%.
The present invention carries out heating treatment by steam heating to esterification, is conducive to improving reaction speed and yield；This
The reaction temperature of 2nd step of invention will be less than the reaction temperature of the 1st step, by temperature difference, realize pressure gap, realize material
There is pressure difference to flow from front to back, be also beneficial to improve product yield and product purity, eliminate safe hidden trouble, shorten reaction production
In the cycle, reduce the use of solvent and the generation of waste.
High flux micro passage reaction is by the preferable glass of antiseptic property or ceramic material, with outstanding anti-corruption
Corrosion energy, remarkable mass transfer and heat transfer efficiency；The present invention avoids using reactive distillation column, is formed using by glass or ceramic making
High flux micro passage reaction, greatly reduce the cost of device.
Brief description of the drawings
Fig. 1 is a kind of structural representation for methyl formate continuous esterification synthesizer of an embodiment of the present invention.
Embodiment
The synthesis for methyl formate continuous esterification that Fig. 1 schematically illustrates one embodiment of the present invention is filled
Put.As shown in figure 1, it is channel reactor 1, first that the synthesizer for being used for methyl formate continuous esterification, which includes the first high flux,
Vapour liquid separator 2, the second high flux are channel reactor 3, the second vapour liquid separator 4, dehydrating tower 5 and alcohol ester knockout tower 6.First
High flux is that channel reactor 1, the first vapour liquid separator 2, the second high flux are the vapour liquid separator 4 of channel reactor 3 and second
It is sequentially connected, the first vapour liquid separator 2 and the second vapour liquid separator 4 are connected with dehydrating tower 5 respectively, and dehydrating tower 5 is separated with alcohol ester
Tower 6 is connected.First high flux is that the bottom that the high flux of channel reactor 1 and second is channel reactor 3 is provided with steam inlet, top
Portion is provided with steam (vapor) outlet, and steam is entered by bottom is discharged by top.In order to strengthen the first high flux for channel reactor 1 and second
High flux is the antiseptic property of channel reactor 3, and the first high flux is that the high flux of channel reactor 1 and second is channel reactor
3 material is glass or ceramics.
Embodiment 1
The method that methyl formate is synthesized using synthesizer as shown in Figure 1, is comprised the following steps：
1st step：Using mol ratio as 1.2:1 methanol and formic acid is raw material, is carried out in the first high pass micro passage reaction
Esterification, esterification is by steam heat temperature raising, and reaction temperature is 130 DEG C.Obtained reaction mass is continuously introduced into first
In vapour liquid separator 2, the isolated gas phase feeding epimere of dehydrating tower 5, it is logical that isolated liquid phase, which sends into the second high flux,
In road reactor 3.
2nd step：Continuous to carry out esterification to the second high flux for feeding methanol in channel reactor 3, esterification is led to
Steam heat temperature raising is crossed, reaction temperature is 120 DEG C.Obtained reaction mass is continuously introduced into the second vapour liquid separator 4, is separated
The gas phase feeding epimere of dehydrating tower 5 arrived, isolated liquid phase enters the hypomere of dehydrating tower 5；
3rd step：The tower top discharging of dehydrating tower 5 enters alcohol ester knockout tower 6, and control reflux ratio makes alcohol ester knockout tower 6 push up methyl esters
Content is 98%, returns the 1st step after the bottom of towe methanol discharge of alcohol ester knockout tower 6 and the 2nd step is applied mechanically.The bottom of towe of dehydrating tower 5 discharge into
Enter sewage disposal system.
Embodiment 2
The method that methyl formate is synthesized using synthesizer as shown in Figure 1, is comprised the following steps：
1st step：Using mol ratio as 2:1 methanol and formic acid are raw material, are esterified in the first high pass micro passage reaction
Reaction, esterification is by steam heat temperature raising, and reaction temperature is 130 DEG C.Obtained reaction mass is continuously introduced into the first vapour-liquid
In separator 2, the isolated gas phase feeding epimere of dehydrating tower 5, it is that passage is anti-that isolated liquid phase, which sends into the second high flux,
Answer in device 3.
2nd step：Continuous to carry out esterification to the second high flux for feeding methanol in channel reactor 3, esterification is led to
Steam heat temperature raising is crossed, reaction temperature is 120 DEG C.Obtained reaction mass is continuously introduced into the second vapour liquid separator 4, is separated
The gas phase feeding epimere of dehydrating tower 5 arrived, isolated liquid phase enters the hypomere of dehydrating tower 5；
3rd step：The tower top discharging of dehydrating tower 5 enters alcohol ester knockout tower 6, and control reflux ratio makes alcohol ester knockout tower 6 push up methyl esters
Content is 99%, returns the 1st step after the bottom of towe methanol discharge of alcohol ester knockout tower 6 and the 2nd step is applied mechanically.The bottom of towe of dehydrating tower 5 discharge into
Enter sewage disposal system.
Above-described is only some embodiments of the present invention.For those of ordinary skill in the art, do not taking off
On the premise of the invention design, various modifications and improvements can be made, these belong to protection scope of the present invention.
Claims (8)
1. a kind of methyl formate continuous esterification synthetic method, it is characterised in that comprise the following steps：
1st step：Using methanol and formic acid as raw material, esterification is carried out in the first high pass micro passage reaction, obtained reaction
Material is continuously introduced into the first vapour liquid separator, isolated gas phase feeding dehydrating tower epimere, isolated liquid phase feeding
In second high flux micro passage reaction；
2nd step：Methanol is continuously sent into the second high flux micro passage reaction and carries out esterification, obtained reaction mass connects
In the second vapour liquid separator of continuous feeding, isolated gas phase feeding dehydrating tower epimere, isolated liquid phase enters dehydrating tower
Hypomere；
3rd step：The tower top discharging of dehydrating tower enters alcohol ester knockout tower, and control reflux ratio is more than alcohol ester separation tower top methyl ester content
97%, return the 1st step after the bottom of towe methanol discharge of alcohol ester knockout tower and the 2nd step is applied mechanically.
2. methyl formate continuous esterification synthetic method according to claim 1, it is characterised in that the methanol and formic acid
Mol ratio is 1.2~2.0:1.
3. methyl formate continuous esterification synthetic method according to claim 1, it is characterised in that the esterification of the 1st step
The esterification of reaction and the 2nd step is by steam heat temperature raising, and the reaction temperature of the 1st step is higher than the 2nd step
Reaction temperature.
4. methyl formate continuous esterification synthetic method according to claim 3, it is characterised in that the esterification of the 1st step
The reaction temperature of reaction is 130 DEG C, and the reaction temperature of the esterification of the 2nd step is 120 DEG C.
5. methyl formate continuous esterification synthetic method according to claim 1, it is characterised in that the bottom of towe of the dehydrating tower
Discharging enters sewage disposal system.
6. answered for claim 1-5 high fluxs micro passage reaction, the first vapour liquid separator, the second high flux microchannel plate
Device, the second vapour liquid separator, dehydrating tower and alcohol ester knockout tower, the first high flux micro passage reaction, the first vapor-liquid separation
Device, the second high flux micro passage reaction and the second vapour liquid separator are sequentially connected, first vapour liquid separator and the second vapour
Liquid/gas separator is connected with the dehydrating tower respectively, and the dehydrating tower is connected with the alcohol ester knockout tower.
7. the synthesizer according to claim 6 for methyl formate continuous esterification, it is characterised in that described first is high
The steam of flux micro passage reaction and the second high flux micro passage reaction is entered by bottom is discharged by top.
8. the synthesizer according to claim 6 for methyl formate continuous esterification, it is characterised in that described first is high
The material of flux micro passage reaction and the second high flux micro passage reaction is glass or ceramics.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710195530.XA CN106966897A (en) | 2017-03-29 | 2017-03-29 | One kind is used for methyl formate continuous esterification synthetic method and device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710195530.XA CN106966897A (en) | 2017-03-29 | 2017-03-29 | One kind is used for methyl formate continuous esterification synthetic method and device |
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| CN201710195530.XA Pending CN106966897A (en) | 2017-03-29 | 2017-03-29 | One kind is used for methyl formate continuous esterification synthetic method and device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400554A (en) * | 2018-12-25 | 2019-03-01 | 江苏兄弟维生素有限公司 | Synthesize alpha-chloro-α-acetyl group-gamma-butyrolacton formate methyl esters method and apparatus |
| CN110590577A (en) * | 2019-09-25 | 2019-12-20 | 山东省化工研究院 | Device and method for continuously synthesizing ester quaternary ammonium compound |
| WO2022199646A1 (en) * | 2021-03-26 | 2022-09-29 | 广州理文科技有限公司 | Continuous flow reaction device and method for flow synthesis of bis(fluorosulfonyl)imide based on same |
-
2017
- 2017-03-29 CN CN201710195530.XA patent/CN106966897A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400554A (en) * | 2018-12-25 | 2019-03-01 | 江苏兄弟维生素有限公司 | Synthesize alpha-chloro-α-acetyl group-gamma-butyrolacton formate methyl esters method and apparatus |
| CN109400554B (en) * | 2018-12-25 | 2020-08-04 | 江苏兄弟维生素有限公司 | Method and device for synthesizing α -chloro- α -acetyl-gamma-butyrolactone and co-producing methyl formate |
| CN110590577A (en) * | 2019-09-25 | 2019-12-20 | 山东省化工研究院 | Device and method for continuously synthesizing ester quaternary ammonium compound |
| WO2022199646A1 (en) * | 2021-03-26 | 2022-09-29 | 广州理文科技有限公司 | Continuous flow reaction device and method for flow synthesis of bis(fluorosulfonyl)imide based on same |
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| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 224100 Southern District of Yancheng City Dafeng Marine Economic Development Zone, Jiangsu Applicant after: Jiangsu Brother Vitamins Co., Ltd. Address before: 224145 Southern District of Yancheng City Marine Economic Development Zone, Jiangsu Applicant before: Jiangsu Brother Vitamins Co., Ltd. |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170721 |
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| RJ01 | Rejection of invention patent application after publication |