Separation system for continuously producing di-tert-butyl dicarbonate

Abstract

The utility model belongs to the technical field of di-tert-butyl dicarbonate ester production, and particularly relates to a separation system for continuously producing di-tert-butyl dicarbonate ester, which comprises a phase separation mechanism for washing reactants for phase separation and a separation mechanism for separating materials generated by the phase separation mechanism, the separation mechanism comprises a rectification system for rectifying materials and an impurity removal system for performing solid-liquid separation on impurities in rectified substances generated by the rectification system, the rectification system is mounted between the phase splitting mechanism and the impurity removal system, and the rectification system comprises a rectification tower, a reboiler and a condenser; according to the utility model, the phase splitting mechanism and the separation mechanism are additionally arranged, so that the continuous feeding and discharging of materials can be realized, the material loss caused by batch treatment is reduced, and the treatment capacity is increased.

Description

Technical Field

[0001] The utility model belongs to the technical field of di-tert-butyl dicarbonate production, and specifically relates to a separation system for continuously producing di-tert-butyl dicarbonate. Background Art

[0002] Di-tert-butyl dicarbonate is a reagent widely used in organic synthesis. The synthesis reaction of the production process of this product is carried out in an organic solvent. The material after the reaction needs to go through separation processes such as water washing, phase separation, desolventization and refining to finally obtain a qualified product. The existing separation process adopts intermittent operation, and water washing, phase separation and desolventization are carried out in an intermittent reactor. The operation is labor-intensive, the processing scale is limited, the batch processing time is long, and the product quality is unstable. Utility Model Content

[0003] The utility model aims to provide a separation system for continuously producing di-tert-butyl dicarbonate, so as to solve the problems raised in the above-mentioned background technology.

[0004] To achieve the above-mentioned purpose, the utility model provides the following technical scheme: a separation system for continuously producing di-tert-butyl dicarbonate, comprising: a phase separation mechanism for washing and phase separation of reactants and a separation mechanism for separating materials produced by the phase separation mechanism, the separation mechanism comprising a distillation system for distilling materials and an impurity removal system for solid-liquid separation of impurities in the distillate produced by the distillation system, and the distillation system is installed between the phase separation mechanism and the impurity removal system.

[0005] Preferably, the distillation system comprises a distillation tower, a reboiler and a condenser, a material discharge end is provided at the bottom of the distillation tower, a circulation pump is installed between the material discharge end and the reboiler, one end of the reboiler away from the circulation pump is connected to the distillation tower, the impurity removal system is installed between the reboiler and the circulation pump, and the phase separation mechanism is installed between the reboiler and the distillation tower;

[0006] A gas phase discharge end is provided at the top of the distillation tower, and the condenser is installed on the gas phase discharge end. A reflux tank and a reflux pump are installed in sequence at the end of the condenser away from the distillation tower. A solvent discharge pipe is installed on the distillation tower at the end of the reflux pump away from the reflux tank.

[0007] Preferably, the distillation tower is one of a packed tower and a sieve plate tower.

[0008] Preferably, a gas phase outlet is provided at the top of the reflux tank, and an exhaust pipe is installed at the gas phase outlet, and a vacuum pump is installed on the exhaust pipe.

[0009] Preferably, the vacuum pump is one of a water ring vacuum pump, a screw vacuum pump and a Roots vacuum pump.

[0010] Preferably, the impurity removal system includes two precision filters installed in parallel, and a feed end, a discharge end and an impurity removal end are installed on the precision filters. The feed ends on the two precision filters are connected between the reboiler and the circulation pump, a BOC discharge pipe is connected in parallel between the discharge ends on the two precision filters, and a slag discharge pipe is connected in parallel between the two impurity removal ends.

[0011] Preferably, a detachable filter element is installed in the precision filter.

[0012] Preferably, the precision filter comprises a covering shell and a top cover, a mounting frame is symmetrically installed on the bottom of the top cover, the top end of the filter element is installed between the two mounting frames, a bolt is screwed on the outer side of the mounting frame, one end of the bolt abuts against the filter element, and one end of the BOC discharge pipe extends into the filter element.

[0013] Preferably, the phase separation mechanism comprises a phase separator and a buffer tank which are connected in sequence, a material transfer pump is installed at one end of the buffer tank away from the phase separator, and the material transfer pump is connected between the distillation tower and the reboiler.

[0014] Preferably, a liquid inlet pipe is installed at the top end of the phase separator, and a drain pipe is installed at the bottom end of the phase separator.

[0015] Compared with the prior art, the utility model has the following beneficial effects:

[0016] (1) The utility model can realize continuous feeding and discharging of materials by adding a phase separation mechanism and a separation mechanism, thereby reducing material loss caused by batch processing and increasing processing capacity.

[0017] (2) The utility model adopts a distillation tower for desolventizing by adding a distillation tower and a condenser, thereby improving the purity of the product; at the same time, the distillation tower adopts negative pressure operation to reduce the operating temperature and make production safer.

[0018] (3) The utility model adds an impurity removal system between the reboiler and the circulation pump, and the precision filter can effectively remove impurities in the product. In addition, two units are operated in parallel, which can realize online switching to remove impurities.

[0019] (4) The utility model adds a mounting frame and bolts in the housing, and the filter element can be detachably mounted on the top cover through the bolts and the mounting frame, so that the filter element can be easily replaced. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a schematic diagram of the structure of the utility model;

[0021] Figure 2 It is a cross-sectional view of the precision filter of the utility model;

[0022] Figure 3 for Figure 2 Enlarged view of point A in the middle;

[0023] Figure 4 It is a top view of the mounting frame and the filter element of the utility model;

[0024] In the figure: 1. Phase separator; 2. Buffer tank; 3. Transfer pump; 4. Distillation tower; 5. Reboiler; 6. Circulation pump; 7. Condenser; 8. Reflux tank; 9. Reflux pump; 10. Precision filter; 11. Slag discharge pipe; 12. Vacuum pump; 13. Liquid inlet pipe; 14. Drain pipe; 15. Solvent discharge pipe; 16. Exhaust pipe; 17. BOC discharge pipe; 18. Filter element; 19. Mounting bracket; 20. Bolts. DETAILED DESCRIPTION

[0025] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0026] refer to Figure 1 As shown, the utility model provides a separation system for continuously producing di-tert-butyl dicarbonate, comprising: a phase separation mechanism for washing and phase separation of reactants and a separation mechanism for separating materials produced by the phase separation mechanism.

[0027] In the present utility model, combined with Figure 1 As shown, the separation mechanism of this embodiment includes a distillation system for distilling materials and an impurity removal system for solid-liquid separation of impurities in the distillate produced by the distillation system. The distillation system is installed between the phase separation mechanism and the impurity removal system.

[0028] refer to Figure 1 As shown, the phase separation mechanism includes a phase separator 1 and a buffer tank 2 which are connected in sequence. A material transfer pump 3 is installed at one end of the buffer tank 2 away from the phase separator 1 . The material transfer pump 3 is connected between the distillation tower 4 and the reboiler 5 .

[0029] refer to Figure 1 As shown, a liquid inlet pipe 13 is installed at the top end of the phase separator 1, and a drain pipe 14 is installed at the bottom end of the phase separator 1.

[0030] As mentioned above, when using the phase separation mechanism provided by the utility model, the phase separation mechanism introduces the external reaction water wash liquid into the phase separator 1 through the liquid inlet pipe 13 for phase separation, and the generated waste water is discharged from the phase separator 1 through the drain pipe 14. The material after phase separation enters the buffer tank 2 for storage. Under the action of the material transfer pump 3, the material in the buffer tank 2 is introduced into the distillation system, and the material is separated and processed by the distillation system.

[0031] In the present utility model, combined with Figure 1 As shown, the distillation system of this embodiment includes a distillation tower 4, a reboiler 5 and a condenser 7. A material discharge end is provided at the bottom of the distillation tower 4. A circulating pump 6 is installed between the material discharge end and the reboiler 5. One end of the reboiler 5 away from the circulating pump 6 is connected to the distillation tower 4. The impurity removal system is installed between the reboiler 5 and the circulating pump 6. The phase separation mechanism is installed between the reboiler 5 and the distillation tower 4.

[0032] A gas phase discharge end is provided at the top of the distillation tower 4, and a condenser 7 is installed on the gas phase discharge end. A reflux tank 8 and a reflux pump 9 are installed in sequence on the end of the condenser 7 away from the distillation tower 4. A solvent discharge pipe 15 is installed on the distillation tower 4, which is away from the reflux tank 8 and the reflux pump 9.

[0033] Combination Figure 1 As shown, a gas phase outlet is provided at the top of the reflux tank 8 , and an exhaust pipe 16 is installed at the gas phase outlet, and a vacuum pump 12 is installed on the exhaust pipe 16 .

[0034] As mentioned above, when using the distillation system provided by the utility model, the material enters the distillation tower 4 after phase separation through the phase separation mechanism, and the generated liquid material enters the reboiler 5 or the impurity removal system through the circulation pump 6. Part of the liquid material is treated with impurities by the impurity removal system, and part of the liquid material enters the distillation tower 4 again through the reboiler 5 for circulation. The gas enters the condenser 7 through the gas phase discharge end of the reflux pump 9 and is liquefied and then collected through the reflux tank 8. At the same time, the solvent generated in the distillation tower 4 and the liquefied liquid are discharged through the solvent discharge pipe 15, and the condensed gas in the reflux tank 8 is collected through the exhaust pipe 16 by the vacuum pump 12.

[0035] Further, in order to better distill the material, refer to Figure 1 As shown, the distillation tower 4 is a kind of a packed tower and a sieve plate tower. The distillation tower 4 can be a packed tower and a sieve plate tower, which increases the selection range of the distillation tower 4, thereby improving the adaptability of the equipment and facilitating its use in different working conditions.

[0036] Furthermore, in order to better discharge the residual gas, refer to Figure 1As shown, the vacuum pump 12 is a water ring vacuum pump, a screw vacuum pump and a Roots vacuum pump. The vacuum pump 12 can be a water ring vacuum pump, a screw vacuum pump and a Roots vacuum pump, which increases the selection range of the vacuum pump 12, thereby improving the adaptability of the equipment and facilitating use in different working conditions.

[0037] In the present utility model, combined with Figure 1 As shown, the impurity removal system of this embodiment includes two precision filters 10 installed in parallel, and a feed end, a discharge end and an impurity removal end are installed on the precision filter 10. The feed ends of the two precision filters 10 are connected between the reboiler 5 and the circulation pump 6, a BOC discharge pipe 17 is connected in parallel between the discharge ends of the two precision filters 10, and a slag discharge pipe 11 is connected in parallel between the two impurity removal ends.

[0038] Combination Figure 3 As shown, a detachable filter element 18 is installed in the precision filter 10.

[0039] As mentioned above, when using the impurity removal system provided by the utility model, part of the BOC material after distillation enters the two precision filters 10 through the circulation pump 6, and the impurities in the BOC material are filtered through the filter element 18 in the precision filter 10, and the pure BOC is discharged and collected through the BOC discharge pipe 17, and the filtered impurities are discharged through the slag discharge pipe 11. Two precision filters 10 are operated in parallel, which can realize online switching to remove impurities. A valve is provided at the feed end of the precision filter 10, and the valve is not drawn in the figure. By switching the valve on and off, the BOC material can enter the two precision filters 10 at the same time or only enter one precision filter 10 at a time. When the BOC material enters only one precision filter 10, the other precision filter 10 can be decontaminated. When the BOC material enters two precision filters 10 at the same time, the filtration efficiency of the BOC material can be improved.

[0040] Further, in order to facilitate the replacement of the filter element 18, refer to Figure 2-4As shown, the precision filter 10 includes a housing and a top cover that are covered, and a mounting frame 19 is symmetrically installed at the bottom of the top cover. The top end of the filter element 18 is installed between the two mounting frames 19. A bolt 20 is screwed on the outer side of the mounting frame 19, and one end of the bolt 20 abuts on the filter element 18. One end of the BOC discharge pipe 17 extends into the filter element 18. When the filter element 18 needs to be replaced, the top cover is removed from the housing, and the bolt 20 on the mounting frame 19 is screwed outward, so as to release the limit of the bolt 20 on the filter element 18, thereby facilitating the removal of the filter element 18 from between the two mounting frames 19. After replacing a new filter element 18, the bolt 20 on the mounting frame 19 is tightened, so that one end of the bolt 20 abuts on the filter element 18, thereby limiting the filter element 18 between the two mounting frames 19. At this time, one end of the BOC discharge pipe 17 is in the filter element 18.

[0041] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A separation system for continuously producing di-tert-butyl dicarbonate, characterized in that: include: A phase separation mechanism for washing and phase separation of reactants and a separation mechanism for separating materials produced by the phase separation mechanism, the separation mechanism includes a distillation system for distilling materials and an impurity removal system for solid-liquid separation of impurities in the distillate produced by the distillation system, and the distillation system is installed between the phase separation mechanism and the impurity removal system.

2. The separation system according to claim 1, characterized in that: The distillation system comprises a distillation tower (4), a reboiler (5) and a condenser (7); a material discharge end is provided at the bottom of the distillation tower (4); a circulation pump (6) is installed between the material discharge end and the reboiler (5); an end of the reboiler (5) away from the circulation pump (6) is connected to the distillation tower (4); the impurity removal system is installed between the reboiler (5) and the circulation pump (6); and the phase separation mechanism is installed between the reboiler (5) and the distillation tower (4); The top of the distillation tower (4) is provided with a gas phase discharge end, the condenser (7) is installed on the gas phase discharge end, the end of the condenser (7) facing away from the distillation tower (4) is successively provided with a reflux tank (8) and a reflux pump (9), and the distillation tower (4) is provided with a solvent discharge pipe (15) at the end of the reflux pump (9) facing away from the reflux tank (8).

3. The separation system according to claim 2, characterized in that: The distillation tower (4) is a type of a packed tower and a sieve plate tower.

4. The separation system according to claim 2, characterized in that: The top of the reflux tank (8) is provided with a gas phase outlet, and the gas phase outlet is installed with an exhaust pipe (16), and the exhaust pipe (16) is installed with a vacuum pump (12).

5. The separation system according to claim 4, characterized in that: The vacuum pump (12) is a water ring vacuum pump, a screw vacuum pump and a Roots vacuum pump.

6. A separation system for continuous production of di-tert-butyl dicarbonate according to claim 2, characterized in that: The impurity removal system comprises two precision filters (10) installed in parallel, wherein a feed end, a discharge end and an impurity removal end are installed on the precision filters (10), the feed ends on the two precision filters (10) are connected between the reboiler (5) and the circulation pump (6), a BOC discharge pipe (17) is connected in parallel between the discharge ends on the two precision filters (10), and a slag discharge pipe (11) is connected in parallel between the two impurity removal ends.

7. A separation system for continuous production of di-tert-butyl dicarbonate according to claim 6, characterized in that: A detachable filter element (18) is installed in the precision filter (10).

8. A separation system for continuous production of di-tert-butyl dicarbonate according to claim 7, characterized in that: The precision filter (10) comprises a housing and a top cover which are covered together, a mounting frame (19) being symmetrically mounted on the bottom of the top cover, the top end of the filter element (18) being mounted between the two mounting frames (19), a bolt (20) being screwed onto the outer side of the mounting frame (19), one end of the bolt (20) being abutted against the filter element (18), and one end of the BOC discharge pipe (17) extending into the filter element (18).

9. A separation system for continuous production of di-tert-butyl dicarbonate according to claim 2, characterized in that: The phase separation mechanism comprises a phase separator (1) and a buffer tank (2) connected in sequence, wherein a material transfer pump (3) is installed at one end of the buffer tank (2) away from the phase separator (1), and the material transfer pump (3) is connected between a distillation tower (4) and a reboiler (5).

10. A separation system for continuous production of di-tert-butyl dicarbonate according to claim 9, characterized in that: A liquid inlet pipe (13) is installed at the top end of the phase separator (1), and a drain pipe (14) is installed at the bottom end of the phase separator (1).

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