A method for synthesizing isoborneol using microfluidic field technology

Abstract

The invention discloses a method for synthesizing isoborneol using microflow field technology, comprising the following steps: step 1, respectively preparing isoborneol acetate and 50% liquid caustic soda; step 2, transporting the prepared isoborneol acetate and 50% liquid caustic soda into a microchannel reactor using a liquid delivery pump, and completing the reaction of the isoborneol acetate and 50% liquid caustic soda by the microchannel reactor; step 3, sending the mixed solution reacted in the microchannel reactor to a water washing and purification kettle, washing the generated sodium acetate and incompletely reacted sodium hydroxide with water, draining the aqueous phase at the bottom, heating the solid isoborneol in the water washing and purification kettle and slowly heating it to 204-210 DEG C, and then obtaining liquid isoborneol; the present invention reduces previous process drawbacks, does not require a solvent to participate in the reaction, also reduces the troubles of solvent separation and residue, introduces microflow field technology, and has simpler reaction operation, shorter reaction time, and higher efficiency.

Description

Technical Field

[0001] The invention relates to the technical field of chemical products, in particular to a method for synthesizing isoborneol by utilizing microflow field technology. Background Art

[0002] Isoborneol, also known as isoborneol, is a forestry chemical product. It is a diastereomer of borneol and has properties similar to camphor. It is used as a fragrance in daily chemical products and as a preservative. White isoborneol, similar in appearance and properties to camphor, is a camphor intermediate and has broad application prospects.

[0003] At present, there are two production processes for synthesizing isoborneol. One is to use the method of camphene hydration, and the other is to obtain it by saponification of isoborneol acetate. At present, the saponification process of isoborneol acetate is selected as the mainstream process in China. It is generally obtained by adding isoborneol acetate to a non-polar solvent and sodium hydroxide solution. It is generally an intermittent kettle reaction. The process flow is relatively complicated and the efficiency is low. Some people also use a continuous reaction method, but polar solvents and non-polar solvents are introduced, and it is necessary to go through saponification, distillation, stratification, water washing, crystallization and other steps, and the process is also relatively complicated.

[0004] In response to the above problems, we provide a method for synthesizing isoborneol using microfluidic field technology to solve the above-mentioned methods. Summary of the Invention

[0005] The object of the present invention is to provide a method for synthesizing isoborneol using microfluidic field technology to solve the problems raised in the above background technology.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A method for synthesizing isoborneol using microfluidic field technology comprises the following steps:

[0008] Step 1, prepare isoborneol acetate and 50% liquid caustic soda respectively;

[0009] Step 2, the prepared isoborneol acetate and 50% liquid caustic soda are delivered to the microchannel reactor by a liquid delivery pump, and the reaction of the isoborneol acetate and 50% liquid caustic soda is completed by the microchannel reactor;

[0010] Step 3, the mixed solution after the reaction is completed in the microchannel reactor is sent to a water washing and purification kettle, the generated sodium acetate and the incompletely reacted sodium hydroxide are washed clean, the aqueous phase is drained at the bottom, and the solid isoborneol in the water washing and purification kettle is slowly heated to 204-210 ° C, and then liquid isoborneol can be obtained;

[0011] Step 4: transferring the obtained liquid isoborneol to a granulation device to obtain the finished isoborneol.

[0012] As a further solution of the present invention: in the step 2, when the microchannel reactor reacts isoborneol acetate and 50% liquid alkali, the reaction temperature is maintained at 205-250°C.

[0013] As a further solution of the present invention: in the step 2, when the microchannel reactor is reacting isoborneol acetate and 50% liquid alkali, the microchannel reactor is pressurized to 3-8 MPa.

[0014] The microchannel reactor comprises a base plate, a first microfluidic reaction plate being provided on one side of the upper end surface of the base plate, and a feeding assembly for feeding isoborneol acetate and 50% liquid caustic soda into the first microfluidic reaction plate;

[0015] The first microfluidic reaction plate is provided with a primary reaction component for performing a first reaction on isoborneol acetate and 50% liquid caustic soda;

[0016] A second microfluidic reaction plate and a third microfluidic reaction plate are further provided on the upper surface of the bottom plate in parallel with the first microfluidic reaction plate, and a conveying component for conveying the mixed liquid is provided between the first microfluidic reaction plate and the second microfluidic reaction plate;

[0017] A first connecting tube for communication is provided between the second microfluidic reaction plate and the third microfluidic reaction plate. Secondary reaction components for further reaction of the mixed solution are provided inside the second microfluidic reaction plate and the third microfluidic reaction plate. A sixth connecting tube for discharging the solution after the reaction is completed is provided at the lower end of the third microfluidic reaction plate.

[0018] As a further solution of the present invention: the feeding assembly includes a second material storage tank, which is arranged on one side of the upper end surface of the bottom plate, and a first material storage tank is provided on the other side of the upper end surface of the bottom plate, and the upper ends of the second material storage tank and the first material storage tank are both provided with a feed port, a second connecting pipe is connected between the discharge port at the lower end of the first material storage tank, a fifth connecting pipe is connected in the middle of the second connecting pipe, an end of the fifth connecting pipe away from the second connecting pipe is connected to a pre-filter, and the other port of the pre-filter is connected to a fourth connecting pipe, an end of the fourth connecting pipe away from the pre-filter is connected to the liquid inlet of the first microfluidic reaction plate, and a delivery pump is connected in series on the fifth connecting pipe.

[0019] As a further solution of the present invention: the primary reaction component includes a microfluidic chamber, which is respectively opened at two sides of the inside of the first microfluidic reaction plate, and a bottom connecting channel is provided between the bottoms of the two microfluidic chambers. A plurality of triangular blocks are provided inside the microfluidic chamber, and the triangular blocks in the two microfluidic chambers are arranged in opposite directions.

[0020] As a further solution of the present invention: the conveying assembly includes a rotating cylinder, the upper end surface of which is arranged on the bottom plate between the first microfluidic reaction plate and the second microfluidic reaction plate, the internal rotation of the rotating cylinder is connected to a screw rod, the upper end of the rotating cylinder is equipped with a motor for driving the screw rod to rotate, the bottom of the rotating cylinder is connected to a third connecting tube, the end of the third connecting tube away from the rotating cylinder is connected to the liquid outlet of the first microfluidic reaction plate, the upper end of the rotating cylinder is connected to a seventh connecting tube, the end of the seventh connecting tube away from the rotating cylinder is connected to the liquid inlet of the second microfluidic reaction plate, the bottom of the rotating cylinder is also connected to a sixth connecting tube, the upper end of the sixth connecting tube is connected to the seventh connecting tube, and a pumping pump is provided in series on the sixth connecting tube.

[0021] As a further solution of the present invention: the secondary reaction component includes a serpentine microfluidic channel, the serpentine microfluidic channel is opened inside the third microfluidic reaction plate, the horizontal part of the serpentine microfluidic channel is provided with a diamond-shaped dispersion block, and the vertical part on one side of the serpentine microfluidic channel is provided with a diverter.

[0022] As a further solution of the present invention: the diverter includes a bracket, which is fixedly connected to the inner wall of the serpentine microfluidic channel. A rotating shaft is rotatably connected in the bracket, and a plurality of guide blades are fixedly connected to the rotating shaft.

[0023] As a further solution of the present invention: the ends of the sixth connecting pipe and the feed port are both provided with connecting flanges.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] 1. The present invention reduces the disadvantages of previous processes, does not require solvents to participate in the reaction, and also reduces the troubles of solvent separation and residue. The introduction of micro-flow field technology makes the reaction operation simpler, the reaction time shorter, and the efficiency higher.

[0026] 2. The microchannel reactor proposed in the present invention can effectively realize the reaction of isoborneol acetate and 50% liquid caustic soda. At the same time, the primary reaction components and secondary reaction components of different structures are utilized to make the reaction more fully and thoroughly. During the reaction, the triangular block is utilized to continuously disperse and polymerize the mixed solution to achieve the preliminary reaction of the solution. The solution is then dispersed and polymerized again by the diamond-shaped dispersion block. The splitter provided at the same time rotates and mixes the solution, and the solution can be fully reacted under the action of the diamond-shaped dispersion block and the splitter. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a structural schematic diagram of the present invention.

[0028] Figure 2 It is a schematic diagram of the local structure of the present invention.

[0029] Figure 3 It is a schematic diagram of the internal structure of the rotating drum in the present invention.

[0030] Figure 4 Schematic diagram of the internal structure of the first microfluidic reaction plate in the present invention.

[0031] Figure 5 Schematic diagram of the internal structure of the third microfluidic reaction plate in the present invention.

[0032] Figure 6 Schematic diagram of the structure of the diverter in the present invention.

[0033] Wherein: 1. bottom plate; 2. first microfluidic reaction plate; 3. microfluidic chamber; 4. second microfluidic reaction plate; 5. third microfluidic reaction plate; 6. first connecting pipe; 7. feed port; 8. first storage tank; 9. second connecting pipe; 10. delivery pump; 11. triangular block; 12. second storage tank; 13. third connecting pipe; 14. pre-filter; 15. diamond-shaped dispersion block; 16. serpentine microfluidic channel; 17. flow divider; 19. fourth connecting pipe; 20. fifth connecting pipe; 21. sixth connecting pipe; 22. pumping pump; 23. seventh connecting pipe; 24. motor; 25. rotating cylinder; 26. screw rod; 27. bottom connecting channel

[0034] 171. Bracket; 172. Rotating shaft; 173. Guide blade. DETAILED DESCRIPTION

[0035] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0036] A method for synthesizing isoborneol using microfluidic field technology, characterized in that it comprises the following steps:

[0037] Step 1, prepare isoborneol acetate and 50% liquid caustic soda respectively;

[0038] Step 2, the prepared isoborneol acetate and 50% liquid caustic soda are delivered to the microchannel reactor using a liquid delivery pump, the reaction temperature is maintained at 205-250 ° C; and the pressure is increased to 3-8 MPa, and the reaction of isoborneol acetate and 50% liquid caustic soda is completed by the microchannel reactor;

[0039] Step 3, the mixed solution after the reaction is completed in the microchannel reactor is sent to a water washing and purification kettle, the generated sodium acetate and the incompletely reacted sodium hydroxide are washed clean, the aqueous phase is drained at the bottom, and the solid isoborneol in the water washing and purification kettle is slowly heated to 204-210 ° C, and then liquid isoborneol can be obtained;

[0040] Step 4: transferring the obtained liquid isoborneol to a granulation device to obtain the finished isoborneol.

[0041] The present invention reduces the disadvantages of previous processes, does not require solvents to participate in the reaction, and also reduces the problems of solvent separation and residue. The introduction of microfluidic field technology makes the reaction operation simpler, the reaction time shorter, and the efficiency higher.

[0042] See also Figures 1-6 In an embodiment of the present invention, a microchannel reactor comprises a base plate 1, a first microfluidic reaction plate 2 is provided on one side of the upper end surface of the base plate 1, and a feeding assembly for conveying isoborneol acetate and 50% liquid alkali to the interior of the first microfluidic reaction plate 2 is further provided on the base plate 1; the feeding assembly comprises a second storage tank 12, the second storage tank 12 is provided at a position on one side of the upper end surface of the base plate 1, a first storage tank 8 is provided on the other side of the upper end surface of the base plate 1, a feed port 7 is provided on the upper ends of the second storage tank 12 and the first storage tank 8, a second connecting pipe 9 is connected between the discharge port at the lower end of the first storage tank 8, a fifth connecting pipe 20 is connected in the middle of the second connecting pipe 9, and a pre-filter 1 is connected at one end of the fifth connecting pipe 20 away from the second connecting pipe 9 4. The other port of the pre-filter 14 is connected to a fourth communicating pipe 19, and one end of the fourth communicating pipe 19 away from the pre-filter 14 is connected to the liquid inlet of the first microfluidic reaction plate 2, and the fifth communicating pipe 20 is connected in series with a delivery pump 10; the ends of the sixth communicating pipe 21 and the feed port 7 are both provided with connecting flanges; during operation, the required isoborneol acetate and 50% liquid caustic soda are stored in the second storage tank 12 and the first storage tank 8, respectively, and then the isoborneol acetate and 50% liquid caustic soda are pumped to the third communicating pipe 13 by the delivery pump 10, and the isoborneol acetate and 50% liquid caustic soda enter the first microfluidic reaction plate 2, and the pre-filter 14 provided can filter the solution to prevent impurities from entering the first microfluidic reaction plate 2.

[0043] A primary reaction component for the first reaction of isoborneol acetate and 50% liquid alkali is provided inside the first microfluidic reaction plate 2; the primary reaction component includes a microfluidic chamber 3, which is respectively opened at positions on both sides of the inside of the first microfluidic reaction plate 2, and a bottom connecting channel 27 is provided between the bottoms of the two microfluidic chambers 3. A plurality of triangular blocks 11 are provided inside the microfluidic chamber 3, and the triangular blocks 11 in the two microfluidic chambers 3 are arranged in opposite directions; during operation, the solution is passed into the first microfluidic reaction plate 2 from the third connecting tube 13. After the solution enters the microfluidic chamber 3, it will be continuously dispersed and then polymerized by the triangular blocks 11, thereby reacting the solution.

[0044] The second microfluidic reaction plate 4 and the third microfluidic reaction plate 5 are also provided at a position side by side with the first microfluidic reaction plate 2 on the upper end surface of the bottom plate 1, and a conveying component for conveying the mixed liquid is provided between the first microfluidic reaction plate 2 and the second microfluidic reaction plate 4; the conveying component includes a rotating cylinder 25, and the rotating cylinder 25 is provided at a position between the first microfluidic reaction plate 2 and the second microfluidic reaction plate 4 on the upper end surface of the bottom plate 1, and a screw rod 26 is rotatably connected inside the rotating cylinder 25, and a motor 24 for driving the screw rod 26 to rotate is installed on the upper end of the rotating cylinder 25, and a third connecting pipe 13 is connected to the bottom of the rotating cylinder 25, and the end of the third connecting pipe 13 away from the rotating cylinder 25 is connected to the liquid outlet of the first microfluidic reaction plate 2, and the upper end of the rotating cylinder 25 is connected to the liquid outlet of the first microfluidic reaction plate 2. The end is connected to a seventh connecting tube 23, and the end of the seventh connecting tube 23 away from the rotating cylinder 25 is connected to the liquid inlet of the second microfluidic reaction plate 4. The bottom of the rotating cylinder 25 is also connected to a sixth connecting tube 21, and the upper end of the sixth connecting tube 21 is connected to the seventh connecting tube 23. The sixth connecting tube 21 is connected in series with a pumping pump 22; during operation, the motor 24 drives the screw rod 26 to rotate, and the rotation of the screw rod 26 can drive the incoming solution to stir, and the solution inside the rotating cylinder 25 will be discharged from the seventh connecting tube 23 to the inside of the second microfluidic reaction plate 4 under the subsequent liquid pressure. The sixth connecting tube 21 and the pumping pump 22 are set at the same time, which can pump the solution at the bottom of the rotating cylinder 25 to the seventh connecting tube 23 when in use, so as to facilitate the emptying of the rotating cylinder 25.

[0045] A first connecting pipe 6 for communication is provided between the second microfluidic reaction plate 4 and the third microfluidic reaction plate 5. A secondary reaction component for further reacting the mixed solution is provided inside the second microfluidic reaction plate 4 and the third microfluidic reaction plate 5. A sixth connecting pipe 21 for discharging the solution after the reaction is completed is provided at the lower end of the third microfluidic reaction plate 5; the secondary reaction component includes a serpentine microfluidic channel 16, which is opened inside the third microfluidic reaction plate 5. A diamond-shaped dispersion block 15 is provided in the horizontal part of the serpentine microfluidic channel 16, and a diverter 17 is provided in the vertical part on one side of the serpentine microfluidic channel 16. During operation, the solution flows along the serpentine microfluidic channel 16, and then the solution is dispersed by the diamond-shaped dispersion block 15, and then aggregated. At the same time, when passing through the diverter 17, the solution is rotated by the diverter 17 for mixing and reacting again. The full reaction of the solution can be achieved by setting multiple groups of diamond-shaped dispersion blocks 15 and diverters 17.

[0046] The diverter 17 includes a bracket 171, which is fixedly connected to the inner wall of the serpentine microfluidic channel 16. A rotating shaft 172 is rotatably connected to the bracket 171, and a plurality of guide blades 173 are fixedly connected to the rotating shaft 172. During operation, the solution flushes the guide blades 173 to rotate the guide blades 173, and at the same time, the corresponding solution will also rotate and flow under the action of the guide blades 173, thereby achieving a more complete reaction.

[0047] The working principle of the present invention is as follows: during operation, the required isoborneol acetate and 50% liquid caustic soda are stored in the second storage tank 12 and the first storage tank 8 respectively, and then the isoborneol acetate and 50% liquid caustic soda are pumped to the third connecting pipe 13 by the delivery pump 10, and the isoborneol acetate and 50% liquid caustic soda enter the first microfluidic reaction plate 2. The pre-filter 14 provided can filter the solution to prevent impurities from entering the first microfluidic reaction plate 2. The solution is passed from the third connecting pipe 13 to the first microfluidic reaction plate 2. After the solution enters the microfluidic cavity 3, it will be filtered by the triangular block 1 1 is continuously dispersed and then aggregated, thereby reacting the solution. The motor 24 drives the screw rod 26 to rotate. The rotation of the screw rod 26 can drive the incoming solution to stir. The solution inside the rotating cylinder 25 will be discharged from the seventh connecting pipe 23 to the inside of the second microfluidic reaction plate 4 under the subsequent liquid pressure. The solution flows along the serpentine microfluidic channel 16, and then the solution is dispersed by the diamond-shaped dispersion block 15, and then aggregated. At the same time, when passing through the diverter 17, the solution is rotated by the diverter 17 to mix and react again. By setting up multiple groups of diamond-shaped dispersion blocks 15 and diverters 17, the solution can be fully reacted.

[0048] It is obvious to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Although this specification describes the embodiments, not every embodiment contains only one technical solution. This description is for clarity only. Those skilled in the art should read the specification as a whole. The technical solutions in the various embodiments can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A microchannel reactor for synthesizing isoborneol using microfluidic field technology, characterized in that: The invention comprises a base plate (1), wherein a first microfluidic reaction plate (2) is provided on one side of an upper end surface of the base plate (1), and a feeding component for feeding isoborneol acetate and 50% liquid caustic soda into the first microfluidic reaction plate (2) is also provided on the base plate (1); The first microfluidic reaction plate (2) is provided with a primary reaction component for performing a first reaction on isoborneol acetate and 50% liquid alkali; A second microfluidic reaction plate (4) and a third microfluidic reaction plate (5) are further provided on the upper end surface of the bottom plate (1) and arranged side by side with the first microfluidic reaction plate (2); a conveying assembly for conveying a mixed liquid is provided between the first microfluidic reaction plate (2) and the second microfluidic reaction plate (4); A first connecting pipe (6) for communication is provided between the second microfluidic reaction plate (4) and the third microfluidic reaction plate (5); a secondary reaction component for further reacting the mixed solution is provided inside the second microfluidic reaction plate (4) and the third microfluidic reaction plate (5); and a sixth connecting pipe (21) for discharging the solution after the reaction is completed is provided at the lower end of the third microfluidic reaction plate (5).

2. The microchannel reactor according to claim 1, characterized in that The feeding assembly includes a second material storage tank (12), the second material storage tank (12) is arranged at a position on one side of the upper end surface of the bottom plate (1), and a first material storage tank (8) is arranged on the other side of the upper end surface of the bottom plate (1), the upper ends of the second material storage tank (12) and the first material storage tank (8) are both provided with a feed port (7), a second connecting pipe (9) is connected between the discharge port at the lower end of the first material storage tank (8), a fifth connecting pipe (20) is connected in the middle of the second connecting pipe (9), the end of the fifth connecting pipe (20) away from the second connecting pipe (9) is connected to a pre-filter (14), the other end of the pre-filter (14) is connected to a fourth connecting pipe (19), the end of the fourth connecting pipe (19) away from the pre-filter (14) is connected to the liquid inlet of the first microfluidic reaction plate (2), and a delivery pump (10) is connected in series to the fifth connecting pipe (20).

3. The microchannel reactor according to claim 2, characterized in that The primary reaction component comprises a microfluidic chamber (3), wherein the microfluidic chamber (3) is respectively provided at positions on both sides of the interior of the first microfluidic reaction plate (2), a bottom connecting channel (27) is provided between the bottoms of the two microfluidic chambers (3), and a plurality of triangular blocks (11) are provided inside each of the microfluidic chambers (3), and the triangular blocks (11) in the two microfluidic chambers (3) are arranged in opposite directions.

4. The microchannel reactor according to claim 3, characterized in that The conveying assembly includes a rotating cylinder (25), which is arranged on the upper end surface of the bottom plate (1) between the first microfluidic reaction plate (2) and the second microfluidic reaction plate (4), and a screw rod (26) is rotatably connected inside the rotating cylinder (25). A motor (24) for driving the screw rod (26) to rotate is installed on the upper end of the rotating cylinder (25). The bottom of the rotating cylinder (25) is connected to a third connecting pipe (13), and the third connecting pipe (13) is away from the rotating cylinder. One end of the cylinder (25) is connected to the liquid outlet of the first microfluidic reaction plate (2), the upper end of the rotating cylinder (25) is connected to the seventh connecting tube (23), the end of the seventh connecting tube (23) away from the rotating cylinder (25) is connected to the liquid inlet of the second microfluidic reaction plate (4), the bottom of the rotating cylinder (25) is also connected to the sixth connecting tube (21), the upper end of the sixth connecting tube (21) is connected to the seventh connecting tube (23), and the sixth connecting tube (21) is provided with a pumping pump (22) in series.

5. The microchannel reactor according to claim 4, characterized in that The secondary reaction component includes a serpentine microfluidic channel (16), which is opened inside the third microfluidic reaction plate (5), and a diamond-shaped dispersion block (15) is provided in the horizontal part of the serpentine microfluidic channel (16), and a diverter (17) is provided in the vertical part on one side of the serpentine microfluidic channel (16).

6. The microchannel reactor according to claim 5, characterized in that The diverter (17) includes a bracket (171), the bracket (171) is fixedly connected to the inner wall of the serpentine microfluidic channel (16), a rotating shaft (172) is rotatably connected inside the bracket (171), and a plurality of guide blades (173) are fixedly connected to the rotating shaft (172).

7. The microchannel reactor according to claim 6, characterized in that The ends of the sixth connecting pipe (21) and the feed port (7) are both provided with connecting flanges.

8. A method for synthesizing isoborneol using microfluidic field technology, characterized in that: The microchannel reactor according to claim 7 specifically comprises the following steps: Step 1, prepare isoborneol acetate and 50% liquid caustic soda respectively; Step 2, the prepared isoborneol acetate and 50% liquid caustic soda are delivered to the microchannel reactor by a liquid delivery pump, and the reaction of the isoborneol acetate and 50% liquid caustic soda is completed by the microchannel reactor; Step 3, the mixed solution after the reaction is completed in the microchannel reactor is sent to a water washing and purification kettle, the generated sodium acetate and the incompletely reacted sodium hydroxide are washed clean, the aqueous phase is drained at the bottom, and the solid isoborneol in the water washing and purification kettle is slowly heated to 204-210 ° C, and then liquid isoborneol can be obtained; Step 4, transferring the obtained liquid isoborneol to a granulation device to obtain the finished product isoborneol; In the step 2, when the microchannel reactor reacts isoborneol acetate and 50% liquid caustic soda, the reaction temperature is maintained at 205-250° C.; In the step 2, when the microchannel reactor is reacting isoborneol acetate and 50% liquid alkali, the microchannel reactor is pressurized to 3-8 MPa.

Images