Oxidation reaction device of Wauteaub oxide

Abstract

The oxidation reaction device comprises a reaction kettle, a stirring mechanism, a paddling mechanism and an oscillating mechanism which are used for homogenizing reaction materials are arranged in the reaction kettle, and a driving mechanism is arranged on the reaction kettle; the stirring mechanism comprises an impeller and a plurality of stirring blades, the paddling mechanism comprises a plurality of blades, the driving mechanism is used for driving the impeller and the stirring blades to rotate and drive the blades to swing, the impeller and the stirring blades stir reaction materials through self rotation, and the blades push the reaction materials to flow circularly through self swing. The oscillating mechanism comprises a plurality of elastic pieces arranged on the oscillating path of the blades, and the blades generate vibration by shifting the elastic pieces so as to oscillate the reaction materials. When the reaction kettle is used for oxidation reaction, materials can be fully and effectively homogenized and dispersed by stirring, stirring and vibrating the materials, so that a reaction substrate, an oxidizing agent and a catalyst are fully contacted, and the product conversion rate and yield brought by the reaction are higher.

Description

Technical Field

[0001] The present invention relates to the technical field of Wo's oxidation reaction devices, in particular to an oxidation reaction device for Wo's oxide. Background Art

[0002] Walter's oxide, chemical name: 16,17α-epoxy-4-pregnene-3,20-dione, Walter's oxide has the parent nucleus of cyclopentane-perhydrophenanthrene, is a typical steroid compound, and is an important intermediate for the synthesis of various corticosteroid drugs.

[0003] To prepare Wo's oxide, it is necessary to first use diene ketone acetate as a reaction substrate, add hydrogen peroxide and alkaline solution to carry out an epoxidation reaction to obtain an oxygen bridge product. After the oxygen bridge product is concentrated, a Wo's oxidation reaction is carried out using the oxygen bridge product as a reaction substrate, cyclohexanone as an oxidant, and aluminum isopropoxide as a catalyst. After that, sodium hydroxide is added to destroy the aluminum isopropoxide, and the product is concentrated under reduced pressure, centrifuged, filtered, and dried to obtain the product. During the above-mentioned Wo's oxidation reaction, sufficient material agitation can significantly improve the reaction effect and reduce the production of by-products. This is because the uniform distribution of materials ensures that all areas in the reaction tank maintain ideal reaction conditions, thereby improving the efficiency and selectivity of the reaction. In addition, it can also promote the timely mixing and diffusion of the former when sodium hydroxide is subsequently added to destroy the aluminum isopropoxide, thereby accelerating the contact between the two and increasing the rate of this process.

[0004] After searching, the Chinese invention patent with publication number CN105289426B discloses an oxidation reaction device, including a self-priming stirred reactor, a condenser and an oxygen supply device. The self-priming stirred reactor includes a reactor body, an oxygen inlet chamber, a motor, a hollow shaft, a centrifugal impeller and a stirring impeller. The oxygen inlet chamber is sealed and fixed in the top of the reactor body. The upper end of the hollow shaft passes through the oxygen inlet chamber and is connected to the motor fixed on the reactor body. The centrifugal impeller is sleeved in the middle of the hollow shaft. The centrifugal impeller is provided with a feed hole and a discharge port. The feed hole is connected to the oxygen inlet chamber through the hollow shaft; the stirring impeller is sleeved at the lower end of the hollow shaft; and the oxygen supply device is connected to the oxygen inlet chamber in the self-priming stirred reactor. This application uses a stirred reactor to assist the oxidation reaction, but its stirring method is relatively simple, so the mixing effect it can bring is limited, which makes it difficult to homogenize and disperse the reaction materials in time, thereby resulting in insufficient product conversion rate and yield brought by the reaction. Summary of the Invention

[0005] In view of the above-mentioned prior art, the present invention provides an oxidation reaction device for Woshi oxide, and the main technical problem to be solved is how to improve the reaction efficiency.

[0006] To achieve the above-mentioned purpose, the technical solution of the embodiment of the present invention is implemented as follows: A Woshi oxide oxidation reaction device comprises a reactor, wherein the reactor is provided with a stirring mechanism, a rowing mechanism and an oscillating mechanism for homogenizing the reaction materials, and the reactor is provided with a driving mechanism; The stirring mechanism includes an impeller and several stirring blades, the paddling mechanism includes several blades, the driving mechanism is used to drive the impeller and stirring blades to rotate and drive the blades to swing, the impeller and stirring blades stir the reaction materials by their own rotation, and the blades push the reaction materials to circulate by their own swinging, and the oscillation mechanism includes several springs arranged on the swinging path of the blades, and the blades generate vibrations by prying the springs to oscillate the reaction materials.

[0007] Furthermore, a first through hole is provided at the bottom end of the reactor, and the reactor is rotatably connected to a central axis at the first through hole. Notches are provided at both ends of the outside of the rod body of the central axis in the reactor, and the central axis is fixedly connected to a reciprocating screw at the two notches. The top inner wall and the bottom end of the reactor are respectively fixedly connected to sleeves on the outside of the two reciprocating screws, and a number of support rods are equidistantly rotatably connected to the outside of the sleeve.

[0008] Furthermore, the outside of the two reciprocating screws are threadedly connected to a nut, and the outside of the nut is equidistantly connected to a number of connecting rods. The outside of the sleeve is equidistantly provided with a number of strip openings. The number of connecting rods and strip openings is the same and corresponds one to one. One end of the connecting rod extends to the outside of the sleeve at the strip opening, and one end of the connecting rod is rotatably connected to the blade, and the top of the blade is fixedly connected to the support rod.

[0009] Furthermore, the impeller is fixedly connected to the outside of the rod body of the central axis, and several support rods are fixedly connected to the outside of the impeller at equal intervals. The number of stirring blades is the same as the number of support rods and corresponds one to one. The stirring blade is fixedly connected to one end of the support rod, and the stirring blade is arc-shaped. The spring piece is fixedly connected to the inner wall of the reactor.

[0010] Furthermore, the spring piece is fixedly connected to the inner wall of the reactor, a base is provided under the reactor, and several brackets are fixedly connected to the base at equal distances between the base and the reactor. A second through hole is provided on one side of the top of the base, and the base is fixedly connected to the casing at the second through hole. The driving mechanism includes a first motor arranged in the casing, and the bottom end of the output shaft of the first motor extends into the base at the second through hole.

[0011] Furthermore, the bottom end of the output shaft of the first motor is connected to the driving wheel through a key, the top of the base is provided with a third through hole below the reactor, the bottom end of the central axis extends into the base at the third through hole, and the outside of the rod body of the central axis in the base is connected to the driven wheel through a key, the outside of the driven wheel and the driving wheel are covered with the same belt, and the diameter of the driving wheel is smaller than the diameter of the driven wheel.

[0012] Furthermore, a control box is fixedly connected to the top of the reactor, and fourth through holes are opened at both ends of one side of the control box. The control box is rotatably connected to a rotating shaft and a connecting shaft at the two fourth through holes respectively. The rotating shaft and the connecting shaft are connected to eccentric rollers on the outside of the rod body in the control box through keys, and the two eccentric rollers are mirror-symmetrical.

[0013] Furthermore, a liquid inlet is provided at the top of the control box, a material pipe is fixedly connected to the control box at the liquid inlet, a hose is fixedly connected to the bottom end of the material pipe, the hose is located between the two eccentric rollers, and a liquid inlet hole is provided at the top of the reactor on the inner side of the control box, the hose extends to the interior of the control box at the liquid inlet hole, and the hose is laid along the inner wall of the reactor.

[0014] Furthermore, the rotating shaft and the eccentric roller are both connected to gears at one end outside the control box through a key, and the two gears are meshed with each other. A fifth through hole is opened on the other side of the control box, and the side wall of the control box is fixedly connected to a cover outside the fifth through hole. The other end of the rotating shaft extends into the control box at the fifth through hole, and a second motor is fixedly connected to the cover, and the output shaft of the second motor is fixedly connected to the rotating shaft.

[0015] Furthermore, an elbow is provided at one end of the blade away from the sleeve, and the elbow is in an inwardly curved arc.

[0016] The beneficial effects of the present invention are: 1. When the oxidation reaction is carried out in a reactor, the rotation of the impeller and the stirring blades can be used to stir the reaction materials. At the same time, the deflection of the blades can also shift the flow of materials in different areas of the reactor. In addition, during the deflection movement of the blades, they can also push the shrapnel to make it vibrate under the action of its own elastic force, thereby shaking the materials. The above stirring, shifting and shaking can fully and effectively homogenize and disperse the materials, so that the reaction substrate, oxidant and catalyst are fully in contact with each other, and the product conversion rate and yield brought about by the reaction are higher. In addition, after sodium hydroxide is added to the reactor, it can promote its rapid mixing and dispersion, thereby increasing the rate of the process of using it to destroy aluminum isopropoxide; 2. By setting up two mirror-symmetrical eccentric rollers, the two rollers rotate synchronously and in opposite directions, which can intermittently squeeze the hose, so that the process of adding sodium hydroxide into the reactor can be slowed down, thereby providing sufficient stirring time for its dispersion and mixing in the reaction materials, thereby ensuring the mass transfer effect and improving the contact efficiency between sodium hydroxide and aluminum isopropoxide; 3. By setting an elbow at the end of the blade, when the blade in this state deflects in the reaction material, it can generate a stronger composite liquid flow in addition to the tangential flow, thereby further promoting the uniform mixing of the reaction materials, thereby further ensuring the reaction rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 A perspective view of an oxidation reaction device for Woshi oxide in Example 1 of the present application; Figure 2 This is a cross-sectional view of an oxidation reaction device for Woshi oxide in Example 1 of the present application; Figure 3 This is an exploded view of a control box of an oxidation reaction device for Woshi oxide in Example 1 of the present application; Figure 4 This is a cross-sectional view of a control box of an oxidation reaction device for Woshi oxide in Example 1 of the present application; Figure 5 This is a cross-sectional view of an oxidation reaction device for Woshi oxide in Example 2 of the present application.

[0018] Description of Figure Numbers: Reactor 1, casing 2, first motor 201, base 3, bracket 4, feed pipe 5, hose 501, control box 6, cover 601, second motor 602, driving pulley 7, belt 8, driven pulley 9, impeller 10, support rod 11, stirring blade 12, spring 13, sleeve 14, support rod 15, blade 16, elbow 1601, connecting rod 17, nut 18, central shaft 19, reciprocating screw 1901, rotating shaft 20, eccentric roller 21, connecting shaft 22, gear 23. DETAILED DESCRIPTION

[0019] The technical solutions of the present invention are further described in detail below with reference to the accompanying drawings and specific embodiments. Unless otherwise defined, all technical and scientific terms used herein have the same meanings as those commonly understood by those skilled in the art to which the present invention pertains. The terms used in the present invention description are for the purpose of describing specific embodiments only and are not intended to limit the present invention.

[0020] Example 1 Refer to the attached Figure 1-4 The present application provides an oxidation reaction device for Wo's oxide, comprising a reactor 1, wherein the reactor 1 is provided with a stirring mechanism, a rowing mechanism and an oscillating mechanism for homogenizing the reaction materials, and the reactor 1 is provided with a driving mechanism; The stirring mechanism includes an impeller 10 and several stirring blades 12, the paddling mechanism includes several blades 16, the driving mechanism is used to drive the impeller 10 and the stirring blades 12 to rotate and drive the blades 16 to swing, the impeller 10 and the stirring blades 12 stir the reaction materials by their own rotation, and the blades 16 push the reaction materials to circulate by their own swinging, and the oscillation mechanism includes several springs 13 arranged on the swinging path of the blades 16, and the blades 16 generate vibrations by prying the springs 13 to oscillate the reaction materials.

[0021] Preferably, the bottom end of the output shaft of the first motor 201 is connected to the driving wheel 7 through a key, and the top of the base 3 is provided with a third through hole below the reactor 1. The bottom end of the central axis 19 extends into the base 3 at the third through hole, and the central axis 19 is located in the base 3. The outside of the rod body is connected to the driven wheel 9 through a key, and the driven wheel 9 and the driving wheel 7 are covered with the same belt 8. The diameter of the driving wheel 7 is smaller than the diameter of the driven wheel 9. The large-diameter driven wheel 9 is driven to rotate by the small-diameter driving wheel 7, which not only saves effort to reduce the load of the first motor 201, but also has a deceleration effect to avoid excessive agitation of the material in the reactor 1.

[0022] When using this device for oxidation reaction, the substrate, catalyst and oxidant can be put into the reactor 1, and then the first motor 201 is started to drive the driving wheel 7 to rotate. The driving wheel 7 drives the driven wheel 9 to rotate through the belt 8, and the driven wheel 9 can drive the central shaft 19 and the reciprocating screw 1901 to rotate. The central shaft 19 can drive the impeller 10 to rotate to make the material produce a vortex, and the impeller 10 drives the stirring blade 12 to rotate through the support rod 11, and can also shear and disperse the material, so as to stir the reaction material to achieve a homogenization effect. A heating tube is also provided in the reactor 1 to provide the reaction material with the temperature required for the reaction.

[0023] Preferably, a first through hole is provided at the bottom end of the reactor 1, and the reactor 1 is rotatably connected to a central axis 19 at the first through hole. Notches are provided at both ends of the outside of the rod body of the central axis 19 in the reactor 1, and the central axis 19 is fixedly connected to a reciprocating screw 1901 at the two notches. The top inner wall and the bottom end of the reactor 1 are respectively fixedly connected to the outside of the two reciprocating screws 1901 with a sleeve 14, and a plurality of support rods 15 are rotatably connected to the outside of the sleeve 14 at equal intervals.

[0024] Preferably, the outside of the two reciprocating screws 1901 are both threadedly connected to a nut 18, and the outside of the nut 18 is equidistantly connected to a number of connecting rods 17. The outside of the sleeve 14 is equidistantly provided with a number of strip openings, and the number of connecting rods 17 and the number of strip openings are the same and correspond one to one. One end of the connecting rod 17 extends to the outside of the sleeve 14 at the strip opening, and one end of the connecting rod 17 is rotatably connected to the blade 16, and the top of the blade 16 is fixedly connected to the support rod 15.

[0025] At the same time, the rotation of the reciprocating screw 1901 can drive the nut 18 to reciprocate in the vertical direction, and the nut 18 can push and pull the blade 16 through the connecting rod 17, so it can drive the blade 16 to produce a deflected reciprocating motion. Therefore, the movement of the blade 16 in the reaction material can be used to promote the circulation of materials at different positions in the reactor 1, so that the material can be more fully stirred and dispersed.

[0026] Preferably, the impeller 10 is fixedly connected to the outside of the rod body of the central axis 19. A number of support rods 11 are fixedly connected to the outside of the impeller 10 at equal intervals. The number of stirring blades 12 is the same as the number of support rods 11 and corresponds one to one. The stirring blades 12 are fixedly connected to one end of the support rods 11. The stirring blades 12 are arc-shaped, and the springs 13 are fixedly connected to the inner wall of the reactor 1. The rotation of the impeller 10 can induce a vortex in the material in the reactor 1, and the stirring blades 12 can shear and disperse the material on this basis.

[0027] Preferably, the spring piece 13 is fixedly connected to the inner wall of the reactor 1, a base 3 is provided under the reactor 1, and a plurality of brackets 4 are fixedly connected to the base 3 and the reactor 1 at equal intervals. A second through hole is provided on one side of the top of the base 3, and the base 3 is fixedly connected to the housing 2 at the second through hole. The driving mechanism includes a first motor 201 arranged in the housing 2, and the bottom end of the output shaft of the first motor 201 extends into the base 3 at the second through hole.

[0028] Moreover, during the deflection movement of the blade 16, the blade 16 can also push the spring 13 to cause it to produce elastic deformation, and after the blade 16 continues to move until it separates from the spring 13, the spring 13 can vibrate through its own elastic force, thereby vibrating the material to further ensure the effect of homogenizing the material; by stirring, paddling and vibrating the reaction material, the material can be fully homogenized and dispersed, thereby improving the reaction efficiency and making the product conversion rate and yield brought by the reaction higher.

[0029] Preferably, a control box 6 is fixedly connected to the top of the reactor 1, and fourth through holes are opened at both ends of one side of the control box 6. The control box 6 is rotatably connected to a rotating shaft 20 and a connecting shaft 22 at the two fourth through holes respectively. The rotating shaft 20 and the connecting shaft 22 are connected to eccentric rollers 21 on the outside of the rod body in the control box 6 through keys, and the two eccentric rollers 21 are mirror-symmetrical.

[0030] Preferably, a liquid inlet is provided at the top of the control box 6, and the control box 6 is fixedly connected to the liquid inlet with a material pipe 5, and the bottom end of the material pipe 5 is fixedly connected with a hose 501, and the hose 501 is located between the two eccentric rollers 21. A liquid inlet hole is provided at the top of the reactor 1 on the inner side of the control box 6, and the hose 501 extends to the interior of the control box 6 at the liquid inlet hole, and the hose 501 is arranged along the inner wall of the reactor 1.

[0031] Preferably, the rotating shaft 20 and the eccentric roller 21 are both connected to a gear 23 at one end outside the control box 6 through a key, and the two gears 23 are meshed with each other. A fifth through hole is opened on the other side of the control box 6, and the side wall of the control box 6 is fixedly connected to a cover 601 outside the fifth through hole. The other end of the rotating shaft 20 extends into the control box 6 at the fifth through hole, and a second motor 602 is fixedly connected to the cover 601, and the output shaft of the second motor 602 is fixedly connected to the rotating shaft 20.

[0032] In addition, when sodium hydroxide is added to the reactor 1 from the feed pipe 5, the second motor 602 can be started to drive the rotating shaft 20 to rotate. The rotating shaft 20 can drive the connecting shaft 22 to rotate through two gears 23, and the rotating shaft 20 and the connecting shaft 22 can drive the two eccentric rollers 21 to rotate synchronously and in opposite directions. Since the hose 501 can be squeezed intermittently during the rotation of the two eccentric rollers 21, the process of supplying sodium hydroxide by the hose 501 can be carried out intermittently, so that sufficient time can be provided for the process of whipping the reaction materials to evenly disperse the sodium hydroxide, so as to increase its contact efficiency with aluminum isopropylate and make it more sufficient to destroy aluminum propoxide.

[0033] Example 2 Refer to the attached Figure 5 The present application provides an oxidation reaction device for Wo's oxide. Compared with Example 1, in order to further ensure uniform mixing of the reaction materials, an elbow 1601 is provided at the end of the blade 16 away from the sleeve 14, and the elbow 1601 is in an inwardly curved arc.

[0034] During the reciprocating motion of the blade 16, since the elbow 1601 has greater resistance, it can generate a stronger composite liquid flow in addition to the tangential flow, thereby further ensuring the uniform mixing of the reaction materials, thereby further ensuring the reaction rate and product conversion rate.

[0035] The above are merely specific embodiments of the present invention, but the scope of protection of the present invention is not limited thereto. Any modifications or substitutions that can be easily conceived by a person skilled in the art within the technical scope disclosed in this invention should be included in the scope of protection of the present invention. The scope of protection of the present invention should be based on the scope of protection of the claims.

Claims

1. A Woshi oxide oxidation reaction device, comprising a reactor (1), characterized in that: The reactor (1) is provided with a stirring mechanism, a rowing mechanism and an oscillating mechanism for homogenizing the reaction materials, and the reactor (1) is provided with a driving mechanism; The stirring mechanism includes an impeller (10) and a plurality of stirring blades (12); the paddling mechanism includes a plurality of blades (16); the driving mechanism is used to drive the impeller (10) and the stirring blades (12) to rotate and drive the blades (16) to swing; the impeller (10) and the stirring blades (12) stir the reaction material by rotating themselves; the blades (16) push the reaction material to circulate by swinging themselves; the oscillation mechanism includes a plurality of springs (13) arranged on the swinging path of the blades (16); the blades (16) generate vibrations by paddling the springs (13) to oscillate the reaction material.

2. The oxidation reaction device of Woshi oxide according to claim 1, characterized in that: The bottom end of the reactor (1) is provided with a first through hole, and the reactor (1) is rotatably connected to a central shaft (19) at the first through hole. The central shaft (19) is provided with notches at both ends of the outside of the rod body in the reactor (1). The central shaft (19) is fixedly connected to a reciprocating screw (1901) at the two notches. The top inner wall and the bottom end of the reactor (1) are respectively fixedly connected to sleeves (14) at the outside of the two reciprocating screws (1901). The outer side of the sleeve (14) is rotatably connected to a plurality of support rods (15) at equal intervals.

3. The oxidation reaction device of Woshi oxide according to claim 2, characterized in that: The exteriors of the two reciprocating screws (1901) are both threadedly connected to a nut (18), and the exteriors of the nut (18) are equidistantly rotatably connected to a plurality of connecting rods (17). The exterior of the sleeve (14) is equidistantly provided with a plurality of strip-shaped openings, and the number of the connecting rods (17) is the same as that of the strip-shaped openings and corresponds one to one. One end of the connecting rod (17) extends to the exterior of the sleeve (14) at the strip-shaped opening, and one end of the connecting rod (17) is rotatably connected to the blade (16), and the top end of the blade (16) is fixedly connected to the support rod (15).

4. The oxidation reaction device of Woshi oxide according to claim 3, characterized in that: The impeller (10) is fixedly connected to the outside of the rod body of the central axis (19), and a plurality of support rods (11) are fixedly connected to the outside of the impeller (10) at equal intervals. The number of the stirring blades (12) is the same as the number of the support rods (11) and corresponds one to one. The stirring blades (12) are fixedly connected to one end of the support rods (11), and the stirring blades (12) are arc-shaped. The springs (13) are fixedly connected to the inner wall of the reactor (1).

5. The oxidation reaction device of Woshi oxide according to claim 4, characterized in that: The spring piece (13) is fixedly connected to the inner wall of the reactor (1); a base (3) is provided below the reactor (1); a plurality of brackets (4) are fixedly connected to the base (3) and the reactor (1) at equal intervals; a second through hole is provided at one side of the top end of the base (3); the base (3) is fixedly connected to the housing (2) at the second through hole; the driving mechanism comprises a first motor (201) provided in the housing (2); the bottom end of the output shaft of the first motor (201) extends into the base (3) at the second through hole.

6. The oxidation reaction device of Woshi oxide according to claim 5, characterized in that: The bottom end of the output shaft of the first motor (201) is connected to a driving wheel (7) via a key, the top end of the base (3) is provided with a third through hole below the reactor (1), the bottom end of the central shaft (19) extends into the base (3) at the third through hole, the outside of the rod body of the central shaft (19) in the base (3) is connected to a driven wheel (9) via a key, the outside of the driven wheel (9) and the driving wheel (7) are provided with a same belt (8), and the diameter of the driving wheel (7) is smaller than the diameter of the driven wheel (9).

7. The oxidation reaction device of Woshi oxide according to claim 1, characterized in that: The top of the reactor (1) is fixedly connected to a control box (6), and fourth through holes are provided at both ends of one side of the control box (6). The control box (6) is rotatably connected to a rotating shaft (20) and a connecting shaft (22) at the two fourth through holes, respectively. The rotating shaft (20) and the connecting shaft (22) are connected to eccentric rollers (21) outside the rod body in the control box (6) through a key, and the two eccentric rollers (21) are mirror-symmetrical.

8. The oxidation reaction device of Woshi oxide according to claim 7, characterized in that: The top of the control box (6) is provided with a liquid inlet, the control box (6) is fixedly connected to a material pipe (5) at the liquid inlet, the bottom of the material pipe (5) is fixedly connected to a hose (501), the hose (501) is located between two eccentric rollers (21), the top of the reactor (1) is provided with a liquid inlet hole on the inner side of the control box (6), the hose (501) extends to the interior of the control box (6) at the liquid inlet hole, and the hose (501) is arranged along the inner wall of the reactor (1).

9. The oxidation reaction device of Woshi oxide according to claim 8, characterized in that: The rotating shaft (20) and the eccentric roller (21) are both connected to a gear (23) at one end outside the control box (6) through a key, and the two gears (23) are meshed with each other. A fifth through hole is provided on the other side of the control box (6), and a cover (601) is fixedly connected to the side wall of the control box (6) outside the fifth through hole. The other end of the rotating shaft (20) extends into the control box (6) at the fifth through hole, and a second motor (602) is fixedly connected to the cover (601), and an output shaft of the second motor (602) is fixedly connected to the rotating shaft (20).

10. The oxidation reaction device of Woshi oxide according to claim 1, characterized in that: An elbow (1601) is provided at one end of the blade (16) away from the sleeve (14), and the elbow (1601) is in an inwardly curved arc shape.

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