CN214971828U - Synthesis device of chiral ester compound - Google Patents
Synthesis device of chiral ester compound Download PDFInfo
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- CN214971828U CN214971828U CN202121046752.3U CN202121046752U CN214971828U CN 214971828 U CN214971828 U CN 214971828U CN 202121046752 U CN202121046752 U CN 202121046752U CN 214971828 U CN214971828 U CN 214971828U
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Abstract
The utility model discloses a synthesizing device of chiral ester compounds, wherein the output end of a first condenser is connected with the input end of a first receiving tank, the output end of the first receiving tank is connected with the input end of a rectifying still, the output end of the rectifying still is connected with the input end of a second condenser, the output end of the second condenser is connected with a second receiving tank, and the distilling still and the rectifying still are respectively provided with a steam input end; the distillation still is provided with a first jacket, and a first heating space for accommodating steam is formed between the distillation still and the first jacket; still include first drain valve, for the distillation still provides the comdenstion water collection container of required cooling water when the cooling, first drain valve and first press from both sides cover and be connected, first drain valve and comdenstion water collection container are connected whether to discharge the comdenstion water collection container in order to control the comdenstion water that forms in the first heating space, and the comdenstion water is collected the container output and is connected with first cover. The utility model discloses be favorable to making the efficiency of decompression desolventizing obtain the guarantee.
Description
Technical Field
The utility model relates to a chemical product production facility technical field, in particular to synthesizer of chiral ester compound.
Background
R-propylene carbonate is a medical intermediate, and is mainly used for synthesizing Tenofovir disoproxil which is a popular anti-AIDS and anti-hepatitis B virus medicine. The preparation method of the R-propylene carbonate comprises the following steps: transesterification, carbon dioxide synthesis, and the like. At present, the domestic industrial production of R-propylene carbonate adopts an ester exchange method of R-propylene glycol and diethyl carbonate.
The current process is roughly as follows: after propylene glycol and dimethyl carbonate are input into the distillation kettle, sodium acetate is added, stirring is carried out, and the first condenser is started to work. Opening a steam valve connected with a distillation still, slowly heating to raise the temperature in the distillation still to 59-62 ℃, distilling out the generated methanol while reacting, then raising the temperature to 64 ℃ within 1 hour, then raising the temperature from 64 ℃ to 110 ℃, distilling out the solvent at the moment, cooling by a first condenser, then entering a first receiving tank, keeping the solvent distilled out, and slowly raising the temperature until the reaction is finished. And closing a steam valve connected with the distillation kettle, and introducing tap water to cool the distillation kettle. Closing a feeding valve of the distillation kettle, pulling vacuum through the first receiving tank to slowly raise the temperature of the distillation kettle, decompressing and releasing the solvent into the first receiving tank until the temperature is raised to 105 ℃ and the solvent cannot be discharged, and then entering a rectification process.
For the above process, in the cooling stage, tap water is directly used to cool the distillation still, and at this time, the temperature of the distillation still and the internal mixed solution thereof is 110 ℃, and the temperature difference between the tap water and the distillation still and the internal mixed solution thereof is very large, so that although the temperature can be rapidly reduced, the mixed solution in the distillation still can be cooled by the rapid cooling method, the efficiency of the subsequent decompression desolventizing is reduced, that is, the amount of the solvent removed by decompression is reduced.
SUMMERY OF THE UTILITY MODEL
The utility model provides a synthesizer of chiral ester compound, the utility model discloses be favorable to making the efficiency of decompression desolventizing obtain the guarantee.
The technical scheme for solving the technical problems is as follows:
the device for synthesizing the chiral ester compound comprises a material storage tank, a metering pump, a distillation kettle, a first condenser, a first receiving tank, a rectification kettle, a second condenser and a second receiving tank, wherein the material storage tank is connected with the metering pump, the output end of the metering pump is connected with the distillation kettle, the distillation kettle is connected with the input end of the first condenser, the output end of the first condenser is connected with the input end of the first receiving tank, the output end of the first receiving tank is connected with the input end of the rectification kettle, the output end of the rectification kettle is connected with the input end of the second condenser, the output end of the second condenser is connected with the second receiving tank, and the distillation kettle and the rectification kettle are respectively provided with a steam input end;
the distillation still is provided with a first jacket, and a first heating space for accommodating steam is formed between the distillation still and the first jacket;
still include first drain valve, for the distillation still provides the comdenstion water collection container of required cooling water when the cooling, first drain valve and first press from both sides cover and be connected, first drain valve and comdenstion water collection container are connected whether to discharge the comdenstion water collection container in order to control the comdenstion water that forms in the first heating space, and the comdenstion water is collected the container output and is connected with first cover.
Further, a second jacket is arranged on the rectifying still, and a second heating space for containing steam is formed between the rectifying still and the second jacket;
the second drain valve is connected with the second jacket and is connected with the condensed water collecting container to control whether condensed water formed in the second heating space is discharged into the condensed water collecting container or not.
Further, the leak detection assembly is also included, and the leak detection assembly includes:
one end of the first valve is connected with the output end of the condensed water collecting container;
a second valve;
and the leak detection valve and the second valve are connected to the other end of the first valve in parallel.
Furthermore, the device also comprises a water replenishing valve and a main pipe, wherein the main pipe is connected with a steam input end on the distillation kettle, and the water replenishing valve and the condensed water collecting container are respectively connected with the main pipe.
In this embodiment, what adopt is that slow cooling mode cools down stills, specifically is: because the steam lets in the first heating space after, can form the comdenstion water after the steam gives out the heat, these comdenstion waters are sent to in the comdenstion water collection container through first drain valve and are saved, though the temperature of comdenstion water is less than the temperature of steam, but the temperature of running water than normal atmospheric temperature is much higher, therefore, when needs are cooled down to stills, export the comdenstion water in the comdenstion water collection container and send to in the first heating space, a cooling for stills, because the difference in temperature between comdenstion water and the stills this moment, the difference in temperature between relative running water and the stills is far less, consequently, can not form the influence of rapid cooling to the mixed solution in the stills, thereby can make corresponding efficiency obtain the guarantee when follow-up decompression desolventizing.
Drawings
Fig. 1 is a schematic diagram of a synthesis apparatus for chiral ester compounds.
The device comprises a material storage tank A, a metering pump 1, a distillation still 2, a first stirrer 2a, a first condenser 3, a first receiving tank 4, a rectifying still 5, a second stirrer 5a, a second condenser 6, a second receiving tank 7, a first jacket 8, a first heating space 9, a first drain valve 10, a condensed water collecting container 11, a second jacket 12, a second heating space 13, a second drain valve 14, a first valve 15, a second valve 16, a leak detection valve 17, a water supplement valve 18 and a header pipe 19.
Detailed Description
As shown in fig. 1, the synthesis apparatus of chiral ester compound of the present invention comprises a material storage tank a, a metering pump 1, a distillation still 2, a first condenser 3, a first receiving tank 4, a rectifying still 5, a second condenser 6, and a second receiving tank 7, and the following describes each part and the relationship between each part in detail respectively:
the material storage tank a is connected to the metering pump 1, in this embodiment, the material storage tank a and the metering pump 1 are respectively plural, and each material storage tank a is pre-filled with a material, such as dimethyl carbonate and propylene glycol. The output end of the metering pump 1 is connected with the distillation still 2, and the metering pump 1 is used for metering the material input into the distillation still 2 so as to control the material consumption.
The distillation still 2 is provided with a first stirrer 2a, and the substances in the distillation still 2 are stirred by the first stirrer 2 a. Stills 2 is connected with first condenser 3's input, first condenser 3's output is connected with first receiving tank 4's input, first receiving tank 4's output is connected with rectifier 5's input, be equipped with second agitator 5a on rectifier 5, stir the material in rectifier 5 through second agitator 5a, rectifier 5's output is connected with second condenser 6's input, second condenser 6's output and second receiving tank 7 are connected, be equipped with the steam input on stills 2 and the rectifier 5 respectively.
The second receiving tank 7 consists of a front fraction collecting tank and a finished product collecting tank, and the concentration of the distilled fraction is lower and is not in accordance with the requirements of the finished product when the rectifying still 5 is subjected to initial distillation, so that the distilled fraction is firstly discharged into the front fraction collecting tank, a concentration detector is arranged on the front fraction collecting tank, the fraction is detected by the concentration detector, and when the concentration of the fraction reaches a set value, the front fraction collecting tank is closed, and the finished product collecting tank is opened, so that the distilled fraction is discharged into the finished product collecting tank.
The distillation still 2 is provided with a first jacket 8, and a first heating space 9 for accommodating steam is formed between the distillation still 2 and the first jacket 8. The embodiment further comprises a first drain valve 10 and a condensate water collecting container 11 for providing required cooling water for the distillation kettle 2 during temperature reduction, the first drain valve 10 is connected with the first jacket 8, the first drain valve 10 is connected with the condensate water collecting container 11 to control whether condensate water formed in the first heating space 9 is drained into the condensate water collecting container 11, and the output end of the condensate water collecting container 11 is connected with the first jacket 8.
After propylene glycol and dimethyl carbonate are fed into the distillation still 2, sodium acetate is added, stirring is carried out, and the first condenser 3 is started to work. And opening a steam valve connected with the distillation kettle 2, slowly heating to ensure that the temperature in the distillation kettle 2 is increased to 59-62 ℃, distilling out the generated methanol while reacting, then heating to 64 ℃ within 1 hour, then heating from 64 ℃ to 110 ℃, distilling out the solvent at the moment, cooling by a first condenser 3, then feeding into a first receiving tank 4, keeping the solvent distilled out, and slowly increasing the temperature until the reaction is finished. The steam valve connected with the distillation still 2 is closed and the distillation still is cooled.
In this embodiment, what adopt is that slow cooling mode is cooled down stills 2, specifically is: because the steam lets in first heating space 9 after, can form the comdenstion water after the steam gives off the heat, these comdenstion waters are sent to condensate water collection container 11 through first drain valve 10 and are stored in, although the temperature of comdenstion water is less than the temperature of steam, but the temperature is higher than the temperature of normal atmospheric temperature running water, therefore, when needing to cool down stills 2, export the comdenstion water in the comdenstion water collection container 11 and send to in first heating space 9 for the cooling of stills 2, because the temperature difference between comdenstion water and stills 2 at this moment, the temperature difference between relative running water and stills 2 is far less, consequently, can not form the influence of rapid cooling to the mixed solution in stills 2, thereby can make corresponding efficiency obtain the guarantee when follow-up decompression desolventizing. In addition, the condensed water is naturally formed, and the distillation kettle 2 is cooled by the condensed water without being heated additionally, so that the energy conservation is facilitated.
Above-mentioned cooling in-process, get back to during condensate water collecting container 11 to the condensate water after the cooling of stills 2, form circulation cooling route, however, the temperature of the condensate water in condensate water collecting container 11 is less than stills 2's temperature all the time, consequently, circulation cooling makes stills 2's temperature slowly descend, from this, the utility model discloses avoided because of stills 2 in the cooling in-process because of the adverse consequence that the volume of the solvent that the temperature drops rapidly makes follow-up decompression deviate from descends.
The rectifying still 5 is provided with a second jacket 12, a second heating space 13 for containing steam is formed between the rectifying still 5 and the second jacket 12, the rectifying still further comprises a second drain valve 14, the second drain valve 14 is connected with the second jacket 12, and the second drain valve 14 is connected with the condensed water collecting container 11 to control whether condensed water formed in the second heating space 13 is discharged into the condensed water collecting container 11 or not.
Steam is introduced into the second heating space 13, and similarly, condensed water is formed after the steam releases heat, so that more condensed water can be collected in the condensed water collection container 11, and the temperature required for rectification in the rectifying still 5 is slightly higher than that of the rectifying still 2, for example, the steam is introduced into the second heating space 13 to slowly raise the temperature of the rectifying still 5, the distilled finished product is condensed by the second condenser 6 and then output to the second receiving tank 7, and the temperature of the rectifying still 5 does not exceed 125 ℃ in the rectification process until 25 to 30kg of residual materials are left in the rectifying still 5. Therefore, as far as the rectifying still 5 is concerned, more steam is required than the rectifying still 2, so that more condensate water can be produced in the second heating space 13, and the condensate water is output to the condensate water collecting container 11 and used in the subsequent cooling of the rectifying still 2.
The present embodiment further includes a leak detection assembly including a first valve 15, a second valve 16, and a leak detection valve 17, one end of the first valve 15 being connected to the output end of the condensate collecting container 11, and the leak detection valve 17 and the second valve 16 being connected in parallel to the other end of the first valve 15. When the condensed water is drained, the first valve 15 and the second valve 16 are both opened. When not draining, at least the first valve 15 is closed. When it is desired to check the first valve 15 for leaks, the second valve 16 and the first valve 15 are closed, and if the leak detection valve 17 continues to allow water to flow, this indicates that there is a leak in the second drain valve 15.
The device also comprises a water replenishing valve 18 and a header pipe 19, wherein the header pipe 19 is connected with a steam input end on the distillation still 2, and the water replenishing valve 18 and the condensed water collecting container 11 are respectively connected with the header pipe 19. When steam is supplied, the first valve 15 is closed, so that condensate in the condensate collection container 11 cannot enter the first heating space 9. When the temperature of the distillation still 2 needs to be reduced, the steam input is stopped at this time, the first valve 15 and the second valve 16 are opened, and the condensed water collected in the condensed water collection container 11 is input into the first heating space 9 and acts on (for example, sprays) the distillation still 2, so that the temperature of the distillation still 2 is reduced. If the materials need to be cooled rapidly after being emptied, the water replenishing valve 18 is directly opened, and the external cooling water is input into the first heating space 9 together through the header pipe 19, so that the cooling speed can be accelerated.
Claims (4)
1. The synthesis device of the chiral ester compound comprises a material storage tank, a metering pump (1), a distillation kettle (2) and a first condenser (3), the device comprises a first receiving tank (4), a rectifying still (5), a second condenser (6) and a second receiving tank (7), wherein a material storage tank is connected with a metering pump (1), the output end of the metering pump (1) is connected with the rectifying still (2), the rectifying still (2) is connected with the input end of a first condenser (3), the output end of the first condenser (3) is connected with the input end of the first receiving tank (4), the output end of the first receiving tank (4) is connected with the input end of the rectifying still (5), the output end of the rectifying still (5) is connected with the input end of the second condenser (6), the output end of the second condenser (6) is connected with the second receiving tank (7), and steam input ends are respectively arranged on the rectifying still (2) and the rectifying still (5);
the steam distillation device is characterized in that a first jacket (8) is arranged on the distillation kettle (2), and a first heating space (9) for containing steam is formed between the distillation kettle (2) and the first jacket (8);
still include first drain valve (10), for stills (2) provide required cooling water's comdenstion water collection container (11) when the cooling, first drain valve (10) are connected with first cover (8), and first drain valve (10) are connected with comdenstion water collection container (11) and are whether discharged comdenstion water collection container (11) in order to control the comdenstion water that forms in first heating space (9), and comdenstion water collection container (11) output is connected with first cover (8).
2. The apparatus for synthesizing chiral ester compound according to claim 1, wherein the rectifying still (5) is provided with a second jacket (12), and a second heating space (13) for accommodating steam is formed between the rectifying still (5) and the second jacket (12);
the heating device also comprises a second drain valve (14), wherein the second drain valve (14) is connected with the second jacket (12), and the second drain valve (14) is connected with the condensed water collecting container (11) to control whether condensed water formed in the second heating space (13) is drained into the condensed water collecting container (11).
3. The apparatus for synthesizing chiral ester compound according to claim 1, further comprising a leak detection assembly, wherein the leak detection assembly comprises:
one end of the first valve (15) is connected with the output end of the condensed water collecting container (11);
a second valve (16);
and a leak detection valve (17), wherein the leak detection valve (17) and the second valve (16) are connected to the other end of the first valve (15) in parallel.
4. The device for synthesizing the chiral ester compound according to claim 1, further comprising a water replenishing valve (18) and a header pipe (19), wherein the header pipe (19) is connected with a steam input end of the distillation still (2), and the water replenishing valve (18) and the condensed water collecting container (11) are respectively connected with the header pipe (19).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202121046752.3U CN214971828U (en) | 2021-05-14 | 2021-05-14 | Synthesis device of chiral ester compound |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202121046752.3U CN214971828U (en) | 2021-05-14 | 2021-05-14 | Synthesis device of chiral ester compound |
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| CN214971828U true CN214971828U (en) | 2021-12-03 |
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| CN202121046752.3U Active CN214971828U (en) | 2021-05-14 | 2021-05-14 | Synthesis device of chiral ester compound |
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