Chiral alcohol ester cyclization reaction device

Abstract

The utility model discloses a chiral alcohol ester cyclization reaction device which comprises a cyclization kettle, a cyclization condenser, a receiving tank, a jacket, a first feeding valve and a second feeding valve, the cyclization kettle is provided with a feeding port and a distillate output port, the jacket is installed on the cyclization kettle, an interval space is formed between the jacket and the cyclization kettle, and the first feeding valve and the second feeding valve are arranged in the interval space. The cyclization kettle is provided with a first feeding valve and a second feeding valve, the first feeding valve and the second feeding valve are respectively connected with the feeding port, the distillate output port is connected with the input end of the cyclization condenser, the cyclization kettle further comprises a first valve, a vacuumizing assembly, a backflow pipeline and a second valve, the other end of the first valve is connected with the vacuumizing assembly, one end of the backflow pipeline and one end of the second valve are connected with the output end of the cyclization condenser, the other end of the backflow pipeline is connected with the backflow opening, and the other end of the second valve is connected with the receiving tank. According to the utility model, the concentration of the chiral alcohol ester can meet the requirement.

Description

Technical Field

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

[0002] Propylene carbonate is a colorless, odorless, flammable liquid. It is miscible with ether, acetone, benzene, chloroform, vinyl acetate, etc., and soluble in water and carbon tetrachloride. It has a strong ability to absorb carbon dioxide and is stable in nature. Propylene carbonate can be used as oily solvents, spinning solvents, olefins, aromatic hydrocarbon extractants, carbon dioxide absorbents, dispersants for water-soluble dyes and pigments, etc.

[0003] At present, propylene carbonate is usually produced by distillation. CN203540544U discloses a self-reflux propylene carbonate reactor, which comprises a reactor body 1, a steam jacket 2, an agitator 3, a self-retaining cooler 4, a cooling water inlet 5 and a cooling water outlet 6; the steam jacket 2 is arranged on the outer side of the reactor body 1, the agitator 3 is arranged in the middle of the reactor body 1, the upper part of one side of the reactor body 1 is connected to the self-retaining cooler 4, one side of the lower part of the self-retaining cooler 4 is provided with a cooling water inlet 5, and the other side of the upper part of the self-retaining cooler 4 is provided with a cooling water outlet 6.

[0004] The above-mentioned reactor only distills and condenses the material, and the distillate flows into the self-retaining cooler 4 for condensation to obtain propylene carbonate liquid, which is finally recovered. Then, the above-mentioned distillation belongs to a conventional process, and the propylene carbonate is directly condensed and recovered. Since the concentration of propylene carbonate is low in the initial stage, direct recovery will eventually reduce the concentration of the overall recoverable propylene carbonate. Utility Model Content

[0005] The utility model provides a chiral alcohol ester cyclization reaction device. The utility model can make the concentration of the chiral alcohol ester meet the requirements.

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

[0007] The chiral alcohol ester cyclization reaction device comprises a cyclization kettle, a cyclization condenser, a receiving tank, a jacket, a first feeding valve, and a second feeding valve. The cyclization kettle is provided with a feeding port and a distillate output port. The jacket is installed on the cyclization kettle to form a spacing space between the jacket and the cyclization kettle. The first feeding valve and the second feeding valve are respectively connected to the feeding port, and the distillate output port is connected to the input end of the cyclization condenser. The device also comprises a first valve, a vacuum pumping component, a reflux pipeline, and a second valve. The cyclization kettle is provided with an air suction port and a reflux port. One end of the first valve is connected to the air suction port, and the other end of the first valve is connected to the vacuum pumping component. One end of the reflux pipeline and one end of the second valve are respectively connected to the output end of the cyclization condenser, and the other end of the reflux pipeline is connected to the reflux port. The other end of the second valve is connected to the receiving tank.

[0008] Furthermore, it also includes a third valve, a first flame arrester, and a first exhaust gas absorption component. One end of the third valve is connected to the air extraction port, the other end of the third valve is connected to one end of the first flame arrester, and the other end of the first flame arrester is connected to the first exhaust gas absorption component.

[0009] Furthermore, it also includes an air supply unit, a pneumatic diaphragm pump, and a dimethyl carbonate storage device. The pneumatic diaphragm pump is connected to the air supply unit, the pneumatic diaphragm pump is connected to the dimethyl carbonate storage device, and the pneumatic diaphragm pump is connected to the second feeding valve.

[0010] Furthermore, the vacuum pump assembly includes a vacuum pump, a first vacuum buffer tank, and a second vacuum buffer tank. The vacuum pump is connected to the first vacuum buffer tank, the first vacuum buffer tank is connected to the second vacuum buffer tank, and the second vacuum buffer tank is connected to the other end of the first valve.

[0011] Furthermore, the vacuum pumping assembly also includes a fourth valve, a second flame arrester, and a second exhaust gas absorption component. One end of the fourth valve is connected to the first vacuum buffer tank, the other end of the fourth valve is connected to one end of the second flame arrester, and the other end of the second flame arrester is connected to the second exhaust gas absorption component.

[0012] In the utility model, after the feeding is completed, steam is input into the interval space to heat the material in the cyclization kettle to make the material react, and the vaporized product generated in the reaction process enters the cyclization condenser to condense into a liquid. Although the liquid at this time is a chiral chiral alcohol ester, the concentration is low. Therefore, the liquid obtained in the reaction stage is refluxed into the cyclization kettle through the reflux pipe and the reflux port until the reaction is completed. The chiral alcohol ester is recovered into the receiving tank by means of reduced pressure distillation. At this time, the concentration of the chiral alcohol ester meets the corresponding requirements. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 It is a schematic diagram of the chiral alcohol ester cyclization reaction device of the utility model.

[0014] Figure 2 for Figure 1 Enlarged view of the Q section in .

[0015] Markings in the accompanying drawings:

[0016] Cyclization kettle 1, feeding port 1a, distillate output port 1b, exhaust port 1c, reflux port 1d, discharge valve 1f, cyclization condenser 2, receiving tank 3, tail gas discharge port 3a, jacket 4, first port 4a, second port 4b, partition space 5, first feeding valve 6, second feeding valve 7, first valve 8, reflux pipeline 9, second valve 10, fourth valve 13, pneumatic diaphragm pump 14, dimethyl carbonate storage 15, vacuum pump 16, first vacuum buffer tank 17, second vacuum buffer tank 18, second flame arrester 19, first stop valve 20, first pneumatic diaphragm regulating valve 21, first pneumatic control valve 22, first ball valve 23, second pneumatic Control valve 24, second stop valve 25, third stop valve 26, fifth valve 27, third flame arrester 28, sixth valve 29, fourth flame arrester 30, second ball valve 31, third pneumatic control valve 32, third ball valve 33, fourth pneumatic control valve 34, fourth ball valve 35, process gas supply unit 36, vent valve 37, propylene glycol solution storage container A, air supply unit PAS, steam storage unit LS, first tail gas absorption component VT1, second tail gas absorption component VT2, third tail gas absorption component VT3, fourth tail gas absorption component VT4, refrigerant supply unit CWS, refrigerant recovery unit CWR, process gas supply unit 36. DETAILED DESCRIPTION

[0017] The utility model is further described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0018] 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.

[0019] like Figure 1 and 2 The chiral alcohol ester cyclization reaction device of the utility model comprises a cyclization kettle 1, a cyclization condenser 2, a receiving tank 3, a jacket 4, a first feeding valve 6, a second feeding valve 7, a first valve 8, a vacuum pumping component, a reflux pipeline 9, a second valve 10, a gas supply unit PAS, a pneumatic diaphragm pump 14, and a dimethyl carbonate storage 15. The various parts and the relationship between them are described in detail below.

[0020] The cyclization kettle 1 is provided with a feed port 1a and a distillate output port 1b, a first feed valve 6 and a second feed valve 7 are respectively connected to the feed port 1a, the first feed valve 6 is connected to the propylene glycol solution storage container A, a pneumatic diaphragm pump 14 is connected to the air supply unit PAS, the pneumatic diaphragm pump 14 is connected to the dimethyl carbonate storage 15, the pneumatic diaphragm pump 14 is connected to the second feed valve 7, and the dimethyl carbonate in the dimethyl carbonate storage 15 is transported to the cyclization kettle 1 through the pneumatic diaphragm pump 14.

[0021] The jacket 4 is installed on the cyclization kettle 1, and a spacing space 5 is formed between the jacket 4 and the cyclization kettle 1. The jacket 4 is provided with a first port 4a and a second port 4b. The first port 4a is connected to the steam supply component, and the second port 4b is connected to the steam output component.

[0022] The steam supply component includes a steam storage unit LS, a first stop valve 20, a first pneumatic diaphragm regulating valve 21, and a first pneumatic control valve 22. The steam storage unit LS is connected to one end of the first stop valve 20, the other end of the first stop valve 20 is connected to one end of the first pneumatic diaphragm regulating valve 21, the other end of the first pneumatic diaphragm regulating valve 21 is connected to one end of the first pneumatic control valve 22, and a first ball valve 23 is provided between the first pneumatic control valve 22 and the first port 4a, the other end of the first pneumatic control valve 22 is connected to one end of the first ball valve 23, and the other end of the first ball valve 23 is connected to the first port 4a.

[0023] The steam output component includes a second pneumatic control valve 24, a second stop valve 25, and a third stop valve 26. One end of the second pneumatic control valve 24 is connected to the second port 4b, and the other end of the second pneumatic control valve 24 is connected to one end of the second stop valve 25. The third stop valve 26 is connected in parallel with the series branch formed by the second pneumatic control valve 24 and the second stop valve 25.

[0024] The distillate output port 1b is connected to the input end of the cyclization condenser 2, and the cyclization kettle 1 is provided with an exhaust port 1c and a reflux port 1d. One end of the first valve 8 is connected to the exhaust port 1c, and the other end of the first valve 8 is connected to the vacuum pump component. The vacuum pump component includes a vacuum pump 16, a first vacuum buffer tank 17, and a second vacuum buffer tank 18. The vacuum pump 16 is a Roots vacuum pump. The vacuum pump 16 is connected to the first vacuum buffer tank 17, the first vacuum buffer tank 17 is connected to the second vacuum buffer tank 18, and the second vacuum buffer tank 18 is connected to the other end of the first valve 8.

[0025] The vacuum pumping assembly also includes a fourth valve 13, a second flame arrester 19, and a second exhaust gas absorption component VT2. One end of the fourth valve 13 is connected to the first vacuum buffer tank 17, the other end of the fourth valve 13 is connected to one end of the second flame arrester 19, and the other end of the second flame arrester 19 is connected to the second exhaust gas absorption component VT2.

[0026] One end of the reflux pipe 9 and the second valve 10 are respectively connected to the output end of the ring-closed condenser 2, the other end of the reflux pipe 9 is connected to the reflux port 1d, and the other end of the second valve 10 is connected to the receiving tank 3. It also includes a third valve 11, a first flame arrester 12, and a first tail gas absorption component VT1, one end of the third valve 11 is connected to the air extraction port 1c, the other end of the third valve 11 is connected to one end of the first flame arrester 12, and the other end of the first flame arrester 12 is connected to the first tail gas absorption component VT1.

[0027] The utility model also includes a fifth valve 27, a third flame arrester 28, and a third tail gas absorption component VT3. One end of the fifth valve 27 is connected to the output end of the annular condenser 2, the other end of the fifth valve 27 is connected to one end of the third flame arrester 28, and the other end of the third flame arrester 28 is connected to the third tail gas absorption component VT3.

[0028] The utility model also includes a sixth valve 29, a fourth flame arrester 30, and a fourth tail gas absorption component VT4. A tail gas discharge port 3a is provided on the receiving tank 3. One end of the sixth valve 29 is connected to the tail gas discharge port 3a on the receiving tank 3, and the other end of the sixth valve 29 is connected to one end of the fourth flame arrester 30, and the other end of the fourth flame arrester 30 is connected to the fourth tail gas absorption component VT4.

[0029] The utility model 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 second ball valve 31, a third pneumatic control valve 32, and a third ball valve 33. The refrigerant supply unit CWS is connected to one end of the second ball valve 31, the other end of the second ball valve 31 is connected to one end of the third pneumatic control valve 32, the other end of the third pneumatic control valve 32 is connected to one end of the third ball valve 33, and the other end of the third ball valve 33 is connected to the second port 4b.

[0030] The refrigerant output control component includes a fourth pneumatic control valve 34, a fourth ball valve 35, and a refrigerant recovery unit CWR. One end of the fourth pneumatic control valve 34 is connected to one end of the first ball valve 23, the other end of the fourth pneumatic control valve 34 is connected to one end of the fourth ball valve 35, and the other end of the fourth ball valve 35 is connected to the refrigerant recovery unit CWR.

[0031] The utility model further comprises a process gas supply unit 36 ​​, the output end of the process gas supply unit 36 ​​is connected to one end of the third ball valve 33 , and the process gas supply unit 36 ​​can be an air compressor.

[0032] The following is a specific example of the working process of the utility model:

[0033] S1, open the first feeding valve 6, the first valve 8, and the vacuum pump 16, and generate a suction force on the cyclization kettle 1 through the negative pressure generated by the vacuum pump 16, so that the propylene glycol solution in the propylene glycol solution storage container A enters the cyclization kettle 1. After the feeding of the propylene glycol solution is completed, close the first feeding valve 6, the first valve 8, and the vacuum pump 16, open the pneumatic diaphragm pump 14 and the second feeding valve 7, and transport the dimethyl carbonate in the dimethyl carbonate storage 15 to the cyclization kettle 1 through the pneumatic diaphragm pump 14. After the feeding of dimethyl carbonate is completed, close and open the pneumatic diaphragm pump 14 and the second feeding valve 7.

[0034] S2, open the first stop valve 20, the first pneumatic diaphragm regulating valve 21, the first pneumatic control valve 22, the first ball valve 23, and open the second pneumatic control valve 24, the second stop valve 25, and the third stop valve 26, input steam into the partition space 5, heat the cyclization kettle 1 with steam, and make the propylene glycol solution and dimethyl carbonate in the cyclization kettle 1 react, and the vaporized product produced in the reaction process enters the cyclization condenser 2 through the distillate outlet 1b and is condensed into liquid, and the liquid is refluxed into the cyclization kettle 1 through the cyclization condenser 2, the reflux pipe 9 and the reflux port 1d until the reaction is completed.

[0035] S3, after the reaction is completed, the first valve 8, the vacuum pump 16, and the second valve 10 are opened, and the product is recovered by vacuum distillation. The distillate produced during the vacuum distillation enters the cyclization condenser 2 through the distillate output port 1b to be condensed into chiral propylene carbonate (chiral propylene carbonate is a product of chiral alcohol esters), and the chiral propylene carbonate enters the receiving tank 3 through the second valve 10. In this process, since the reflux pipe 9 has a concave portion 9a, the concave portion 9a forms an obstacle to the chiral propylene carbonate output by the cyclization condenser 2. Therefore, the chiral propylene carbonate flows smoothly through the second valve 10 into the receiving tank 3.

[0036] S4, after the distillation is completed, open the process gas supply unit 36, the third ball valve 33, the first ball valve 23 and the vent valve 37, so that the compressed air enters the partition space 5 from the bottom of the partition space 5, and the steam in the partition space 5 is pressed out from bottom to top by the compressed air, and the compressed air is discharged through the first port 4a, the first ball valve 23 and the vent valve 37.

[0037] S5, after all the steam is pressed out, open the second ball valve 31, the third pneumatic control valve 32, the third ball valve 33, the first ball valve 23, the fourth pneumatic control valve 34, and the fourth ball valve 35, so that the refrigerant in the refrigerant supply unit CWS enters the partition space 5 from the bottom of the partition space 5, and the material in the cyclization kettle 1 is cooled by the refrigerant. After the cooling is completed, the material is output to the designated position through the discharge valve 1f provided at the bottom of the cyclization kettle 1.

[0038] In the above process, the first tail gas absorption component VT1, the second tail gas absorption component VT2, the third tail gas absorption component VT3, and the fourth tail gas absorption component VT4 absorb the tail gas in the corresponding container to improve the installation performance of the system. In addition, a stirrer current sensor, a pressure sensor, and a temperature sensor are set on the cyclization reactor 1 for protection and control.

[0039] 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 cyclization reaction device, comprising a cyclization kettle (1), a cyclization condenser (2), a receiving tank (3), a jacket (4), a first feed valve (6), and a second feed valve (7), wherein the cyclization kettle (1) is provided with a feed port (1a) and a distillate outlet (1b), the jacket (4) is installed on the cyclization kettle (1), and a separation space (5) is formed between the jacket (4) and the cyclization kettle (1), the first feed valve (6) and the second feed valve (7) are respectively connected to the feed port (1a), and the distillate outlet (1b) is connected to the input end of the cyclization condenser (2), characterized in that: The invention also comprises a first valve (8), a vacuum pumping assembly, a reflux pipe (9), and a second valve (10). The cyclization kettle (1) is provided with a vacuum port (1c) and a reflux port (1d). One end of the first valve (8) is connected to the vacuum port (1c), and the other end of the first valve (8) is connected to the vacuum pumping assembly. One end of the reflux pipe (9) and one end of the second valve (10) are respectively connected to the output end of the cyclization condenser (2), the other end of the reflux pipe (9) is connected to the reflux port (1d), and the other end of the second valve (10) is connected to the receiving tank (3).

2. The chiral alcohol ester cyclization reaction device according to claim 1, characterized in that: It also includes a third valve (11), a first flame arrester (12), and a first tail gas absorption component (VT1); one end of the third valve (11) is connected to the air extraction port (1c); the other end of the third valve (11) is connected to one end of the first flame arrester (12); and the other end of the first flame arrester (12) is connected to the first tail gas absorption component (VT1).

3. The chiral alcohol ester cyclization reaction device according to claim 1, characterized in that: It also includes an air supply unit (PAS), a pneumatic diaphragm pump (14), and a dimethyl carbonate storage device (15). The pneumatic diaphragm pump (14) is connected to the air supply unit (PAS), the pneumatic diaphragm pump (14) is connected to the dimethyl carbonate storage device (15), and the pneumatic diaphragm pump (14) is connected to the second feeding valve (7).

4. The chiral alcohol ester cyclization reaction device according to claim 1, characterized in that: The vacuum pump assembly comprises a vacuum pump (16), a first vacuum buffer tank (17), and a second vacuum buffer tank (18); the vacuum pump (16) is connected to the first vacuum buffer tank (17), the first vacuum buffer tank (17) is connected to the second vacuum buffer tank (18), and the second vacuum buffer tank (18) is connected to the other end of the first valve (8).

5. The chiral alcohol ester cyclization reaction device according to claim 4, characterized in that: The vacuum pumping assembly further comprises a fourth valve (13), a second flame arrester (19), and a second tail gas absorption component (VT2); one end of the fourth valve (13) is connected to the first vacuum buffer tank (17), the other end of the fourth valve (13) is connected to one end of the second flame arrester (19), and the other end of the second flame arrester (19) is connected to the second tail gas absorption component (VT2).

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