CN211158688U - A preprocessing device for taxol chromatography - Google Patents
A preprocessing device for taxol chromatography Download PDFInfo
- Publication number
- CN211158688U CN211158688U CN201921758570.1U CN201921758570U CN211158688U CN 211158688 U CN211158688 U CN 211158688U CN 201921758570 U CN201921758570 U CN 201921758570U CN 211158688 U CN211158688 U CN 211158688U
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- Prior art keywords
- tank body
- dissolving tank
- pumping
- dissolving
- pipeline
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- 229930012538 Paclitaxel Natural products 0.000 title claims abstract description 25
- 229960001592 paclitaxel Drugs 0.000 title claims abstract description 25
- RCINICONZNJXQF-MZXODVADSA-N taxol Chemical compound O([C@@H]1[C@@]2(C[C@@H](C(C)=C(C2(C)C)[C@H](C([C@]2(C)[C@@H](O)C[C@H]3OC[C@]3([C@H]21)OC(C)=O)=O)OC(=O)C)OC(=O)[C@H](O)[C@@H](NC(=O)C=1C=CC=CC=1)C=1C=CC=CC=1)O)C(=O)C1=CC=CC=C1 RCINICONZNJXQF-MZXODVADSA-N 0.000 title claims abstract description 25
- 238000004587 chromatography analysis Methods 0.000 title claims abstract description 15
- 238000007781 pre-processing Methods 0.000 title abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000007599 discharging Methods 0.000 claims abstract description 12
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 7
- 238000005485 electric heating Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 20
- 238000005086 pumping Methods 0.000 claims description 15
- 239000002893 slag Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 abstract description 60
- 238000001953 recrystallisation Methods 0.000 abstract description 11
- YWLXLRUDGLRYDR-UHFFFAOYSA-N 10-deacetylbaccatin Chemical compound CC(=O)OC12COC1CC(O)C(C(C(O)C1=C(C)C(O)CC3(O)C1(C)C)=O)(C)C2C3OC(=O)C1=CC=CC=C1 YWLXLRUDGLRYDR-UHFFFAOYSA-N 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000006071 cream Substances 0.000 abstract description 8
- 239000012452 mother liquor Substances 0.000 abstract description 7
- 241001149649 Taxus wallichiana var. chinensis Species 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 15
- 238000000034 method Methods 0.000 description 15
- 239000000047 product Substances 0.000 description 7
- 238000005406 washing Methods 0.000 description 5
- 238000004440 column chromatography Methods 0.000 description 4
- 239000011265 semifinished product Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 238000002386 leaching Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- WGLUMOCWFMKWIL-UHFFFAOYSA-N dichloromethane;methanol Chemical compound OC.ClCCl WGLUMOCWFMKWIL-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000003810 ethyl acetate extraction Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The utility model relates to a chinese yew deep-processing technology field, concretely relates to preprocessing device for taxol chromatography. The pretreatment device comprises a dissolving tank, a material pump, a vacuum filtration tank and a concentration tank which are sequentially connected through a pipeline, wherein the dissolving tank comprises a dissolving tank body, the top of the dissolving tank body is provided with a material pouring port, the bottom of the dissolving tank body is provided with a material discharging port, one side of a steam heating cavity is provided with a steam inlet, and the other side of the steam heating cavity is provided with a steam backflow port; the vacuum filtration tank comprises a filtration tank body, wherein one side of the filtration tank body is provided with a feeding pipe, the other side of the filtration tank body is provided with a first discharging pipe, the outer wall of the filtration tank body is provided with a vacuum pump, and a filter screen is arranged in the filtration tank body; the concentrating tank comprises a concentrating tank body, a vacuum pump and a feeding pipe are arranged at the top of the concentrating tank body, an electric heating disc is arranged on the inner wall of the concentrating tank body, and a collector is arranged in the concentrating tank body. The utility model provides an in the current taxol finished product production process, the unable problem of extracting 10-DAB and taxol through recrystallization of products such as acetonitrile mother liquor cream, and low in production cost.
Description
Technical Field
The utility model relates to a chinese yew deep-processing technology field, concretely relates to preprocessing device for taxol chromatography.
Background
After the taxus chinensis branches and leaves are leached and extracted, branch and leaf leaching liquor produced in the leaching process is concentrated through a concentrating pot, and methanol is recovered to finally obtain an extract product. Usually, ethyl acetate extraction paste is added, acetonitrile is adopted to carry out recrystallization process treatment on the semi-finished product, and after 2-3 times of recrystallization, a part of semi-finished product with the 10-DAB content of more than 20% and a part of 10-DAB acetonitrile mother liquor paste can be obtained. Usually, the acetonitrile mother liquor paste contains 10-DAB 0.6-1.2% and taxol 0.3-0.4%. If the acetonitrile paste is put into a recrystallization process, 10-DAB and paclitaxel cannot be effectively extracted at present, and the method for solving the problem generally puts the acetonitrile paste into a column chromatography process again for separation to possibly extract the acetonitrile paste, but the putting of the acetonitrile paste into the column chromatography process again needs higher cost and wastes time and labor. In addition, during the production process of the finished product, acetonitrile can not be used for recrystallization to extract 10-DAB and taxol from the products of the process, such as alcohol extract, viscous mother liquor and the like.
SUMMERY OF THE UTILITY MODEL
The utility model discloses to prior art's not enough, provide a simple structure is reasonable is used for preprocessing device of taxol chromatography, solved current taxol finished product production in-process, the unable problem of extracting 10-DAB and taxol through recrystallization of products such as acetonitrile mother liquor cream, and low in production cost.
The technical scheme of the utility model is realized like this: a pretreatment device for paclitaxel chromatography comprises a dissolving tank, a material pump, a vacuum filtration tank and a concentration tank which are sequentially connected through a pipeline, wherein the dissolving tank comprises a dissolving tank body, the top of the dissolving tank body is provided with a material pouring port, the bottom of the dissolving tank body is provided with a material outlet connected with the pipeline, the surface of the dissolving tank body is provided with a steam heating cavity, one side of the steam heating cavity is provided with a steam inlet, and the other side of the steam heating cavity is provided with a steam backflow port; the vacuum filtration tank comprises a filtration tank body, wherein one side of the filtration tank body is provided with a feeding pipe connected with a pipeline, the other side of the filtration tank body is provided with a first discharging pipe connected with the pipeline, the outer wall of the filtration tank body is provided with a first vacuum pump for vacuumizing, and the middle inside the filtration tank body is provided with a filter screen; the concentrated jar is including the concentrated jar body, its top of the concentrated jar body is equipped with the second vacuum pump and with pipe connection's pan feeding pipe, and its bottom is equipped with the second discharging pipe, and its inner wall is equipped with electric heating plate, the internal portion of concentrated jar is equipped with the collection ware that is used for gaseous state solvent to collect.
The dissolving tank is internally provided with an electric stirring paddle for stirring the mixture, and the electric stirring paddle comprises a driving motor, a stirring shaft in power connection with the driving motor and a stirring blade welded on the stirring shaft.
The filter screen is an inverted eccentric cone, the bottom of the filter screen is provided with a slag discharge port, and the lower part of the slag discharge port is detachably connected with a slag storage box.
The middle part of the concentrating tank body is provided with an observation window, and the steam heating cavity is internally provided with a plurality of heat exchange fins.
The utility model provides an existing defect among the background art, have following beneficial effect:
the utility model provides a preprocessing device for paclitaxel chromatography simple structure is reasonable, has solved current paclitaxel finished product production in-process, and the unable problem of extracting 10-DAB and paclitaxel through recrystallization of products such as acetonitrile mother liquor cream, and low in production cost. The utility model discloses an in to acetonitrile cream to dissolving tank, add dichloromethane to the heating is to the operation of washing of dissolving of acetonitrile cream. After the acetonitrile cream in the tank is agglomerated, the dichloromethane solution is discharged. And (3) carrying out suction filtration on the dissolved washing liquid cooled to the normal temperature by using a vacuum suction filtration tank, putting the filtrate into a common concentration pot for concentration and recovery, and carrying out recrystallization treatment on the obtained crude paste by using acetonitrile. Adopt the utility model discloses afterwards, the solvent consumption descends by a wide margin, and the time also reduces by a wide margin, and the technology operation step also very reduces, adopts the device after, and the cream sediment volume is 40% ~ 60% of input usually, can make 10-DAB and taxol content improve by a wide margin, can reach semi-manufactured goods output requirement through the recrystallization process again. The utility model discloses can regard as chromatography preliminary treatment means, by 0.3% ~ 0.4% with the taxol content in the mother liquor, improve to 0.8% ~ 1.2%, sample loading volume when reducing taxol crude product chromatography production by a wide margin reaches reduction in production cost's purpose.
Drawings
Fig. 1 is a schematic structural view of the present invention;
in the figure: 1-a dissolving tank, 2-a vacuum filtration tank, 3-a concentration tank, 4-a pipeline, 5-a material pump, 11-a dissolving tank body, 12-a pouring port, 13-a discharge port, 14-an electric stirring paddle, 15-a steam heating chamber, 16-a steam inlet, 17-a steam return port, 21-a filtration tank body, 22-a feeding pipe, 23-a first discharging pipe, 24-a first vacuum pump, 25-a filter screen, 26-a slag storage box, 31-a concentration tank body, 32-a feeding pipe, 33-an electric heating plate, 34-a second vacuum pump, 35-a second discharging pipe and 36-a collector.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
An embodiment of a pretreatment device for paclitaxel chromatography shown in fig. 1 comprises a dissolving tank 1, a material pump 5, a vacuum filtration tank 2 and a concentration tank 3 which are sequentially connected through a pipeline 4, wherein the dissolving tank 1 comprises a dissolving tank body 11, the top of the dissolving tank body 11 is provided with a material pouring port 12, the bottom of the dissolving tank body 11 is provided with a material discharging port 13 connected with the pipeline 4, the surface of the dissolving tank body 11 is provided with a steam heating cavity 15, one side of the steam heating cavity 15 is provided with a steam inlet 16, and the other side is provided with a steam return port 17; the vacuum pumping and filtering tank 2 comprises a pumping and filtering tank body 21, one side of the pumping and filtering tank body 21 is provided with a feeding pipe 22 connected with the pipeline 4, the other side of the pumping and filtering tank body 21 is provided with a first discharging pipe 23 connected with the pipeline 4, the outer wall of the pumping and filtering tank body 21 is provided with a first vacuum pump 24 for pumping vacuum, and the middle of the interior of the pumping and filtering tank body is provided with a filter screen 25; the concentration tank 3 comprises a concentration tank body 31, a second vacuum pump 34 and a feeding pipe 32 connected with the pipeline 4 are arranged at the top of the concentration tank body 31, a second discharging pipe 35 is arranged at the bottom of the concentration tank body 31, an electric heating plate 33 is arranged on the inner wall of the concentration tank body, and a collector 36 for collecting gaseous solvents is arranged inside the concentration tank body 31. An electric stirring paddle 14 for stirring the mixture is arranged in the dissolving tank body 11, and the electric stirring paddle 14 comprises a driving motor, a stirring shaft in power connection with the driving motor and a stirring blade welded on the stirring shaft. The filter screen 25 is in an inverted eccentric cone shape, the bottom of the filter screen is provided with a slag discharge port, and the lower part of the slag discharge port is detachably connected with a slag storage box 26. An observation window is arranged in the middle of the concentrating tank body 31, and a plurality of heat exchange fins are arranged in the steam heating cavity 15.
The utility model discloses a working process is:
1. adding about 70 kg-80 kg of acetonitrile paste into the dissolving tank 1 from the pouring port 12, adding 400L industrial dichloromethane, sealing the pouring port 12, starting the cooling liquid of the reflux device, simultaneously introducing high-temperature water vapor into the steam heating cavity 15 through the steam inlet 16 to heat the dissolving tank 1 to be controlled to be between about 40 ℃ and 50 ℃, and simultaneously starting the electric stirring paddle 14 to perform dissolving and washing operation on the acetonitrile paste.
2. Each time of the dissolution washing is about 40 to 60 minutes, and then the steam inlet 16 is closed and the heating is stopped. And (3) cooling and standing the solution, discharging dichloromethane solution from a discharge port 13 after the acetonitrile paste in the tank is agglomerated, and pumping the dichloromethane solution into a suction filtration tank 21 through a material pump 5. After the dissolved washing liquid cooled to normal temperature is vacuumized by the first vacuum pump 24, the filtrate filtered by the filter screen 25 enters the concentration tank 3 through the feeding pipe 32 for concentration and recovery.
3. The filtrate is concentrated and recovered in a concentration tank 3 at the normal temperature of 40-65 ℃. After the paste is formed, the collector 36 is drained for a short time, the vacuum is pumped to be more than-0.060 MPa, the crude paste is pumped to be dry until the liquid is not drained from the collector 36, and then acetonitrile is added for recrystallization treatment of the semi-finished product, so that the output requirement of the semi-finished product is met.
The traditional method processes 70 kg-80 kg acetonitrile paste and puts into column chromatography process, expect to put into about 4 columns (20 kg/column), about 7000L-8000L dichloromethane-methanol solvent is needed to put into each column chromatography, about 30000L solvent is needed to put into chromatography 4 column, but adopt the utility model discloses afterwards, only need to put into about 3000L solvent, solvent consumption reduces by a wide margin, time reduces by a wide margin too, the process operation step is also reduced greatly, after adopting the device, the cream sediment amount is usually 40% -60% of input amount, can make 10-DAB and taxol content improve by a wide margin, can pass through recrystallization process again, reach the output requirement of semi-manufactured goods.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The pretreatment device for paclitaxel chromatography is characterized by comprising a dissolving tank (1), a material pump (5), a vacuum filtration tank (2) and a concentration tank (3) which are sequentially connected through a pipeline (4), wherein the dissolving tank (1) comprises a dissolving tank body (11), the top of the dissolving tank body (11) is provided with a material pouring port (12), the bottom of the dissolving tank body is provided with a material outlet (13) connected with the pipeline (4), the surface of the dissolving tank body (11) is provided with a steam heating cavity (15), one side of the steam heating cavity (15) is provided with a steam inlet (16), and the other side of the steam heating cavity is provided with a steam backflow port (17); the vacuum pumping and filtering tank (2) comprises a pumping and filtering tank body (21), one side of the pumping and filtering tank body (21) is provided with a feeding pipe (22) connected with the pipeline (4), the other side of the pumping and filtering tank body is provided with a first discharging pipe (23) connected with the pipeline (4), the outer wall of the pumping and filtering tank body (21) is provided with a first vacuum pump (24) for pumping vacuum, and the middle inside of the pumping and filtering tank body is provided with a filter screen (25); concentrated jar (3) is including the concentrated jar body (31), its top of the concentrated jar body (31) is equipped with second vacuum pump (34) and pan feeding pipe (32) be connected with pipeline (4), and its bottom is equipped with second discharging pipe (35), and its inner wall is equipped with electric heating dish (33), the concentrated jar body (31) inside is equipped with collector (36) that are used for gaseous state solvent to collect.
2. The pretreatment device for paclitaxel chromatography according to claim 1, wherein: the dissolving tank is characterized in that an electric stirring paddle (14) for stirring the mixture is arranged in the dissolving tank body (11), and the electric stirring paddle (14) comprises a driving motor, a stirring shaft in power connection with the driving motor and a stirring blade welded on the stirring shaft.
3. The pretreatment device for paclitaxel chromatography according to claim 1 or 2, characterized in that: the filter screen (25) is in an inverted eccentric taper shape, the bottom of the filter screen is provided with a slag discharge port, and the lower part of the slag discharge port is detachably connected with a slag storage box (26).
4. The pretreatment device for paclitaxel chromatography according to claim 3, wherein: the middle part of the concentration tank body (31) is provided with an observation window, and the steam heating cavity (15) is internally provided with a plurality of heat exchange fins.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921758570.1U CN211158688U (en) | 2019-10-19 | 2019-10-19 | A preprocessing device for taxol chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921758570.1U CN211158688U (en) | 2019-10-19 | 2019-10-19 | A preprocessing device for taxol chromatography |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN211158688U true CN211158688U (en) | 2020-08-04 |
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ID=71817270
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201921758570.1U Expired - Fee Related CN211158688U (en) | 2019-10-19 | 2019-10-19 | A preprocessing device for taxol chromatography |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN211158688U (en) |
-
2019
- 2019-10-19 CN CN201921758570.1U patent/CN211158688U/en not_active Expired - Fee Related
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200804 |