CN214916022U - Adenine reaction crystallization system - Google Patents
Adenine reaction crystallization system Download PDFInfo
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- CN214916022U CN214916022U CN202120618938.5U CN202120618938U CN214916022U CN 214916022 U CN214916022 U CN 214916022U CN 202120618938 U CN202120618938 U CN 202120618938U CN 214916022 U CN214916022 U CN 214916022U
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Abstract
The utility model provides an adenine reaction crystallization system, includes reation kettle and crystallization kettle, reation kettle includes the reation kettle body (1), first (mixing) shaft (2), first agitator motor (3) and a pair of unloading pipe (4), and crystallization kettle includes the crystallization kettle body (20), second (mixing) shaft (21), second agitator motor (22) and a set of supplementary (mixing) shaft (23), the utility model discloses the advantage is: the raw materials enter the reaction kettle body from the discharge holes of the pair of blanking pipes respectively, the raw materials are dispersed when liquid in the reaction kettle body flows, the elliptical pipeline can play a role in blocking and dispersing the liquid flowing in the reaction kettle body while blanking, and the mixing efficiency is improved; the liquid in the crystallization kettle is cooled from the outside and the inside simultaneously by the water cooling jacket and the middle water cooling cylinder in the crystallization process, and the liquid mixing speed in the crystallization kettle is effectively improved by the group of spiral stirring blades, so that the crystallization efficiency is improved.
Description
Technical Field
The utility model relates to a thermal reaction technical field, concretely relates to adenine reaction crystallization system.
Background
At present, tenofovir is an aids antiviral drug, and the production process thereof is to dissolve diethyl phosphite, paraformaldehyde and triethylamine in toluene, carry out heating reaction in a reaction kettle, then cool the reaction product, add tosyl chloride and triethylamine again to carry out low-temperature reaction to obtain a raw material of tosyloxymethyl phosphonic acid diethyl ester, dissolve propylene glycol carbonate, adenine, tosyloxymethyl phosphonic acid diethyl ester and sodium hydroxide in dimethylformamide to react to obtain propyl adenine, dissolve propyl adenine in acetonitrile, add bromotrimethylsilane to obtain a crude tenofovir product, crystallize with water, the whole process is mostly completed in the reaction kettle, the mixing efficiency of the existing reaction system during the addition of raw materials and crystallization is not high, and the working efficiency is directly influenced.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide an adenine reaction crystallization system aiming at the defects.
The utility model comprises a reaction kettle and a crystallization kettle, wherein the reaction kettle comprises a reaction kettle body, a first stirring shaft, a first stirring motor and a pair of blanking pipes, a steam jacket is arranged on the reaction kettle body, one end of the bottom of the first stirring shaft is provided with a stirrer, the first stirring motor is arranged at the top of the reaction kettle body, and the stirrer is driven to rotate in the reaction kettle body through the first stirring shaft; the reaction kettle is characterized in that a pair of feed openings are formed in the top of the reaction kettle body, a discharge opening is formed in the bottom of the reaction kettle body, one end of each feed pipe penetrates through each feed opening and extends into the reaction kettle body, each feed pipe located in the reaction kettle body is an oval pipeline, a plurality of groups of discharge holes are formed in the pipe wall of each oval pipeline, one end of the top of each feed pipe is rotatably connected to each feed opening of the reaction kettle body, an angle adjusting plate is arranged on the reaction kettle body between the pair of feed pipes, an adjusting plate mounting shaft is arranged on the reaction kettle body, a locking handle is screwed on the adjusting plate mounting shaft, an adjusting plate mounting shaft avoiding hole is formed in the middle of each angle adjusting plate, each angle adjusting plate is movably mounted on the corresponding adjusting plate mounting shaft and locked through the locking handle, a swing arm is arranged at one end of the top of each feed pipe, and two ends of each angle adjusting plate are movably connected with the corresponding swing arms through connecting rods;
the crystallization kettle comprises a crystallization kettle body, a second stirring shaft, a second stirring motor and a group of auxiliary stirring shafts, wherein a water-cooling jacket is arranged on the crystallization kettle body, a middle water-cooling barrel with the bottom communicated with the water-cooling jacket is arranged in the crystallization kettle body, the middle water-cooling barrel and the crystallization kettle body are arranged in a concentric shaft mode, an annular stirring cavity is formed between the crystallization kettle body and the middle water-cooling barrel, a main stirring blade in a shape like a Chinese character 'ji' is arranged on the second stirring shaft, the bottom of the main stirring blade is contacted with the inner bottom of the crystallization kettle body, the inner side of the main stirring blade is contacted with the outer wall of the middle water-cooling barrel, the second stirring motor is arranged at the top of the crystallization kettle body, and drives the main stirring blade to rotate in the annular stirring cavity through the second stirring shaft; the auxiliary stirring shafts are provided with spiral stirring blades, a group of auxiliary stirring shafts are arranged in an annular stirring cavity in an annular array, and the group of auxiliary stirring shafts are respectively in belt transmission with the second stirring shaft; the top of the crystallization kettle body is provided with a feeding hole, the feeding hole of the crystallization kettle body is communicated with a discharging hole of the reaction kettle body through a pipeline, a valve is arranged on the discharging hole of the reaction kettle body, the bottom of the crystallization kettle body is provided with a discharging pipe, an auger blade is arranged in the discharging pipe, the bottom of the crystallization kettle body is provided with an auger driving motor for driving the auger blade to rotate, and the pipe wall of the discharging pipe is provided with a discharging valve.
The bottom in the reaction kettle body is provided with a stirring shaft mounting seat, and one end of the bottom of the first stirring shaft is movably mounted on the stirring shaft mounting seat.
The first stirring shaft in the reaction kettle body is rotatably connected with a shaft sleeve, a discharging pipe connecting rod is arranged on the shaft sleeve, and one end of the bottom of each discharging pipe is movably connected with the discharging pipe connecting rod.
The stirrer is an anchor frame type stirrer.
The minor axis of the inner diameter of the oval tube has a length no greater than half the length of the major axis.
Two ends of the second stirring shaft are respectively movably connected with the crystallization kettle body and the middle water cooling barrel.
Two ends of the inverted U-shaped main stirring blade are respectively provided with a scraper contacted with the inner wall of the crystallization kettle body.
The bottom of the crystallization kettle body is arc-shaped, and the bottoms of the two ends of the inverted U-shaped main stirring blade are arc-shaped plates matched with the bottom of the crystallization kettle body.
Belt pulleys are arranged on the auxiliary stirring shaft and the second stirring shaft at one end outside the crystallization kettle body, and a group of auxiliary stirring shafts are in belt transmission with the second stirring shaft respectively.
The utility model has the advantages that: the raw materials enter the reaction kettle body from the discharge holes of the pair of blanking pipes respectively, the raw materials are dispersed when liquid in the reaction kettle body flows, the elliptical pipeline can play a role in blocking and dispersing the liquid flowing in the reaction kettle body while blanking, and the mixing efficiency is improved; the liquid in the crystallization kettle is cooled from the outside and the inside simultaneously by the water cooling jacket and the middle water cooling cylinder in the crystallization process, and the liquid mixing speed in the crystallization kettle is effectively improved by the group of spiral stirring blades, so that the crystallization efficiency is improved.
Description of the drawings
Fig. 1 is a schematic structural diagram of the present invention.
FIG. 2 is a schematic view of the reactor structure.
FIG. 3 is a schematic view of a pair of linking structures at the top of the blanking pipe.
FIG. 4 is a schematic view of a crystallization kettle structure.
FIG. 5 is a schematic view of a set of auxiliary agitator shaft drives.
Detailed Description
As shown in the attached drawing, the utility model comprises a reaction kettle and a crystallization kettle, wherein the reaction kettle comprises a reaction kettle body 1, a first stirring shaft 2, a first stirring motor 3 and a pair of discharging pipes 4, a steam jacket 5 is arranged on the reaction kettle body 1, one end of the bottom of the first stirring shaft 2 is provided with a stirrer 6, the first stirring motor 3 is arranged at the top of the reaction kettle body 1, and the stirrer 6 is driven by the first stirring shaft 2 to rotate in the reaction kettle body 1; the top of the reaction kettle body 1 is provided with a pair of feed openings, the bottom of the reaction kettle body 1 is provided with a discharge opening, one end of the feed pipe 4 passes through the feed openings and extends into the reaction kettle body 1, the feed pipe 4 positioned in the reaction kettle body 1 is an elliptical pipeline, a plurality of groups of discharge holes are arranged on the pipe wall of the oval pipeline, one end of the top of each discharge pipe 4 is rotatably connected on a discharge port of the reaction kettle body 1, an angle adjusting plate 8 is arranged on the reaction kettle body 1 between the pair of discharge pipes 4, an adjusting plate mounting shaft is arranged on the reaction kettle body 1, a locking handle 9 is screwed on the adjusting plate mounting shaft, an adjusting plate mounting shaft avoiding hole is arranged in the middle of the angle adjusting plate 8, the angle adjusting plate 8 is movably mounted on the adjusting plate mounting shaft, the blanking tube is locked by a locking handle 9, one end of the top of the blanking tube 4 is provided with a swing arm 10, and two ends of an angle adjusting plate 8 are respectively movably connected with the corresponding swing arms 10 through connecting rods;
the crystallization kettle comprises a crystallization kettle body 20, a second stirring shaft 21, a second stirring motor 22 and a group of auxiliary stirring shafts 23, wherein a water cooling jacket 25 is arranged on the crystallization kettle body 20, a middle water cooling barrel 26 with the bottom communicated with the water cooling jacket 25 is arranged in the crystallization kettle body 20, the middle water cooling barrel 26 and the crystallization kettle body 20 are arranged in a concentric shaft mode, an annular stirring cavity is formed between the crystallization kettle body 20 and the middle water cooling barrel 26, a 'n' -shaped main stirring blade 28 is arranged on the second stirring shaft 21, the bottom of the main stirring blade 28 is contacted with the inner bottom of the crystallization kettle body 20, the inner side of the main stirring blade 28 is contacted with the outer wall of the middle water cooling barrel 26, the second stirring motor 22 is arranged at the top of the crystallization kettle body 20, and the main stirring blade 28 is driven to rotate in the annular stirring cavity through the second stirring shaft 21; the auxiliary stirring shafts 23 are provided with spiral stirring blades 29, a group of auxiliary stirring shafts 23 are annularly arrayed in the annular stirring cavity, and the group of auxiliary stirring shafts 23 are respectively in belt transmission with the second stirring shaft 21; the top of the crystallization kettle body 20 is provided with a feeding hole, the feeding hole of the crystallization kettle body 20 is communicated with the discharging hole of the reaction kettle body 1 through a pipeline, the discharging hole of the reaction kettle body 1 is provided with a valve, the bottom of the crystallization kettle body 20 is provided with a discharging pipe, an auger blade 30 is arranged in the discharging pipe, the bottom of the crystallization kettle body 20 is provided with an auger driving motor 31 for driving the auger blade 30 to rotate, and the pipe wall of the discharging pipe is provided with a discharge valve.
The bottom in the reaction kettle body 1 is provided with a stirring shaft mounting seat 11, and one end of the bottom of the first stirring shaft 2 is movably mounted on the stirring shaft mounting seat 11.
The first stirring shaft 2 in the reaction kettle body 1 is rotatably connected with a shaft sleeve 12, a feeding pipe connecting rod 13 is arranged on the shaft sleeve 12, and one end of the bottom of each feeding pipe 4 is movably connected with the feeding pipe connecting rod 13.
The stirrer 6 is an anchor frame stirrer.
The minor axis of the inner diameter of the oval tube has a length no greater than half the length of the major axis.
Two ends of the second stirring shaft 21 are respectively movably connected with the crystallization kettle body 20 and the middle water cooling cylinder 26.
The two ends of the inverted V-shaped main stirring blade 28 are respectively provided with a scraper 33 which is contacted with the inner wall of the crystallization kettle body 20.
The bottom of the crystallization kettle body 20 is arc-shaped, and the bottoms of the two ends of the inverted V-shaped main stirring blade 28 are arc-shaped plates matched with the bottom of the crystallization kettle body 20.
Belt pulleys are arranged on the auxiliary stirring shaft 23 and the second stirring shaft 21 at one end outside the crystallization kettle body 20, and a group of auxiliary stirring shafts 23 are in belt transmission with the second stirring shaft 21 respectively.
The working mode and principle are as follows: all raw materials enter organic solution in the reaction kettle body 1 from the pair of discharging pipes 4 in sequence, the stirrer 6 stirs the organic solution in the reaction kettle body 1, the organic solution brings out all raw materials in the discharging pipes 4 from a discharging hole when flowing, so that the organic solution is uniformly dispersed, meanwhile, the pair of discharging pipes 4 play a role in blocking liquid flowing in the reaction kettle body 1, the speed of the liquid rotating coaxially with the stirrer 6 in the reaction kettle body 1 is reduced, the dispersing speed and the stirring efficiency are improved, the resistance of the pair of discharging pipes 4 to flowing liquid can be adjusted according to needs, the discharging pipes 4 in the reaction kettle body 1 are oval pipes, the orientations of the oval pipes facing the flowing direction of the liquid are different, the resistance is also different, when in adjustment, the rotating angle adjusting plate 8, two ends of the angle adjusting plate 8 drive two swing arms 10 to synchronously through connecting rods respectively, the pair of discharging pipes 4 rotate a certain angle along the axis of the discharging pipes respectively, the blocking area of the discharging pipes for flowing liquid is changed, the resistance of the discharging pipes is the largest when the inner diameter long shaft surface of the oval pipe faces the flowing direction of the liquid, on the contrary, the resistance of the discharging pipes for flowing liquid is the smallest when the inner diameter short shaft surface of the oval pipe faces the flowing direction of the liquid, the liquid passing through the discharging pipes 4 passes through the discharging holes, the mixed liquid is dispersed, and the stirring efficiency is improved.
The crude tenofovir product of high-temperature reaction in the reaction kettle is injected into the crystallization kettle body 20 for cooling and crystallization, the liquid in the crystallization kettle body 20 is cooled from the outside by the water cooling jacket 25, and the liquid in the crystallization kettle body 20 is cooled from the inside by the middle water cooling cylinder 26, so that the cooling efficiency is improved. The main stirring blade 28 can scrape the crystal attached to the crystallizing kettle body 20 and the middle water cooling cylinder 26 when stirring corresponding to the liquid in the annular stirring cavity, the second stirring shaft 21 drives a set of auxiliary stirring shaft 23 to rotate through a belt when rotating, the speed of liquid flowing in the crystallizing kettle body 20 can be improved when the spiral stirring blade 29 rotates, and the cooling crystallization efficiency is improved. After crystallization, the second stirring shaft 21 continues to rotate, the packing auger driving motor 31 is started, and the packing auger blades 30 discharge crystals in the crystallization kettle body 20, so that the crystal blockage of the discharge pipe is avoided.
Claims (9)
1. An adenine reaction crystallization system is characterized by comprising a reaction kettle and a crystallization kettle, wherein the reaction kettle comprises a reaction kettle body (1), a first stirring shaft (2), a first stirring motor (3) and a pair of discharging pipes (4), a steam jacket (5) is arranged on the reaction kettle body (1), a stirrer (6) is arranged at one end of the bottom of the first stirring shaft (2), the first stirring motor (3) is arranged at the top of the reaction kettle body (1), and the stirrer (6) is driven to rotate in the reaction kettle body (1) through the first stirring shaft (2); the top of the reaction kettle body (1) is provided with a pair of feed openings, the bottom of the reaction kettle body (1) is provided with a discharge opening, one end of the feed pipe (4) penetrates through the feed opening and extends into the reaction kettle body (1), the feed pipe (4) positioned in the reaction kettle body (1) is an oval pipeline, the pipe wall of the oval pipeline is provided with a plurality of groups of discharge openings, one end of the top of the feed pipe (4) is rotatably connected on the feed opening of the reaction kettle body (1), the reaction kettle body (1) positioned between the pair of feed pipes (4) is provided with an angle adjusting plate (8), the reaction kettle body (1) is provided with an adjusting plate mounting shaft, the adjusting plate mounting shaft is screwed with a locking handle (9), the middle part of the angle adjusting plate (8) is provided with an adjusting plate avoiding hole, the angle adjusting plate (8) is movably arranged on the adjusting plate mounting shaft and locked by the locking handle (9), one end of the top of the feed pipe (4) is provided with a swing arm (10), two ends of the angle adjusting plate (8) are respectively movably connected with the corresponding swing arms (10) through connecting rods;
the crystallization kettle comprises a crystallization kettle body (20), a second stirring shaft (21), a second stirring motor (22) and a group of auxiliary stirring shafts (23), a water-cooling jacket (25) is arranged on the crystallization kettle body (20), a middle water-cooling barrel (26) with the bottom communicated with the water-cooling jacket (25) is arranged in the crystallization kettle body (20), the middle water-cooling barrel (26) and the crystallization kettle body (20) are arranged in a concentric shaft manner, an annular stirring cavity is formed between the crystallization kettle body (20) and the middle water-cooling barrel (26), a main stirring blade (28) in a shape like a Chinese character 'ji' is arranged on the second stirring shaft (21), the bottom of the main stirring blade (28) is contacted with the inner bottom of the crystallization kettle body (20), the inner side of the main stirring blade (28) is contacted with the outer wall of the middle water-cooling barrel (26), the second stirring motor (22) is arranged at the top of the crystallization kettle body (20), the main stirring blade (28) is driven to rotate in the annular stirring cavity through the second stirring shaft (21); spiral stirring blades (29) are arranged on the auxiliary stirring shafts (23), a group of auxiliary stirring shafts (23) are annularly arrayed in the annular stirring cavity, and the group of auxiliary stirring shafts (23) are respectively in belt transmission with the second stirring shaft (21); the top of the crystallization kettle body (20) is provided with a feeding hole, the feeding hole of the crystallization kettle body (20) is communicated with a discharging hole of the reaction kettle body (1) through a pipeline, a valve is arranged on the discharging hole of the reaction kettle body (1), a discharging pipe is arranged at the bottom of the crystallization kettle body (20), an auger blade (30) is arranged in the discharging pipe, an auger driving motor (31) for driving the auger blade (30) to rotate is arranged at the bottom of the crystallization kettle body (20), and a discharging valve is arranged on the pipe wall of the discharging pipe.
2. The adenine reaction crystallization system as claimed in claim 1, wherein a stirring shaft mounting seat (11) is arranged at the bottom in the reaction kettle body (1), and one end of the bottom of the first stirring shaft (2) is movably mounted on the stirring shaft mounting seat (11).
3. The adenine reaction crystallization system as claimed in claim 1, wherein a shaft sleeve (12) is rotatably connected to the first stirring shaft (2) in the reaction vessel body (1), a feeding pipe connecting rod (13) is arranged on the shaft sleeve (12), and one end of the bottom of the pair of feeding pipes (4) is movably connected with the feeding pipe connecting rod (13) respectively.
4. An adenine reaction crystallization system as claimed in claim 1, characterized in that the stirrer (6) is an anchor frame stirrer.
5. An adenine reaction crystallizing system as in claim 1 wherein the minor axis of the inner diameter of the oval tube is no more than half the length of the major axis.
6. The adenine reaction crystallizing system as claimed in claim 1, wherein both ends of the second stirring shaft (21) are movably connected with the crystallizing still body (20) and the middle water cooling cylinder (26), respectively.
7. An adenine reaction crystallizing system as claimed in claim 1, wherein both ends of the main stirring blade (28) in the shape of "ji" are respectively provided with scrapers (33) contacting with the inner wall of the crystallizing tank body (20).
8. The adenine reaction crystallizing system as claimed in claim 1, wherein the bottom of the crystallizing kettle body (20) is arc-shaped, and the bottoms of both ends of the inverted V-shaped main stirring blade (28) are arc-shaped plates matched with the bottom of the crystallizing kettle body (20).
9. The adenine reaction crystallizing system as claimed in claim 1, wherein the auxiliary stirring shaft (23) and the second stirring shaft (21) at the outer end of the crystallizing still body (20) are both provided with belt pulleys, and a group of auxiliary stirring shafts (23) are respectively in belt transmission with the second stirring shaft (21).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120618938.5U CN214916022U (en) | 2021-03-26 | 2021-03-26 | Adenine reaction crystallization system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120618938.5U CN214916022U (en) | 2021-03-26 | 2021-03-26 | Adenine reaction crystallization system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN214916022U true CN214916022U (en) | 2021-11-30 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202120618938.5U Active CN214916022U (en) | 2021-03-26 | 2021-03-26 | Adenine reaction crystallization system |
Country Status (1)
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|---|---|
| CN (1) | CN214916022U (en) |
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2021
- 2021-03-26 CN CN202120618938.5U patent/CN214916022U/en active Active
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