Chiral alcohol ester ring-opening reaction system

Abstract

The utility model discloses a chiral alcohol ester ring-opening reaction system, comprising a chiral alcohol ester synthesis unit, a chiral alcohol ester mixing unit, and a ring-opening product reaction unit, wherein the output end of the chiral alcohol ester synthesis unit is connected to the input end of the chiral alcohol ester mixing unit, and the output end of the chiral alcohol ester mixing unit is connected to the ring-opening product reaction unit. The utility model can prepare chiral binary or polyvalent alcohol ester products.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical engineering, in particular to a chiral alcohol ester ring-opening reaction system. Background Art

[0002] Chiral propylene carbonate is a pharmaceutical intermediate, mainly used in the synthesis of the best-selling anti-AIDS and hepatitis B virus drug tenofovir disoproxil. The methods for preparing chiral propylene carbonate include: transesterification method, carbon dioxide synthesis method, etc. The reactor is one of the essential equipment for the production of chiral propylene carbonate.

[0003] The chiral propylene carbonate synthesis device currently in use includes a material storage tank, a metering pump, a reactor, an ethanol receiving tank, a finished product receiving tank and pipelines connecting the above components. The material storage tanks are arranged in parallel on one side of the reactor, and the ethanol receiving tank and the finished product receiving tank are connected by a main pipeline and arranged on the other side of the reactor, wherein: an integrated reaction distillation tower is arranged on the main pipeline connecting the reactor with the ethanol receiving tank and the finished product receiving tank, and the integrated reaction distillation tower consists of a distillation tower and a reflux condenser arranged on the distillation tower.

[0004] Chiral propylene carbonate is only a pharmaceutical intermediate. Therefore, if it needs to be made into a drug, it needs to be further processed. The above-mentioned synthesis device is only suitable for the synthesis of chiral propylene carbonate. Therefore, the above-mentioned synthesis device needs to be optimized. Utility Model Content

[0005] The utility model provides a chiral alcohol ester ring-opening reaction system. The utility model can prepare chiral dibasic or polybasic alcohol ester products.

[0006] The technical solutions to the above technical problems are as follows:

[0007] The chiral alcohol ester ring-opening reaction system comprises a chiral alcohol ester synthesis unit, a chiral alcohol ester mixing unit and a ring-opening product reaction unit. The output end of the chiral alcohol ester synthesis unit is connected to the input end of the chiral alcohol ester mixing unit, and the output end of the chiral alcohol ester mixing unit is connected to the ring-opening product reaction unit.

[0008] Furthermore, the chiral alcohol ester synthesis unit includes a cyclization distillation kettle, a first jacket, a first condenser, a first receiving tank, a first vacuum assembly, a first steam input assembly, and a first steam output assembly. The distillation kettle is provided with a first feeding port, a first vacuum port, and a first output port. The first jacket is installed on the outside of the cyclization distillation kettle to form a first spacing space between the cyclization distillation kettle and the first jacket. The first jacket is provided with a first steam input port and a first steam output port. The first steam input assembly is connected to the first steam input port, the first steam output assembly is connected to the first steam output port, the first vacuum port is connected to the first vacuum assembly, the first output port is connected to the input end of the first condenser, and the output end of the first condenser is connected to the first receiving tank.

[0009] Furthermore, the chiral alcohol ester mixing unit includes a first container, a first valve, a mixing tank, a second valve, and a second container. The first container is connected to the output end of the chiral alcohol ester synthesis unit, one end of the first valve is connected to the first container, the other end of the first valve is connected to the mixing tank, the mixing tank is connected to the other end of the second valve, the other end of the second valve is connected to the second container, and the second container is connected to the open-ring reaction unit.

[0010] Furthermore, the chiral alcohol ester mixing unit also includes a third valve and a first tail gas absorption component. One end of the third valve is connected to the mixing tank, and the other end of the third valve is connected to the first tail gas absorption component.

[0011] Furthermore, the open-loop reaction unit includes a third container, a delivery pump, a reactor, a second jacket, a second steam input component, a second steam output component, a second condenser, and a second receiving tank. The third container is connected to the delivery pump, the reactor is provided with a second feeding port and a second output port, the output end of the delivery pump is connected to the second feeding port, the second jacket is arranged on the outside of the reactor, and a second interval space is formed between the reactor and the second jacket, the second jacket is provided with a first port and a second port, the second steam input component is connected to the first port, the second steam output component is connected to the second port, the second output port is connected to the second condenser, and the second condenser is connected to the second receiving tank.

[0012] Further, the open-loop reaction unit also includes a refrigerant input control component and a refrigerant output control component, the refrigerant input control component includes a refrigerant supply unit, a first ball valve, a first pneumatic control valve, the refrigerant supply unit is connected to one end of the first ball valve, the other end of the first ball valve is connected to one end of the first pneumatic control valve, and the other end of the first pneumatic control valve is connected to the first port;

[0013] The refrigerant output control assembly includes a second pneumatic control valve, a second ball valve, and a refrigerant recovery unit. One end of the second pneumatic control valve is connected to the second port, the other end of the second pneumatic control valve is connected to one end of the second ball valve, and the other end of the second ball valve is connected to the refrigerant recovery unit.

[0014] The utility model adds a chiral alcohol ester mixing unit and a ring-opening product reaction unit on the basis of a chiral alcohol ester synthesis unit; the chiral alcohol ester synthesized is mixed by the chiral alcohol ester mixing unit to make the concentration of the chiral alcohol ester uniform; the chiral alcohol ester and the raw material are reacted by the ring-opening product reaction unit, and distillation is performed to obtain a ring-opening chiral alcohol ester product. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a schematic diagram of the chiral alcohol ester ring-opening reaction system of the utility model.

[0016] Figure 2 for Figure 1 Enlarged view of part A in .

[0017] Figure 3 for Figure 1 Enlarged view of part B in .

[0018] Figure 4 for Figure 1 Enlarged view of section C in .

[0019] Figure 5 for Figure 4 Enlarged view of the Q section in .

[0020] Markings in the attached drawings:

[0021] Chiral alcohol ester synthesis unit A, cyclization distillation kettle 1, first feeding port 1a, first vacuum port 1b, first output port 1c, first jacket 2, first partition space 2a, first steam input port 2b, first condenser 3, first receiving tank 4, first vacuum assembly 5, first steam input assembly 6, first steam output assembly 7.

[0022] Chiral alcohol ester mixing unit B, first container 8, first valve 9, mixing tank 10, second valve 11, second container 12, third valve 13, first tail gas absorption component VT1.

[0023] Open-loop reaction unit C, third container 14, delivery pump 15, reactor 16, second feed port 16a, second output port 16b, second air extraction port 16c, second air extraction assembly 16d, discharge valve 16e, second jacket 17, second partition space 17a, first port 17b, second port 17c, second steam input assembly 18, second steam output assembly 19, second condenser 20, second receiving tank 21, refrigerant supply unit CWS, first ball valve 22, first pneumatic control valve 23, second pneumatic control valve 24, second ball valve 25, refrigerant recovery unit CWR, fourth valve 26, fifth valve 27, process gas supply unit 28, recovery container 29. DETAILED DESCRIPTION

[0024] The utility model is further described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0025] First of all, it should be explained that the described embodiments are merely embodiments derived from the explanation of the drawings, and are not all embodiments of the present utility model. As for the directional words used, such as "upper end" and "lower end", they are merely further explanations of the drawings, rather than limitations on the present utility model.

[0026] like Figures 1 to 5 The chiral alcohol ester ring-opening reaction system of the utility model comprises a chiral alcohol ester synthesis unit A, a chiral alcohol ester mixing unit B, and a ring-opening product reaction unit C. The output end of the chiral alcohol ester synthesis unit A is connected to the input end of the chiral alcohol ester mixing unit B, and the output end of the chiral alcohol ester mixing unit B is connected to the ring-opening product reaction unit C.

[0027] The chiral alcohol ester synthesis unit A comprises a cyclization still 1, a first jacket 2, a first condenser 3, a first receiving tank 4, a first vacuum assembly 5, a first steam input assembly 6, and a first steam output assembly 7. The still 1 is provided with a first feeding port 1a, a first vacuum port 1b, and a first output port 1c. The first jacket 2 is installed on the outside of the cyclization still 1, and a first interval space 2a is formed between the cyclization still 1 and the first jacket 2. The first jacket 2 is provided with a first steam input port 2b and a first steam output port 2c. The first steam input assembly 6 is connected to the first steam input port 2b, the first steam output assembly 7 is connected to the first steam output port 2c, the first vacuum port 1b is connected to the first vacuum assembly 5, the first vacuum assembly 5 adopts a vacuum pump, the first output port 1c is connected to the input end of the first condenser 3, and the output end of the first condenser 3 is connected to the first receiving tank 4.

[0028] Since the concentration of the chiral alcohol ester synthesized by the chiral alcohol ester synthesis unit A is not always kept consistent, therefore, in the utility model, the chiral alcohol ester synthesized is mixed by the chiral alcohol ester mixing unit B to make the concentration of the chiral alcohol ester uniform. The chiral alcohol ester mixing unit B comprises a first container 8, a first valve 9, a mixing tank 10, a second valve 11, and a second container 12, wherein the first container 8 is connected to the output end of the chiral alcohol ester synthesis unit A, the first container 8 is connected to the output end of the first receiving tank 4, one end of the first valve 9 is connected to the first container 8, the other end of the first valve 9 is connected to the mixing tank 10, an agitator (not shown) is provided in the mixing tank 10, the stirring speed of the agitator is lower than 20 revolutions per minute, the mixing tank 10 is connected to the other end of the second valve 11, the other end of the second valve 11 is connected to the second container 12, and the second container 12 is connected to the ring-opening product reaction unit C.

[0029] Dangerous gas may be generated in the mixing tank 10. In order to increase safety, in the present invention, the chiral alcohol ester mixing unit B further includes a third valve 13 and a first tail gas absorption component VT1. One end of the third valve 13 is connected to the mixing tank 10, and the other end of the third valve 13 is connected to the first tail gas absorption component VT1. If dangerous gas is generated, the third valve 13 is opened to allow the gas to enter the first tail gas absorption component VT1.

[0030] The ring-opening product reaction unit C includes a third container 14, a delivery pump 15, a reactor 16, a second jacket 17, a second steam input component 18, a second steam output component 19, a second condenser 20, and a second receiving tank 21. The third container 14 is connected to the delivery pump 15. The reactor 16 is provided with a second feed port 16a and a second output port 16b. The output end of the delivery pump 15 is connected to the second feed port 16a. The second jacket 17 is arranged outside the reactor 16, and a second space is formed between the reactor 16 and the second jacket 17. The second jacket 17 is provided with a first port 17b and a second port 17c, the second steam input assembly 18 is connected to the first port 17b, a fourth valve 26 is installed between the second steam input assembly 18 and the first port 17b, the second steam output assembly 19 is connected to the second port 17c, a fifth valve 27 is installed between the second steam output assembly 19 and the second port 17c, the second output port 16b is connected to the second condenser 20, and the second condenser 20 is connected to the second receiving tank 21. The reactor 16 is provided with a second air extraction port 16c, the second air extraction port 16c is connected to a second air extraction assembly 16d, and the second receiving tank 21 is connected to the second air extraction assembly 16d.

[0031] The open-loop reaction unit C also includes a refrigerant input control component and a refrigerant output control component. The refrigerant input control component includes a refrigerant supply unit CWS, a first ball valve 22, and a first pneumatic control valve 23. The refrigerant supply unit CWS is connected to one end of the first ball valve 22, and the other end of the first ball valve 22 is connected to one end of the first pneumatic control valve 23, and the other end of the first pneumatic control valve 23 is connected to the first port 17b. The refrigerant output control component includes a second pneumatic control valve 24, a second ball valve 25, and a refrigerant recovery unit CWR. One end of the second pneumatic control valve 24 is connected to the second port 17c, the other end of the second pneumatic control valve 24 is connected to one end of the second ball valve 25, and the other end of the second ball valve 25 is connected to the refrigerant recovery unit CWR.

[0032] In the present utility model, the preferred method is that the other end of the first pneumatic control valve 23 is connected to the fourth valve 26, and one end of the second pneumatic control valve 24 is connected to the fifth valve 27, that is, the refrigerant input control component and the second steam input component 18 form a parallel relationship, and the refrigerant output control component and the second steam output component 19 form a parallel relationship.

[0033] The utility model further comprises a process gas supply unit 28 , which is connected to one end of the fourth valve 26 , and the process gas supply unit 28 can be an air compressor.

[0034] The working process of the utility model is as follows:

[0035] S1, turn on the first vacuum assembly 5, and generate a suction force on the cyclization distillation kettle 1 through the negative pressure generated by the first vacuum assembly 5, so that the raw materials (propylene glycol solution and dimethyl carbonate) in the raw material container Y enter the cyclization distillation kettle 1. After the feeding is completed, close the first vacuum assembly 5.

[0036] S2, open the first steam input component 6 and the first steam output component 7, input steam into the first partition space 2a, heat the cyclization still 1 with steam, and make the propylene glycol solution and dimethyl carbonate in the cyclization still 1 react, and the vaporized product produced in the reaction process enters the first condenser 3 through the first output port 1c to be condensed into propylene carbonate, and the condensed propylene carbonate is output to the first receiving tank 4.

[0037] S3, the propylene carbonate in the first receiving tank 4 is output to the first container 8, the first valve 9 is opened to input the propylene carbonate in the first container 8 into the mixing tank 10, so that the depth of the propylene carbonate in the mixing tank 10 becomes uniform, and the propylene carbonate in the mixing tank 10 is output to the second container 12.

[0038] S4, the propylene carbonate in the second container 12 is output to the reactor 16, and the sodium hydroxide solution in the third container 14 is delivered to the reactor 16 by a delivery pump, the second steam input component 18 and the second steam output component 19 are opened, and steam is input into the second partition space 17a, and the reactor 16 is heated by steam. After a period of reaction (for example, 1 hour), the second vacuum component 16d is started to generate negative pressure in the reactor 16, and the material in the reactor 16 is subjected to reduced pressure distillation, and the generated distillate enters the second condenser 20 through the second output port 16b, and is condensed by the second condenser 20 and output to the second receiving tank 21.

[0039] S5. After the distillation is completed, the process gas supply unit 28 and the second steam output component 19 are opened to input the compressed gas into the second partition space 17a. After the steam in the second partition space 17a is pressed out, the process gas supply unit 28 and the second steam output component 19 are closed, and the refrigerant input control component and the refrigerant output control component are opened to input the refrigerant into the second partition space 17a to cool the material in the reactor 16. After the cooling is completed, the discharge valve 16e provided at the bottom of the reactor 16 is opened to discharge the material into the recovery container 29.

[0040] Finally, it should be noted that the above-described implementation mode is only a preferred embodiment of the utility model to illustrate the technical solution of the utility model, and does not limit it, let alone limit the protection scope of the utility model; although the utility model is described in detail with reference to the aforementioned embodiments, ordinary technicians in this field should understand that they can still modify the technical solutions recorded in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents; and these modifications or replacements do not make the essence of the corresponding technical solution deviate from the protection scope of the claims.

Claims

1. A chiral alcohol ester ring-opening reaction system, comprising a chiral alcohol ester synthesis unit (A), characterized in that: It also includes a chiral alcohol ester mixing unit (B) and a ring-opening product reaction unit (C). The output end of the chiral alcohol ester synthesis unit (A) is connected to the input end of the chiral alcohol ester mixing unit (B), and the output end of the chiral alcohol ester mixing unit (B) is connected to the ring-opening product reaction unit (C).

2. The chiral alcohol ester ring-opening reaction system according to claim 1, characterized in that: The chiral alcohol ester synthesis unit (A) comprises a cyclization still (1), a first jacket (2), a first condenser (3), a first receiving tank (4), a first exhaust assembly (5), a first steam input assembly (6), and a first steam output assembly (7). The still (1) is provided with a first feed port (1a), a first exhaust port (1b), and a first output port (1c). The first jacket (2) is installed on the outside of the cyclization still (1), and a first steam outlet (1c) is formed between the cyclization still (1) and the first jacket (2). A separation space (2a) is formed, and a first steam input port (2b) and a first steam output port (2c) are provided on the first jacket (2); a first steam input component (6) is connected to the first steam input port (2b); a first steam output component (7) is connected to the first steam output port (2c); a first air extraction port (1b) is connected to the first air extraction component (5); a first output port (1c) is connected to the input end of a first condenser (3); and an output end of the first condenser (3) is connected to a first receiving tank (4).

3. The chiral alcohol ester ring-opening reaction system according to claim 1, characterized in that: The chiral alcohol ester mixing unit (B) comprises a first container (8), a first valve (9), a mixing tank (10), a second valve (11), and a second container (12). The first container (8) is connected to the output end of the chiral alcohol ester synthesis unit (A), one end of the first valve (9) is connected to the first container (8), the other end of the first valve (9) is connected to the mixing tank (10), the mixing tank (10) is connected to the other end of the second valve (11), the other end of the second valve (11) is connected to the second container (12), and the second container (12) is connected to the ring-opening product reaction unit (C).

4. The chiral alcohol ester ring-opening reaction system according to claim 3, characterized in that: The chiral alcohol ester mixing unit (B) further comprises a third valve (13) and a first tail gas absorption component (VT1). One end of the third valve (13) is connected to the mixing tank (10), and the other end of the third valve (13) is connected to the first tail gas absorption component (VT1).

5. The chiral alcohol ester ring-opening reaction system according to claim 1, characterized in that: The ring-opening product reaction unit (C) comprises a third container (14), a delivery pump (15), a reactor (16), a second jacket (17), a second steam input component (18), a second steam output component (19), a second condenser (20), and a second receiving tank (21). The third container (14) is connected to the delivery pump (15). The reactor (16) is provided with a second feed port (16a) and a second output port (16b). The output end of the delivery pump (15) is connected to the second feed port (16a). The second jacket (17) is connected to the second steam input component (18), the second steam output component (19), a second condenser (20), and a second receiving tank (21). 7) is arranged outside the reaction kettle (16), and a second spacing space (17a) is formed between the reaction kettle (16) and the second jacket (17); the second jacket (17) is provided with a first port (17b) and a second port (17c); a second steam input component (18) is connected to the first port (17b), a second steam output component (19) is connected to the second port (17c), the second output port (16b) is connected to the second condenser (20), and the second condenser (20) is connected to the second receiving tank (21).

6. The chiral alcohol ester ring-opening reaction system according to claim 5, characterized in that: The open-loop reaction unit (C) further comprises a refrigerant input control component and a refrigerant output control component. The refrigerant input control component comprises a refrigerant supply unit (CWS), a first ball valve (22), and a first pneumatic control valve (23). The refrigerant supply unit (CWS) is connected to one end of the first ball valve (22), the other end of the first ball valve (22) is connected to one end of the first pneumatic control valve (23), and the other end of the first pneumatic control valve (23) is connected to the first port (17b). The refrigerant output control component includes a second pneumatic control valve (24), a second ball valve (25), and a refrigerant recovery unit (CWR). One end of the second pneumatic control valve (24) is connected to the second port (17c), the other end of the second pneumatic control valve (24) is connected to one end of the second ball valve (25), and the other end of the second ball valve (25) is connected to the refrigerant recovery unit (CWR).

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