Continuous hydrogenation device for 1, 3-cyclohexanedione

Abstract

The invention relates to a continuous hydrogenation device for 1, 3-cyclohexanedione, which comprises a kettle body of a reaction kettle, a vertical stirring shaft is arranged in the kettle body, the stirring shaft comprises a hollow rotating shaft, a gas outlet impeller is arranged in the middle of the hollow rotating shaft, and a dispersion impeller is arranged at the bottom of the hollow rotating shaft; the dispersion impeller comprises a conical wheel disc, the wheel disc is fixed to the hollow rotating shaft in an inserted and sleeved mode, a plurality of annularly-distributed rib plates are formed on the inner wall of the wheel disc, a plurality of stirring blade handles are fixedly connected to the outer wall of the wheel disc, and stirring blades are fixedly connected to the outer ends of the stirring blade handles; the air outlet impeller comprises an air guide wheel which is fixed to the hollow rotating shaft in an inserted and sleeved mode and communicated with the hollow rotating shaft, an arc-shaped air outlet pipe is fixedly connected to the outer wall of the air guide wheel, and the air outlet pipe is communicated with an inner cavity of the air guide wheel and annularly and evenly distributed around the central axis of the air guide wheel. According to the device, a stirring and hydrogenation structure in the hydrogenation reaction kettle is optimally designed, and the efficiency of dissolving hydrogen into reaction liquid can be improved, so that sufficient hydrogen reaction can be realized, and the yield of 1, 3-cyclohexanedione is improved.

Description

Technical field:

[0001] The invention relates to the technical field of machining equipment, and more specifically to a continuous hydrogenation device for 1,3-cyclohexanedione. Background technology:

[0002] 1,3-cyclohexanedione is an important chemical intermediate. It can be used to synthesize the specific drug carvedilol and the antiemetic drug anthracene for protecting cardiovascular and cerebrovascular and treating hypertension. It can also be used to synthesize cosmetics, polymer additives, excellent herbicides mesotrione and sulcotrione, etc. There are two main methods for synthesizing 1,3-cyclohexanedione. At present, the reduction method is usually adopted, which uses resorcinol as the starting material and synthesizes 1,3-cyclohexanedione through alkalization, hydrogenation reduction or hydrogen transfer reduction, acidification and rearrangement. Therefore, the process of preparing 1,3-cyclohexanedione is carried out in a continuous hydrogenation device. The continuous hydrogenation device for preparing 1,3-cyclohexanedione is also called a hydrogenation reactor. In the preparation of 1,3-cyclohexanedione, achieving full dissolution of hydrogen into the reaction liquid is the key to increasing the yield of 1,3-cyclohexanedione. Therefore, it is necessary to design the hydrogenation and dissolution in the reactor to improve the efficiency of hydrogen dissolution, thereby increasing the yield. Summary of the invention:

[0003] The purpose of the present invention is to address the deficiencies of the prior art and to provide a continuous hydrogenation device for 1,3-cyclohexanedione, which optimizes the design of the stirring and hydrogenation structures in the hydrogenation reactor, can improve the efficiency of hydrogen dissolving into the reaction liquid, thereby achieving sufficient hydrogen reaction and increasing the output of 1,3-cyclohexanedione.

[0004] A continuous hydrogenation device for 1,3-cyclohexanedione comprises a kettle body of a reaction kettle, a feed pipe is fixedly connected to the top of the kettle body, a nitrogen addition pipe and an exhaust pipe are respectively plugged and fixed on the kettle body on one side of the feed pipe, and the ends of the nitrogen addition pipe and the exhaust pipe are inserted in the kettle body and located at the upper part of the kettle body; a vertical stirring shaft is arranged in the kettle body, the stirring shaft comprises a vertical hollow rotating shaft, a gas outlet impeller is arranged in the middle of the hollow rotating shaft, and a dispersion impeller is arranged at the bottom;

[0005] The dispersing impeller comprises a conical wheel disc, the wheel disc sleeve is fixed on the hollow rotating shaft, a plurality of ribs distributed in an annular shape are formed on the inner wall of the wheel disc, a plurality of stirring blade petioles are fixed on the outer wall of the wheel disc, and a stirring blade is fixed on the outer end of the stirring blade petiole;

[0006] The air outlet impeller comprises an air guide wheel which is fixed on a hollow rotating shaft by a sleeve and communicated with the hollow rotating shaft, an arc-shaped air outlet pipe is fixed on the outer wall of the air guide wheel, the air outlet pipe is communicated with the inner cavity of the air guide wheel and is evenly distributed in a ring shape around the central axis of the air guide wheel; a sealing block is inserted and fixed in the hollow rotating shaft on the upper side of the air outlet impeller;

[0007] A hydrogenation pipe is inserted into the kettle body on one side of the stirring shaft, and the hydrogenation pipe includes an air supply pipe and an air outlet pipe assembly, and the air outlet pipe assembly is located directly below the hollow rotating shaft; the air outlet pipe assembly includes a vertical guide pipe, and the upper end of the guide pipe is formed with a conical guide disk opposite to the wheel disk, and a vertical valve pipe is provided below the guide pipe, and the lower end of the valve pipe is fixedly connected to the kettle body, and the upper end of the valve pipe is formed with a cylindrical connector, and the connector is plugged and fixed on the guide pipe; a vertical valve stem is inserted in the guide pipe, and the upper end of the valve stem extends out of the guide pipe and is formed with a conical valve head, and the valve head is pressed against the inner wall of the guide disk; the lower end of the valve stem passes through the connector and is inserted into the valve pipe and fixed with a retaining ring, and a spring is inserted on the valve stem on the upper side of the retaining ring, and the lower end of the spring is pressed against the retaining ring, and the upper end is pressed against the valve pipe;

[0008] The air supply pipe comprises a vertical pipe, the upper end of which is plugged and fixed on the kettle body, the lower end of which is located under the dispersion impeller and is bent to form a horizontal pipe, and the end of which is fixed on the guide pipe and communicated with the guide pipe.

[0009] Preferably, a catalyst inlet pipe is inserted and fixed on the kettle body, and the lower end of the catalyst inlet pipe is located inside the kettle body and close to the air outlet impeller on the stirring shaft.

[0010] Preferably, the central axis of the guide pipe on the air outlet pipe assembly coincides with the central axis of the hollow rotating shaft.

[0011] Preferably, a cylindrical base is threadedly fixed to the lower end of the valve tube, and the base is welded and fixed to the inner bottom surface of the kettle body.

[0012] Preferably, a heat exchange component is arranged in the kettle body on the upper side of the dispersion impeller, and the heat exchange component includes a plurality of sheet-shaped heat exchange plates, and a rectangular heat exchange cavity is formed in the heat exchange plates. The heat exchange plates are evenly distributed in the kettle body around the outlet impeller in a ring shape around the central axis of the hollow rotating shaft;

[0013] The heat exchange plate on one side of the hollow shaft is fixedly connected with a heat exchange inlet pipe connected to the heat exchange cavity in the heat exchange plate, and the heat exchange plate on the other side of the hollow shaft is fixedly connected with a heat exchange outlet pipe connected to the heat exchange cavity in the heat exchange plate. The heat exchange outlet pipe and the heat exchange inlet pipe are respectively plugged and fixed on the kettle walls on two opposite sides of the kettle body; the adjacent heat exchange plates between the heat exchange inlet pipe and the heat exchange outlet pipe are connected through the connecting pipe, and the connecting pipes on both sides of the heat exchange plate are respectively staggered in the upper and lower positions.

[0014] Preferably, the number of heat exchange plates on the heat exchange assembly in the kettle body is an even number, and a plurality of support rods are fixedly connected to the side of the heat exchange plates close to the kettle wall of the kettle body, and the ends of the support rods are fixedly connected to the kettle wall of the kettle body.

[0015] Preferably, a plurality of bulges connected to the heat exchange cavity are respectively formed on both side walls of the heat exchange plate, and the bulge array is distributed on the heat exchange plate.

[0016] The beneficial effects of the present invention are:

[0017] The device optimizes the design of the stirring and hydrogenation structure in the hydrogenation reactor, which can improve the efficiency of hydrogen dissolving into the reaction liquid, thereby achieving sufficient hydrogen reaction and increasing the yield of 1,3-cyclohexanedione. Description of the drawings:

[0018] Figure 1 It is a schematic diagram of the structure of a partial cross-section of the present invention;

[0019] Figure 2 A schematic diagram of the three-dimensional structure of the stirring shaft part of the present invention;

[0020] Figure 3 It is a schematic cross-sectional structure diagram of the stirring shaft part of the present invention;

[0021] Figure 4 It is a cross-sectional schematic diagram of a heat exchange component provided in the present invention.

[0022] In the figure: 1. kettle body; 2. feed pipe; 3. outlet impeller; 31. hollow shaft; 32. dispersion impeller; 33. outlet impeller; 4. catalyst inlet pipe; 5. nitrogen addition pipe; 6. exhaust pipe; 7. hydrogenation pipe; 71. air supply pipe; 72. outlet pipe assembly; 81. heat exchange plate; 4. heat exchange inlet pipe; 83. heat exchange outlet pipe. Specific implementation method:

[0023] Example: See Figures 1 to 3 As shown, a continuous hydrogenation device for 1,3-cyclohexanedione comprises a kettle body 1 of a reaction kettle, a feed pipe 2 is fixedly connected to the top of the kettle body 1, a nitrogen addition pipe 5 and an exhaust pipe 6 are respectively inserted and fixed on the kettle body 1 on one side of the feed pipe 2, and the ends of the nitrogen addition pipe 5 and the exhaust pipe 6 are inserted in the kettle body 1 and located at the upper part of the kettle body 1; a vertical stirring shaft 3 is arranged in the kettle body 1, and the stirring shaft 3 comprises a vertical hollow rotating shaft 31, and a gas outlet impeller 33 is arranged in the middle of the hollow rotating shaft 31, and a dispersion impeller 32 is arranged at the bottom;

[0024] The dispersing impeller 32 includes a conical wheel disc 321, which is fixed on the hollow rotating shaft 31 by inserting and sleeve. The inner wall of the wheel disc 321 is formed with a plurality of ribs 322 distributed in an annular shape. The outer wall of the wheel disc 321 is fixed with a plurality of stirring blade handles 323, and the outer end of the stirring blade handle 323 is fixed with a stirring blade 324.

[0025] The outlet impeller 33 includes an air guide wheel 331 which is fixed on the hollow rotating shaft 31 by a sleeve and communicated with the hollow rotating shaft 31. An arc-shaped air outlet pipe 332 is fixedly connected to the outer wall of the air guide wheel 331. The air outlet pipe 332 is communicated with the inner cavity of the air guide wheel 331 and is evenly distributed in a ring shape around the central axis of the air guide wheel 331. A sealing block 34 is inserted and fixed in the hollow rotating shaft 31 on the upper side of the outlet impeller 33.

[0026] A hydrogenation pipe 7 is inserted into the kettle body 1 on one side of the stirring shaft 3, and the hydrogenation pipe 7 includes an air supply pipe 71 and an air outlet pipe assembly 72. The air outlet pipe assembly 72 is located directly below the hollow rotating shaft 31; the air outlet pipe assembly 72 includes a vertical guide pipe 721, and the upper end of the guide pipe 721 is formed with a conical guide disc 7211 opposite to the wheel disc 321, and a vertical valve pipe 722 is provided below the guide pipe 721, and the lower end of the valve pipe 722 is fixedly connected to the kettle body 1, and the upper end of the valve pipe 722 is formed with a cylindrical connector 7221, and the connector 7 221 is plugged and fixed on the guide tube 721; a vertical valve stem 724 is inserted in the guide tube 721, and the upper end of the valve stem 724 extends out of the guide tube 721 and is formed with a conical valve head 7241, and the valve head 7241 is pressed against the inner wall of the guide plate 7211; the lower end of the valve stem 724 passes through the connector 7221 and is inserted into the valve tube 722 and is fixed with a retaining ring 725, and a spring 726 is inserted on the valve stem 724 on the upper side of the retaining ring 725, and the lower end of the spring 726 is pressed against the retaining ring 725, and the upper end is pressed against the valve tube 722;

[0027] The air supply pipe 71 includes a vertical pipe 711 , the upper end of which is plugged and fixed to the kettle body 1 , and the lower end of which is located at the lower side of the dispersion impeller 32 and is bent to form a horizontal pipe 712 . The end of the horizontal pipe 712 is fixed to the guide pipe 721 and communicates with the guide pipe 721 .

[0028] A catalyst inlet pipe 4 is inserted and fixed on the kettle body 1, and the lower end of the catalyst inlet pipe 4 is located in the kettle body 1 and close to the air outlet impeller 33 on the stirring shaft 3. When preparing 1,3-cyclohexanedione, it is necessary to add catalyst to the reaction liquid in the kettle body 1 through the catalyst inlet pipe 4 before the hydrogenation reaction.

[0029] The central axis of the guide tube 721 on the outlet pipe assembly 72 coincides with the central axis of the hollow rotating shaft 31. If they are aligned, half of the hydrogen output by the guide tube 721 can enter the hollow rotating shaft 31. If they are not aligned, most of the hydrogen output by the guide tube 721 is dispersed by the dispersion impeller 32 into the reaction liquid around the dispersion impeller 32, and only a small amount of hydrogen flows through the hollow rotating shaft 31 to the outlet impeller 33.

[0030] The lower end of the valve tube 722 is screwed and fixed with a cylindrical base 723, and the base 723 is welded and fixed to the inner bottom surface of the kettle body 1. The base 723 facilitates the disassembly and assembly of the air outlet pipe assembly 72.

[0031] See Figure 4 As shown, a heat exchange component is arranged in the kettle body 1 on the upper side of the dispersion impeller 32, and the heat exchange component includes a plurality of sheet-shaped heat exchange plates 81, and a rectangular heat exchange cavity is formed in the heat exchange plate 81. The heat exchange plate 81 is evenly distributed in the kettle body 1 around the outlet impeller 33 in a ring shape around the central axis of the hollow rotating shaft 31; the heat exchange component adopts a plate heat exchanger arranged in the kettle;

[0032] The heat exchange plate 81 on one side of the hollow shaft 31 is fixedly connected with a heat exchange inlet pipe 82 connected to the heat exchange cavity in the heat exchange plate 81, and the heat exchange plate 81 on the other side of the hollow shaft 31 is fixedly connected with a heat exchange outlet pipe 83 connected to the heat exchange cavity in the heat exchange plate 81. The heat exchange outlet pipe 83 and the heat exchange inlet pipe 82 are respectively plugged and fixed on the kettle walls on two opposite sides of the kettle body 1; the adjacent heat exchange plates 81 between the heat exchange inlet pipe 82 and the heat exchange outlet pipe 83 are connected through the connecting pipe, and the connecting pipes on both sides of the heat exchange plate 81 are respectively staggered in the upper and lower positions; the heat exchange liquid enters the heat exchange plate 81 provided with the heat exchange inlet pipe 82, and then the heat exchange liquid flows to the heat exchange plates 81 on both sides of this heat exchange plate 81 through the connecting pipe, and finally converges into the heat exchange plate 81 provided with the heat exchange outlet pipe 83, and is output from the heat exchange outlet pipe 83.

[0033] The number of heat exchange plates 81 on the heat exchange assembly in the kettle body 1 is an even number. A plurality of support rods are fixedly connected to the side of the heat exchange plate 81 close to the kettle wall of the kettle body 1. The ends of the support rods are fixedly connected to the kettle wall of the kettle body 1. The heat exchange plate 81 in the kettle body 1 is supported only by the heat exchange outlet pipe 83, the heat exchange inlet pipe 82 and the connecting pipe. The strength of the entire heat exchange assembly is weak, and the strength is increased by the support rods.

[0034] A number of bulges 811 connected to the heat exchange cavity are respectively formed on the two side walls of the heat exchange plate 81. The bulges 811 can be protruding or recessed. The protruding bulges 811 are taken as an example in the drawings of the present application. The bulges 811 are distributed in an array on the heat exchange plate 81. The bulges 811 can increase the surface area of ​​the heat exchange plate 81 in contact with the reaction liquid, and the surface of the bulges 811 can further retain hydrogen molecules to achieve a sufficient hydrogenation reaction.

[0035] Working principle: This scheme is a continuous hydrogenation device for preparing 1,3-cyclohexanedione, which is actually a hydrogenation reactor. A dispersion impeller 32 is arranged at the bottom end of the stirring shaft 3 in the reactor, and the outlet for adding hydrogen is arranged below the stirring shaft 3. After the hydrogen is output, part of it is dispersed by the dispersion impeller 32 and dissolved in the reaction liquid around the dispersion impeller 32 (the reaction liquid at the bottom of the reactor), and part of it is sucked into the hollow shaft 31 of the stirring shaft 3, and then thrown out by the dispersion impeller 32 and dissolved in the reaction liquid around the dispersion impeller 32 (the reaction liquid in the middle of the reactor), which reduces the hydrogen moving through the reaction liquid to the reactor on the upper layer of the reaction liquid, and can effectively improve the dissolution of hydrogen;

[0036] At the same time, the outlet pipe assembly 72 on the hydrogenation pipe 7 is sealed with a spring to prevent the reaction liquid from flowing into the hydrogenation pipe 7. During hydrogenation, the pressure of the hydrogen will overcome the force of the spring and push open the valve head 7241 to enter the reaction liquid.

[0037] The embodiments are used to illustrate the present invention, but not to limit the present invention. Any person skilled in the art may modify the embodiments without violating the spirit and scope of the present invention, and therefore, the scope of protection of the present invention shall be as set forth in the claims of the present invention.

Claims

1. A continuous hydrogenation device for 1,3-cyclohexanedione, comprising a reactor body (1), a feed pipe (2) is fixedly connected to the top of the reactor body (1), a nitrogen addition pipe (5) and an exhaust pipe (6) are respectively inserted and fixed on the reactor body (1) on one side of the feed pipe (2), and the ends of the nitrogen addition pipe (5) and the exhaust pipe (6) are inserted in the reactor body (1) and located at the upper part of the reactor body (1); a vertical stirring shaft (3) is arranged in the reactor body (1), characterized in that: The stirring shaft (3) comprises a vertical hollow rotating shaft (31), wherein an air outlet impeller (33) is arranged in the middle of the hollow rotating shaft (31) and a dispersion impeller (32) is arranged at the bottom; The dispersing impeller (32) comprises a conical wheel disc (321), the wheel disc (321) is fixed on the hollow rotating shaft (31) by inserting and sleeve, a plurality of ribs (322) distributed in an annular shape are formed on the inner wall of the wheel disc (321), a plurality of stirring blade handles (323) are fixedly connected to the outer wall of the wheel disc (331), and a stirring blade (324) is fixedly connected to the outer end of the stirring blade handle (323); The air outlet impeller (33) comprises an air guide wheel (331) which is fixed on the hollow rotating shaft (31) by means of a sleeve and is connected to the hollow rotating shaft (31); an arc-shaped air outlet pipe (332) is fixedly connected to the outer wall of the air guide wheel (331); the air outlet pipe (332) is connected to the inner cavity of the air guide wheel (331) and is evenly distributed in a ring shape around the central axis of the air guide wheel (331); a sealing block (34) is inserted and fixed in the hollow rotating shaft (31) on the upper side of the air outlet impeller (33); A hydrogenation pipe (7) is inserted into the kettle body (1) on one side of the stirring shaft (3), and the hydrogenation pipe (7) includes an air supply pipe (71) and an air outlet pipe assembly (72), and the air outlet pipe assembly (72) is located directly below the hollow rotating shaft (31); the air outlet pipe assembly (72) includes a vertical guide pipe (721), and the upper end of the guide pipe (721) is formed with a conical guide disc (7211) opposite to the wheel disc (321), and a vertical valve pipe (722) is provided below the guide pipe (721), and the lower end of the valve pipe (722) is fixedly connected to the kettle body (1), and the upper end of the valve pipe (722) is formed with a cylindrical connector (7221), and the connector ( 7221) is inserted and fixed on the guide tube (721); a vertical valve stem (724) is inserted in the guide tube (721), the upper end of the valve stem (724) protrudes from the guide tube (721) and is formed with a conical valve head (7241), and the valve head (7241) is pressed against the inner wall of the guide plate (7211); the lower end of the valve stem (724) passes through the connector (7221) and is inserted into the valve tube (722) and is fixed with a retaining ring (725), a spring (726) is inserted on the valve stem (724) on the upper side of the retaining ring (725), the lower end of the spring (726) is pressed against the retaining ring (725), and the upper end is pressed against the valve tube (722); The air supply pipe (71) comprises a vertical pipe (711), the upper end of which is plugged and fixed to the kettle body (1), and the lower end of which is located at the lower side of the dispersion impeller (32) and is bent to form a horizontal pipe (712), and the end of the horizontal pipe (712) is fixed to the guide pipe (721) and communicates with the guide pipe (721).

2. A continuous hydrogenation device for 1,3-cyclohexanedione according to claim 1, characterized in that: A catalyst inlet pipe (4) is inserted and fixed on the kettle body (1), and the lower end of the catalyst inlet pipe (4) is located inside the kettle body (1) and close to the air outlet impeller (33) on the stirring shaft (3).

3. A continuous hydrogenation device for 1,3-cyclohexanedione according to claim 1, characterized in that: The central axis of the flow guide pipe (721) on the air outlet pipe assembly (72) coincides with the central axis of the hollow rotating shaft (31).

4. A continuous hydrogenation device for 1,3-cyclohexanedione according to claim 3, characterized in that: A cylindrical base (723) is screwed and fixed to the lower end of the valve tube (722), and the base (723) is welded and fixed to the inner bottom surface of the kettle body (1).

5. A continuous hydrogenation device for 1,3-cyclohexanedione according to claim 1, characterized in that: A heat exchange component is arranged in the kettle body (1) on the upper side of the dispersion impeller (32), and the heat exchange component includes a plurality of sheet-shaped heat exchange plates (81), and a rectangular heat exchange cavity is formed in the heat exchange plates (81). The heat exchange plates (81) are evenly distributed in the kettle body (1) around the outlet impeller (33) in a ring shape around the central axis of the hollow rotating shaft (31); A heat exchange inlet pipe (82) connected to the heat exchange cavity in the heat exchange plate (81) is fixedly connected to the heat exchange plate (81) on one side of the hollow rotating shaft (31); a heat exchange outlet pipe (83) connected to the heat exchange cavity in the heat exchange plate (81) is fixedly connected to the heat exchange plate (81) on the other side of the hollow rotating shaft (31); the heat exchange outlet pipe (83) and the heat exchange inlet pipe (82) are respectively plugged and fixed on the kettle walls on two opposite sides of the kettle body (1); the adjacent heat exchange plates (81) between the heat exchange inlet pipe (82) and the heat exchange outlet pipe (83) are connected by a pipe; the pipes on the two sides of the heat exchange plate (81) are respectively staggered in an upward and downward manner.

6. A continuous hydrogenation device for 1,3-cyclohexanedione according to claim 5, characterized in that: The number of heat exchange plates (81) on the heat exchange assembly in the kettle body (1) is an even number, and a plurality of support rods are fixedly connected to the side of the heat exchange plates (81) close to the kettle wall of the kettle body (1), and the ends of the support rods are fixedly connected to the kettle wall of the kettle body (1).

7. A continuous hydrogenation device for 1,3-cyclohexanedione according to claim 5, characterized in that: A plurality of bulges (811) connected to the heat exchange cavity are respectively formed on the two side walls of the heat exchange plate (81), and the bulges (811) are distributed in an array on the heat exchange plate (81).

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