A high-purity cyclopentyl methyl ether etherification reaction production device

Abstract

This utility model relates to the field of organic synthesis technology, and discloses a high-purity cyclopentyl methyl ether etherification reaction production device, comprising a base and a controller. The controller is located on the left side of the top of the base, and a mixing tank is fixedly connected to the top of the base. A pump body is installed on the right side of the mixing tank, with a drain pipe fixedly connected to the top of the pump body and a suction pipe fixedly connected to the bottom of the pump body. A second valve is fixedly installed on the outside of the suction pipe. This high-purity cyclopentyl methyl ether etherification reaction production device, through the inclusion of a reactor shell and other components, uses an inlet to add 570 mL of spherical strong acidic cationic catalyst with a particle size of 0.8-1.0 mm. The product material is directly fed into a distillation column for separation. The temperature of the distillation column bottom is controlled at 75-90℃. The cyclopentyl methyl ether and methanol mixed solution collected from the column has a purity greater than 99%. The solid acid catalyst replaces the liquid acid, solving the problems of strong corrosiveness of catalysts (such as concentrated sulfuric acid) and complex subsequent processing.

Description

Technical Field

[0001] This utility model relates to the field of organic synthesis technology, specifically to a high-purity cyclopentyl methyl ether etherification reaction production device. Background Technology

[0002] Cyclopentyl methyl ether (CME) is a novel hydrophobic ether solvent. Compared to other ether solvents such as tetrahydrofuran, methyltetrahydrofuran, methyl tert-butyl ether (MTBE), and dioxane, it is easier to separate and recover from water, reducing wastewater discharge. As a reaction solvent, it can be used in coupling reactions, Grignard reactions, coupling amination reactions, n-BuLi reactions, metal reduction reactions, Lewis acid reactions, and Friedel-Crafts reactions. Using CME as a reaction solvent simplifies reaction processing steps and ensures greater solvent safety. Furthermore, the relative stability and safety characteristics of CME significantly enhance the safety of laboratory and production facilities.

[0003] The existing high-purity cyclopentyl methyl ether etherification reaction production equipment is not suitable because the catalyst (such as concentrated sulfuric acid) is highly corrosive and the subsequent treatment is complex, which does not conform to the trend of green chemistry. Therefore, its structure needs to be improved.

[0004] Now, a novel high-purity cyclopentyl methyl ether etherification reaction production device is proposed to solve the above problems. Utility Model Content

[0005] The purpose of this invention is to provide a high-purity cyclopentyl methyl ether etherification reaction production device to solve the problems mentioned in the background art, such as the strong corrosiveness of catalysts (e.g., concentrated sulfuric acid) and the complexity of subsequent processing.

[0006] To achieve the above objectives, this utility model provides the following technical solution: a high-purity cyclopentyl methyl ether etherification reaction production device, comprising a base platform and a controller. The controller is located on the left side of the top of the base platform. A mixing tank is fixedly connected to the top of the base platform. A pump body is installed on the right side of the mixing tank. A drain pipe is fixedly connected to the top of the pump body. A suction pipe is fixedly connected to the bottom of the pump body. A second valve is fixedly installed on the outside of the suction pipe. A third valve is fixedly installed on the outside of the drain pipe. A fixing pipe is fixedly connected to the top of the drain pipe. A first diversion pipe is fixedly connected to the bottom of the fixing pipe. A fourth valve is fixedly installed on the outside of the first diversion pipe. A reactor shell is fixedly connected to the right side of the top of the base. An inner tube is fixedly connected inside the reactor shell. An oil inlet is fixedly connected to the left side of the top of the reactor shell. A feed inlet is fixedly connected to the top of the inner tube. Temperature measuring resistors are fixedly connected to the top, middle and bottom of the outer side of the inner tube. A discharge port is fixedly connected to the bottom of the inner tube. A first discharge pipe is fixedly connected to the bottom of the discharge port. A seventh valve is fixedly installed on the outside of the first discharge pipe. A distillation column is provided at the rear end of the reactor shell.

[0007] As a further technical solution of this utility model, the left side of the liquid extraction pipe is connected to the interior of the mixing tank, and the reactor shell is provided with two sets, and the reactor shell and the inner tube are made of stainless steel.

[0008] As a further technical solution of this utility model, a drive motor is fixedly installed at the top of the mixing box, the output end of the drive motor passes through the interior of the top of the mixing box and is fixedly connected to a stirring shaft, and support legs are fixedly connected to both sides of the top of the mixing box, and a fixing frame is fixedly connected to the top of the support legs.

[0009] As a further technical solution of this utility model, a material injection pipe is fixedly connected to the bottom end of the fixed frame, a first valve is fixedly installed on the outside of the material injection pipe, and the bottom end of the material injection pipe is connected to the inside of the top of the mixing box.

[0010] As a further technical solution of this utility model, an injection cylinder is provided inside the top of the fixed frame, the front end of the injection cylinder is provided with a scale, and two sets of injection cylinders are provided.

[0011] As a further technical solution of this utility model, a circulating oil is provided between the reactor shell and the interior of the inner tube, and 570 mL of spherical strong acid cationic catalyst with a particle size of 0.8-1.0 mm is placed inside the inner tube.

[0012] As a further technical solution of this utility model, a second feed pipe is fixedly connected to one side of the bottom end of the distillation column, a fifth valve is fixedly installed on the outside of the second feed pipe, a water inlet pipe is fixedly connected to the top end of the distillation column, a water inlet is fixedly connected to the right side of the water inlet pipe, a second branch pipe is fixedly connected to the bottom end of the water inlet pipe, a sixth valve is fixedly installed on the outside of the second branch pipe, and the first feed pipe is connected to the inside of the distillation column.

[0013] As a further technical solution of this utility model, the second diversion pipe is provided in two sets, and the distillation column is provided in two sets.

[0014] Compared with the prior art, the beneficial effects of this utility model are: the high-purity cyclopentyl methyl ether etherification reaction production device is not only environmentally friendly and does not use solvents, but also achieves easy and uniform mixing and precise proportioning, and optimizes the process and improves performance.

[0015] (1) By setting up a reactor shell, oil inlet, temperature measuring resistor, inner tube, distillation column, feed inlet, first feed pipe, second feed pipe, fifth valve, and feed inlet, 570 mL of spherical strong acid cationic catalyst with a particle size of 0.8-1.0 mm is added through the feed inlet, and the produced material is directly fed into the distillation column for separation. The temperature of the distillation column bottom is controlled at 75-90℃. The cyclopentyl methyl ether and methanol mixed solution with a content of more than 99% is collected from the column. The solid acid catalyst replaces the liquid acid, which is easy to recover and non-corrosive.

[0016] (2) A mixing tank, drive motor, stirring shaft, support legs, fixed frame, injection cylinder, injection pipe, and first valve are provided. Cyclopentene and methanol are injected into the injection cylinder according to the molar ratio of alcohol and olefin, respectively. The first valve is opened, and cyclopentene and methanol are injected into the mixing tank at a molar ratio of 2:1 through the injection pipe. The drive motor is turned on, and the stirring shaft is driven to mix them. Since the front end of the injection cylinder is marked, it is convenient to accurately check the injection ratio. The pump flow rate is 5 mL / min to pump the raw materials, and the volumetric liquid hourly velocity of the material is controlled at 0.53 hr. -1 ;

[0017] (3) By setting up an inlet pipe, a second branch pipe, a sixth valve, a seventh valve, and a water injection port, deionized water with a methanol content of 2-2.5 times is injected into the distillation column and washed with water. Then, the cyclopentyl methyl ether and methanol mixed solution collected from the column is washed with water 2-3 times, and the clear liquid is taken. This upper liquid is cyclopentyl methyl ether with a purity greater than 99%. By controlling the excess methanol to inhibit the polymerization of cyclopentene, the process is optimized. Attached Figure Description

[0018] Figure 1 This is a frontal cross-sectional view of the present invention.

[0019] Figure 2 This is a rear view schematic diagram of the connection between the water inlet pipe and the distillation column of this utility model;

[0020] Figure 3 This is a front view structural diagram of the connection method between the fixed frame and the mixing box of this utility model;

[0021] Figure 4 This is a front view structural diagram of the connection method between the inner tube and the first diversion tube of this utility model.

[0022] In the diagram: 1. Base platform; 2. Mixing tank; 3. Drive motor; 4. Stirring shaft; 5. Support leg; 6. Fixing frame; 7. Feeding cylinder; 8. Feeding pipe; 9. First valve; 10. Pump body; 11. Liquid extraction pipe; 12. Second valve; 13. Drain pipe; 14. Third valve; 15. Fixing pipe; 16. First branch pipe; 17. Fourth valve; 18. Reactor shell; 19. Oil inlet; 20. Temperature measuring resistor; 21. Inner tube; 22. Distillation column; 23. Feed outlet; 24. First feed pipe; 25. Second feed pipe; 26. Fifth valve; 27. Water inlet pipe; 28. Second branch pipe; 29. ​​Sixth valve; 30. Seventh valve; 31. Water inlet; 32. Feed inlet; 33. Controller. Detailed Implementation

[0023] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0024] Please see Figure 1-4This utility model provides an embodiment of a high-purity cyclopentyl methyl ether etherification reaction production device, including a base platform 1 and a controller 33. The controller 33 is located on the left side of the top of the base platform 1. A mixing tank 2 is fixedly connected to the top of the base platform 1. A pump body 10 is installed on the right side of the mixing tank 2. A drain pipe 13 is fixedly connected to the top of the pump body 10. A suction pipe 11 is fixedly connected to the bottom of the pump body 10. A second valve 12 is fixedly installed on the outside of the suction pipe 11. A third valve 14 is fixedly installed on the outside of the drain pipe 13. A fixed pipe 15 is fixedly connected to the top of the drain pipe 13. A first diversion pipe 16 is fixedly connected to the bottom of the fixed pipe 15. A fourth valve 17 is fixedly installed on the outside of the flow tube 16. A reactor shell 18 is fixedly connected to the right side of the top of the base 1. An inner tube 21 is fixedly connected inside the reactor shell 18. An oil inlet 19 is fixedly connected to the left side of the top of the reactor shell 18. A feed inlet 32 ​​is fixedly connected to the top of the inner tube 21. Temperature measuring resistors 20 are fixedly connected to the top, middle and bottom of the outer side of the inner tube 21. A discharge port 23 is fixedly connected to the bottom of the inner tube 21. A first discharge pipe 24 is fixedly connected to the bottom of the discharge port 23. A seventh valve 30 is fixedly installed on the outside of the first discharge pipe 24. A distillation column 22 is provided at the rear end of the reactor shell 18.

[0025] The left side of the extraction pipe 11 is connected to the interior of the mixing box 2. The reactor shell 18 is provided with two sets. The reactor shell 18 and the inner tube 21 are made of stainless steel.

[0026] A circulating oil is provided between the reactor shell 18 and the interior of the inner tube 21. 570 mL of spherical strong acid cationic catalyst with a particle size of 0.8-1.0 mm is placed inside the inner tube 21.

[0027] Specifically, such as Figure 1 and Figure 4 As shown, 570 mL of spherical strong acid cationic catalyst with a particle size of 0.8-1.0 mm is added through inlet 32. Circulating oil is injected between the inner tube 21 and the reactor shell 18 through oil inlet 19. The reaction feed rate is controlled by pump 10 using temperature measuring resistor 20. The reaction temperature is set at 140℃, and the system pressure is controlled at 2 MPa. The product material is directly fed into distillation column 22 for separation. The bottom temperature of the distillation column is controlled at 75-90℃. A mixed solution of cyclopentyl methyl ether and methanol with a content greater than 99% is collected from the column. The solid acid catalyst replaces the liquid acid, making it easy to recover and non-corrosive.

[0028] A drive motor 3 is fixedly installed at the top of the mixing box 2. The output end of the drive motor 3 passes through the interior of the top of the mixing box 2 and is fixedly connected to a stirring shaft 4. Support legs 5 are fixedly connected to both sides of the top of the mixing box 2, and a fixing frame 6 is fixedly connected to the top of the support legs 5.

[0029] The bottom end of the fixed frame 6 is fixedly connected to the injection pipe 8, and the outside of the injection pipe 8 is fixedly installed with the first valve 9. The bottom end of the injection pipe 8 is connected to the inside of the top of the mixing box 2.

[0030] The top of the fixed frame 6 is equipped with an injection cylinder 7. The front end of the injection cylinder 7 is marked with a scale. There are two sets of injection cylinders 7.

[0031] Specifically, such as Figure 1 and Figure 3 As shown, cyclopentene and methanol are injected into the injection cylinder 7 according to the molar ratio of alcohol to olefin, respectively. The first valve 9 is opened, allowing cyclopentene and methanol to be injected into the mixing tank 2 at a molar ratio of 2:1 through the injection pipe 8. The drive motor 3 is turned on, driving the stirring shaft 4 to mix them. Because the front end of the injection cylinder is marked with graduations, the injection ratio can be easily and accurately checked. The pump flow rate is 5 mL / min, and the liquid hourly space velocity (LHSV) of the material is controlled at 0.53 hr. -1 .

[0032] A second feed pipe 25 is fixedly connected to one side of the bottom end of the distillation column 22. A fifth valve 26 is fixedly installed on the outside of the second feed pipe 25. A water inlet pipe 27 is fixedly connected to the top end of the distillation column 22. A water inlet 31 is fixedly connected to the right side of the water inlet pipe 27. A second branch pipe 28 is fixedly connected to the bottom end of the water inlet pipe 27. A sixth valve 29 is fixedly installed on the outside of the second branch pipe 28. The first feed pipe 24 is connected to the inside of the distillation column 22.

[0033] The second diversion pipe 28 is provided in two sets, and the distillation column 22 is provided in two sets;

[0034] Specifically, such as Figure 1 and Figure 2 As shown, deionized water with a methanol content of 2-2.5 times is injected into the distillation column 22 through water injection port 31 and washed with water. Then, the cyclopentyl methyl ether and methanol mixture solution collected from the column is washed with water 2-3 times, and the clear liquid from the previous wash is taken. This upper liquid is cyclopentyl methyl ether with a purity greater than 99%. By controlling the excess methanol to inhibit the polymerization of cyclopentene, the process is optimized.

[0035] Working Principle: In use, cyclopentene and methanol are first injected into the injection cylinder 7 according to their respective molar ratios. The first valve 9 is opened, allowing the cyclopentene and methanol to be injected into the mixing tank 2 at a molar ratio of 2:1 through the injection pipe 8. The drive motor 3 is then turned on, driving the stirring shaft 4 to mix the materials. The injection cylinder has graduations at the front end for easy and accurate monitoring of the injection ratio. The pump flow rate is 5 mL / min, and the liquid hourly space velocity (LHSV) is controlled at 0.53 hr. -1Using inlet 32, 570 mL of spherical strong acidic cationic catalyst with a particle size of 0.8-1.0 mm is added. Using oil inlet 19, circulating oil is injected between the inner tube 21 and the reactor shell 18. The reaction feed rate is controlled by pump 10 using a temperature measuring resistor 20. The reaction temperature is set at 140℃, and the system pressure is controlled at 2 MPa. The product material is directly fed into distillation column 22 for separation. The distillation column bottom temperature is controlled at 75-90℃. Cyclopentylmethyl methacrylate is collected from the column. The ether and methanol mixture solution has a content greater than 99%. Solid acid catalyst replaces liquid acid, which is easy to recover and non-corrosive. Finally, deionized water with a methanol content of 2-2.5 times is injected into the distillation column 22 through water injection port 31 and washed with water. The cyclopentyl methyl ether and methanol mixture solution collected from the column is then washed with water 2-3 times. The supernatant is taken, which is the cyclopentyl methyl ether with a purity greater than 99%. By controlling the excess methanol to inhibit cyclopentene polymerization, the process is optimized.

[0036] It will be apparent to those skilled in the art that this invention is not limited to the details of the exemplary embodiments described above, and that it can be implemented in other specific forms without departing from the spirit or essential characteristics of this invention. Therefore, the embodiments should be considered illustrative and non-limiting in all respects, and the scope of this invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within this invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

Claims

1. A high-purity cyclopentyl methyl ether etherification reaction production device, comprising a base table (1) and a controller (33), characterized in that: A controller (33) is provided on the left side of the top of the base (1). A mixing tank (2) is fixedly connected to the top of the base (1). A pump body (10) is installed on the right side of the mixing tank (2). A drain pipe (13) is fixedly connected to the top of the pump body (10). A suction pipe (11) is fixedly connected to the bottom of the pump body (10). A second valve (12) is fixedly installed on the outside of the suction pipe (11). A third valve (14) is fixedly installed on the outside of the drain pipe (13). A fixed pipe (15) is fixedly connected to the top of the drain pipe (13). A first diversion pipe (16) is fixedly connected to the bottom of the fixed pipe (15). A fourth valve (17) is fixedly installed on the outside of the first diversion pipe (16). A reactor shell (18) is fixedly connected to the right side of the top of the base (1). An inner tube (21) is fixedly connected inside the reactor shell (18). An oil inlet (19) is fixedly connected to the left side of the top of the reactor shell (18). A feed inlet (32) is fixedly connected to the top of the inner tube (21). Temperature measuring resistors (20) are fixedly connected to the top, middle and bottom of the outer side of the inner tube (21). A discharge port (23) is fixedly connected to the bottom of the inner tube (21). A first discharge pipe (24) is fixedly connected to the bottom of the discharge port (23). A seventh valve (30) is fixedly installed on the outside of the first discharge pipe (24). A distillation column (22) is provided at the rear end of the reactor shell (18).

2. The high-purity cyclopentyl methyl ether etherification reaction production apparatus according to claim 1, characterized in that: The left side of the liquid extraction pipe (11) is connected to the interior of the mixing tank (2). The reactor shell (18) is provided in two sets. The reactor shell (18) and the inner tube (21) are made of stainless steel.

3. The high-purity cyclopentyl methyl ether etherification reaction production apparatus according to claim 1, characterized in that: A drive motor (3) is fixedly installed at the top of the mixing box (2). The output end of the drive motor (3) passes through the interior of the top of the mixing box (2) and is fixedly connected to a stirring shaft (4). Support legs (5) are fixedly connected to both sides of the top of the mixing box (2). A fixed frame (6) is fixedly connected to the top of the support legs (5).

4. The high-purity cyclopentyl methyl ether etherification reaction production apparatus according to claim 3, characterized in that: The bottom end of the fixed frame (6) is fixedly connected to the injection pipe (8), and the outside of the injection pipe (8) is fixedly installed with a first valve (9). The bottom end of the injection pipe (8) is connected to the inside of the top of the mixing box (2).

5. The high-purity cyclopentyl methyl ether etherification reaction production apparatus according to claim 3, characterized in that: The top of the fixed frame (6) is provided with an injection cylinder (7), the front end of the injection cylinder (7) is provided with a scale, and there are two sets of injection cylinders (7).

6. The apparatus for producing high-purity cyclopentyl methyl ether via etherification reaction according to claim 1, characterized in that: A circulating oil is provided between the reactor shell (18) and the inner tube (21), and 570 mL of spherical strong acid cationic catalyst with a particle size of 0.8-1.0 mm is placed inside the inner tube (21).

7. The apparatus for producing high-purity cyclopentyl methyl ether via etherification reaction according to claim 1, characterized in that: A second feed pipe (25) is fixedly connected to one side of the bottom end of the distillation column (22). A fifth valve (26) is fixedly installed on the outside of the second feed pipe (25). A water inlet pipe (27) is fixedly connected to the top end of the distillation column (22). A water inlet (31) is fixedly connected to the right side of the water inlet pipe (27). A second branch pipe (28) is fixedly connected to the bottom end of the water inlet pipe (27). A sixth valve (29) is fixedly installed on the outside of the second branch pipe (28). The first feed pipe (24) is connected to the inside of the distillation column (22).

8. The apparatus for producing high-purity cyclopentyl methyl ether via etherification reaction according to claim 7, characterized in that: The second diversion pipe (28) is provided in two sets, and the distillation column (22) is provided in two sets.

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