CN215901728U - Di-tert-butyl dicarbonate synthesizer based on acyl chloride or sulfonyl chloride method - Google Patents
Di-tert-butyl dicarbonate synthesizer based on acyl chloride or sulfonyl chloride method Download PDFInfo
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- CN215901728U CN215901728U CN202122147393.7U CN202122147393U CN215901728U CN 215901728 U CN215901728 U CN 215901728U CN 202122147393 U CN202122147393 U CN 202122147393U CN 215901728 U CN215901728 U CN 215901728U
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Abstract
The utility model discloses a di-tert-butyl dicarbonate synthesis device based on an acyl chloride or sulfonyl chloride method, which comprises a first reaction kettle, a second reaction kettle, a centrifugal machine, a flash evaporation kettle, a scraper evaporator, a circulating pump, a condenser, a solvent receiving tank and a product receiving tank. According to the utility model, the scraper evaporator is connected between the feed inlet and the discharge outlet of the flash evaporation kettle, so that the product is quickly distilled, the high-temperature decomposition of di-tert-butyl dicarbonate is reduced, and the product yield is improved; make solvent receiving tank bottom connect first reation kettle and batching jar through setting up the pipeline, realize that the realization manifold cycles of solvent is returned and is overlapped and use.
Description
Technical Field
The utility model belongs to the technical field of production of di-tert-butyl dicarbonate, and particularly relates to a di-tert-butyl dicarbonate synthesis device based on an acyl chloride or sulfonyl chloride method.
Background
Di-tert-butyl dicarbonate as amino protective agent is widely used in organic synthesis of chemical industry, medicine, pesticide and the like. The prior industrial preparation method of di-tert-butyl dicarbonate mainly comprises phosgene, diphosphine and triphosgene methods, and the diphosphine and triphosgene methods are synthesized after being decomposed into phosgene essentially, and the use of phosgene is limited by China due to the severe toxicity of phosgene.
To comply with national policy requirements, liquid acid chloride or sulfonyl chloride reagents are used instead of the above-described methods. However, in the currently used di-tert-butyl dicarbonate production device, after the di-tert-butyl dicarbonate product is synthesized, the product enters a tower to be crystallized, so that the di-tert-butyl dicarbonate is easy to decompose at high temperature, and the product yield is reduced.
Disclosure of Invention
In order to solve the defects in the prior art, the utility model provides a synthesis device of di-tert-butyl dicarbonate based on an acyl chloride or sulfonyl chloride method, which solves the problem that the high-temperature decomposition of the di-tert-butyl dicarbonate is easy to occur in the existing synthesis device, so that the product yield is reduced.
In order to solve the technical problems, the utility model adopts the following technical scheme:
a di-tert-butyl dicarbonate synthesis device based on an acyl chloride or sulfonyl chloride method comprises a first reaction kettle, a second reaction kettle, a centrifuge, a flash evaporation kettle, a scraper evaporator, a circulating pump, a condenser, a solvent receiving tank and a product receiving tank; the first reaction kettle, the second reaction kettle, the centrifuge, the flash evaporation kettle, the scraper evaporator, the condenser and the solvent receiving tank are respectively provided with a feed inlet and a discharge outlet, and the first reaction kettle is also provided with an air inlet; the feed inlet of the second reaction kettle is respectively connected with the discharge outlet of the first reaction kettle and the discharge outlet of the liquid preparation tank, and the discharge outlet of the second reaction kettle is connected with the feed inlet of the centrifuge; the discharge hole of the centrifuge comprises a centrifuge filter cake discharge hole and a centrifugate discharge hole; the centrifugal liquid discharge port is connected with the feed port of the flash evaporation kettle; two discharge ports are arranged on the scraper evaporator, the discharge ports of the flash evaporation kettle are connected with the feed port of the scraper evaporator, one discharge port of the scraper evaporator is connected with the feed port of the flash evaporation kettle, and the other discharge port of the scraper evaporator is connected with the feed port of the condenser; the circulating pump is arranged on a pipeline between the discharge hole of the flash evaporation kettle and the feed inlet of the scraper evaporator; and a discharge hole of the condenser is respectively connected with a feed inlet of the solvent receiving tank and a feed inlet of the product receiving tank.
Preferably, two discharge gates of the scraper evaporator are respectively arranged at the top and the bottom of the scraper evaporator, a feed inlet of the scraper evaporator is arranged at the top of the scraper evaporator, a feed inlet of the scraper evaporator is connected with a discharge gate arranged at the bottom of the flash evaporation kettle, a discharge gate at the bottom of the scraper evaporator is connected with a feed inlet arranged at the top of the flash evaporation kettle, and a discharge gate at the top of the scraper evaporator is connected with a feed inlet of the condenser.
Preferably, the discharge port of the solvent receiving tank is respectively connected with the feed port of the first reaction kettle and the feed port of the liquid preparation tank.
Preferably, the air inlet of the first reaction kettle is arranged at the bottom of the first reaction kettle.
Preferably, the air inlet of the first reaction kettle coincides with the liquid outlet of the first reaction kettle, and the air inlet pipeline is sleeved in the discharge pipeline of the first reaction kettle.
Further, the device also comprises a liquid preparation tank for bearing the acyl chloride/sulfonyl chloride reagent, wherein a discharge hole of the liquid preparation tank is connected with a feed hole of the second reaction kettle, and the feed hole of the liquid preparation tank is connected with a discharge hole of the solvent receiving tank.
Compared with the prior art, the utility model has the beneficial effects that:
the synthesis device can realize the rapid distillation of the product, reduce the high-temperature decomposition of the di-tert-butyl dicarbonate and improve the product yield;
the bottom of the solvent receiving tank is connected with the first reaction kettle and the batching tank through a pipeline, so that the solvent can be recycled for multiple times;
the bottom of the first reaction kettle is provided with a carbon dioxide inlet, so that carbon dioxide enters the first reaction kettle from the bottom, the utilization efficiency of the carbon dioxide can be improved, and the reaction time can be shortened;
the device is simple, easy to implement, safe and reliable, and production halt caused by phosgene limited use is avoided.
Other advantages of the utility model are detailed in the detailed description of the embodiments.
Drawings
FIG. 1 is a schematic view of a synthesis apparatus according to an embodiment of the present invention, in which the direction of arrows indicates the flow direction of materials or gases.
The various reference numbers in the figures illustrate:
1-a first reaction kettle, 2-a second reaction kettle, 3-a liquid preparation tank, 4-a centrifuge, 5-a flash evaporation kettle, 6-a scraper evaporator, 7-a circulating pump, 8-a condenser, 9-a solvent receiving tank, 10-a product receiving tank, 11-an air inlet pipeline, 12-a discharge pipeline and 13-a product filling room;
(4-1) -a centrifugal filter cake discharge port, and (4-2) -a centrifugal liquid discharge port.
Detailed Description
Specific examples of the present invention are given below. It should be noted that, in the following description, unless explicitly stated or limited otherwise, terms such as "disposed" and "connected" are to be understood broadly, and may be, for example, fixedly connected, detachably connected, or integrated; either a direct connection or an indirect connection, and the like. The specific meaning of the above terms in the present technical solution can be understood by those of ordinary skill in the art according to specific situations.
In the present invention, unless otherwise specified, the use of the terms of orientation such as "upper" and "lower" generally means that they are defined with reference to the drawing plane of the corresponding drawing, and "inner" and "outer" means that they are defined with reference to the outline of the corresponding drawing.
The individual features described in the following embodiments can be combined in any suitable manner without departing from the inventive idea, which should also be regarded as disclosed in the present application.
The utility model discloses a synthesis device of di-tert-butyl dicarbonate based on an acyl chloride or sulfonyl chloride method in a specific embodiment, as shown in fig. 1, the synthesis device of the embodiment comprises a first reaction kettle 1, a second reaction kettle 2, a centrifuge 4, a flash evaporation kettle 5, a scraper evaporator 6, a circulating pump 7, a condenser 8, a solvent receiving tank 9 and a product receiving tank 10.
The first reaction kettle 1 is used for reacting sodium tert-butoxide with carbon dioxide to generate reaction liquid, and the second reaction kettle 2 is used for reacting acyl chloride/sulfonyl chloride with the reaction liquid to generate materials. The first reaction kettle 1, the second reaction kettle 2, the centrifuge 4, the flash evaporation kettle 5, the scraper evaporator 6, the condenser 8 and the solvent receiving tank 9 are respectively provided with a feeding hole and a discharging hole.
In addition, the first reaction kettle 1 is also provided with an air inlet, preferably, the air inlet of the first reaction kettle 1 is arranged at the bottom of the first reaction kettle 1, so that the utilization efficiency of carbon dioxide is improved.
In this embodiment, the respective discharge ports of the first reaction kettle 1, the second reaction kettle 2, the liquid preparation tank 3, the centrifuge 4, the flash evaporation kettle 5 and the condenser 8 are all arranged at the bottom, the feed ports are arranged at the top, and two feed ports are arranged at the 5 feed ports of the flash evaporation kettle.
Because the air inlet and the discharge gate of first reation kettle 1 all set up in the bottom, consequently with the air inlet of first reation kettle 1 and the coincidence of first reation kettle 1's liquid outlet, establish inlet duct 11 cover in first reation kettle 1 discharge pipeline, because inlet duct 11 diameter is less, in one end directly inserts first reation kettle 1 through first reation kettle's discharge pipeline 12, the other end is connected with the air supply, it can to set up an opening in first reation kettle 1 bottom like this.
The feed inlet of the second reaction kettle 2 is respectively connected with the discharge outlet of the first reaction kettle 1 and the discharge outlet of the liquid preparation tank 3, and the discharge outlet of the second reaction kettle 2 is connected with the feed inlet of the centrifuge 4.
The discharge port of the centrifuge 4 comprises a centrifuge filter cake discharge port 4-1 and a centrifugate discharge port 4-2, and the centrifugate discharge port 4-2 is connected with the feed port of the flash evaporation kettle 5. A control valve is arranged at the position of the centrifugal filter cake discharge port 401 and used for taking out the centrifugal filter cake.
The discharge port of the flash evaporation kettle 5 is connected with the feed port of the scraper evaporator 6, two discharge ports are arranged on the scraper evaporator 6, one discharge port of the scraper evaporator 6 is connected with the feed port of the flash evaporation kettle 5, and the other discharge port of the scraper evaporator 6 is connected with the feed port of the condenser 8. Circulating pump 7 sets up on the pipeline between flash distillation cauldron 5's discharge gate and scraper evaporator 6's feed inlet, and like this, scraper evaporator 6 forms circulation evaporation return circuit with flash distillation cauldron 5, and the material in flash distillation cauldron 5 can realize the quick distillation of material through circulation circuit circulation evaporation.
Preferably, two discharge gates of the scraper evaporator 6 are respectively arranged at the top and the bottom of the scraper evaporator 6, a feed inlet of the scraper evaporator 6 is arranged at the top of the scraper evaporator 6, a feed inlet of the scraper evaporator 6 is connected with a discharge gate arranged at the bottom of the flash evaporation kettle 5, a discharge gate at the bottom of the scraper evaporator 6 is connected with a feed inlet arranged at the top of the flash evaporation kettle 5, a discharge gate at the top of the scraper evaporator 6 is connected with a feed inlet of the condenser 8, so that the whole distillation heat exchange area can be improved, the distillation efficiency is increased, the distillation time is shortened, and the distillation loss of di-tert-butyl dicarbonate is further reduced.
The discharge hole of the condenser 8 is respectively connected with the feed inlet of the solvent receiving tank 9 and the feed inlet of the product receiving tank 10. In order to realize the recovery of the solvent, the discharge hole of the solvent receiving tank 9 is connected with the feed inlet of the first reaction kettle 1, so that the recovered solvent can enter the first reaction kettle 1 again, and the solvent can be recycled.
The pipeline between any two devices of this embodiment all is provided with the valve for opening and closing of control pipeline.
In addition, this embodiment can also set up pressure sensor, temperature sensor etc. in flash distillation cauldron 5 for detect pressure and temperature in flash distillation cauldron 5.
As another alternative embodiment of the utility model, on the basis of the above-mentioned device, a solution preparation tank 3 is also provided for carrying acyl chloride/sulfonyl chloride reagent. The liquid preparation tank 3 is provided with a feed inlet and a discharge outlet which are respectively positioned at the top and the bottom of the liquid preparation tank 3. More preferably, the discharge port of the solvent receiving tank 9 is connected with the feed port of the dosing tank 3, and the recovered solvent can enter the dosing tank 3. In this embodiment, the flow direction of the solvent in the solvent receiving tank 9, i.e. into the first reaction vessel 1 or the dispensing tank 3, is controlled by setting a valve.
The reaction kettle, the centrifuge 4, the flash evaporation kettle 5, the scraper evaporator 6 and the condenser of the embodiment of the utility model are all common equipment on the market and can be obtained through the market.
The process of synthesizing materials using the synthesis apparatus of the present invention is given below:
adding sodium tert-butoxide and a solvent which participate in the reaction into the first reaction kettle 1 in proportion, and reacting at-20-0 ℃ for 2-6 hours by introducing carbon dioxide;
transferring the reaction liquid in the first reaction kettle 1 into a second reaction kettle 2, transferring the acyl chloride/sulfonyl chloride reagent prepared in advance in the liquid preparation tank 3 into the first reaction kettle 2, and reacting for 3-6 hours at 0-20 ℃;
after the reaction is finished, transferring the materials in the second reaction kettle 2 into a centrifuge 4, discharging a centrifugal filter cake through a centrifugal filter cake discharge port 4-1 for temporary storage, transferring the centrifugal liquid into a flash evaporation kettle 5 through a centrifugal liquid discharge port 4-2, and circularly evaporating the materials in the flash evaporation kettle 5 at 40-100 ℃ and-80-99 kpa through a scraper evaporator 6;
the evaporated material is condensed by a condenser 8, the solvent enters a solvent receiving tank 9, then the solvent returns to the first reaction kettle 1 and the batching tank 3, the product enters a product receiving tank 10, and then the product is transferred into a product filling room 13 for filling.
Claims (6)
1. A di-tert-butyl dicarbonate synthesis device based on an acyl chloride or sulfonyl chloride method is characterized by comprising a first reaction kettle (1), a second reaction kettle (2), a centrifuge (4), a flash evaporation kettle (5), a scraper evaporator (6), a circulating pump (7), a condenser (8), a solvent receiving tank (9) and a product receiving tank (10); the first reaction kettle (1), the second reaction kettle (2), the centrifuge (4), the flash evaporation kettle (5), the scraper evaporator (6), the condenser (8) and the solvent receiving tank (9) are respectively provided with a feed inlet and a discharge outlet, and the first reaction kettle (1) is also provided with an air inlet;
a feed port of the second reaction kettle (2) is respectively connected with a discharge port of the first reaction kettle (1) and a discharge port of the liquid preparation tank (3), and a discharge port of the second reaction kettle (2) is connected with a feed port of the centrifugal machine (4);
the discharge hole of the centrifuge (4) comprises a centrifuge cake discharge hole (4-1) and a centrifugate discharge hole (4-2); the centrifugal liquid discharge port (4-2) is connected with a feed port of the flash evaporation kettle (5);
two discharge ports are arranged on the scraper evaporator (6), the discharge port of the flash evaporation kettle (5) is connected with the feed port of the scraper evaporator (6), one discharge port of the scraper evaporator (6) is connected with the feed port of the flash evaporation kettle (5), and the other discharge port of the scraper evaporator (6) is connected with the feed port of the condenser (8); the circulating pump (7) is arranged on a pipeline between the discharge hole of the flash evaporation kettle (5) and the feed inlet of the scraper evaporator (6);
and a discharge hole of the condenser (8) is respectively connected with a feed inlet of the solvent receiving tank (9) and a feed inlet of the product receiving tank (10).
2. The synthesis device of di-tert-butyl dicarbonate for acyl chloride or sulfonyl chloride processes according to claim 1, wherein the two discharge ports of the scraper evaporator (6) are respectively arranged at the top and the bottom of the scraper evaporator (6), the feed port of the scraper evaporator (6) is arranged at the top of the scraper evaporator (6), the feed port of the scraper evaporator (6) is connected with the discharge port arranged at the bottom of the flash evaporation kettle (5), the discharge port at the bottom of the scraper evaporator (6) is connected with the feed port arranged at the top of the flash evaporation kettle (5), and the discharge port at the top of the scraper evaporator (6) is connected with the feed port of the condenser (8).
3. The apparatus for synthesizing di-tert-butyl dicarbonate by using an acid chloride or sulfonyl chloride process according to claim 1, wherein the discharge ports of the solvent receiving tank (9) are respectively connected with the feed ports of the first reaction vessel (1).
4. The apparatus for synthesizing di-tert-butyl dicarbonate by the acid chloride or sulfonyl chloride process according to claim 1, wherein the gas inlet of the first reaction vessel (1) is disposed at the bottom of the first reaction vessel (1).
5. The synthesis apparatus of di-tert-butyl dicarbonate by acyl chloride or sulfonyl chloride method according to claim 1, wherein the gas inlet of the first reaction vessel (1) coincides with the liquid outlet of the first reaction vessel (1), and the gas inlet pipeline (11) is sleeved in the discharge pipeline of the first reaction vessel (1).
6. The synthesis device of di-tert-butyl dicarbonate for acyl chloride or sulfonyl chloride process according to claim 1, further comprising a liquid preparation tank (3) for carrying acyl chloride/sulfonyl chloride reagent, wherein the discharge port of the liquid preparation tank (3) is connected with the feed port of the second reaction vessel (2), and the feed port of the liquid preparation tank (3) is connected with the discharge port of the solvent receiving tank (9).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122147393.7U CN215901728U (en) | 2021-09-07 | 2021-09-07 | Di-tert-butyl dicarbonate synthesizer based on acyl chloride or sulfonyl chloride method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122147393.7U CN215901728U (en) | 2021-09-07 | 2021-09-07 | Di-tert-butyl dicarbonate synthesizer based on acyl chloride or sulfonyl chloride method |
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| CN215901728U true CN215901728U (en) | 2022-02-25 |
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| CN202122147393.7U Active CN215901728U (en) | 2021-09-07 | 2021-09-07 | Di-tert-butyl dicarbonate synthesizer based on acyl chloride or sulfonyl chloride method |
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