CN211005191U - Drug intermediate production device combination - Google Patents
Drug intermediate production device combination Download PDFInfo
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- CN211005191U CN211005191U CN201921883065.XU CN201921883065U CN211005191U CN 211005191 U CN211005191 U CN 211005191U CN 201921883065 U CN201921883065 U CN 201921883065U CN 211005191 U CN211005191 U CN 211005191U
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Abstract
The utility model discloses a medicine midbody apparatus for producing combination, including first midbody apparatus for producing combination, second midbody apparatus for producing combination and finished product apparatus for producing combination, first midbody apparatus for producing combination front end is provided with the chloroform metering tank, there is first condensation reation kettle chloroform metering tank rear end through the tube coupling, there is first filter first condensation reation kettle rear end through the tube coupling, there is salifying extraction cauldron first filter rear end through the tube coupling, still be connected with first alkali groove on the salifying extraction cauldron, there is first stills salifying extraction cauldron rear end through the tube coupling, there is first vacuum distillation cauldron first stills rear end through the tube coupling, install first condenser on the pipeline of first vacuum distillation cauldron rear end. The production device combination omits the use of raw materials of thionyl chloride, reduces the pollution influence of the process on the environment and people to a certain degree, and simultaneously, the first intermediate and the second intermediate both adopt a high-temperature reduced pressure distillation method, thereby improving the quality of the intermediate product.
Description
Technical Field
The utility model belongs to the technical field of the production of medicine midbody, concretely relates to medicine midbody apparatus for producing combination.
Background
The modern life rhythm is accelerated, the eating rule of people cannot be guaranteed, the incidence rate of stomach diseases is higher and higher, and acute or chronic stomach diseases almost occur to different degrees in the life of each person. The data show that nearly 30% of people in China have various gastritis, nearly 4 hundred million people are estimated to be in the total number of patients with the national stomach illness at present, and 40% of the patients have serious illness. The amount of gastric drug developed, studied and produced has increased year by year.
Nizatidine is an H2 receptor antagonist, is marketed by Eli L illy, USA in 1987, has better curative effect on gastric and duodenal ulcers than cimetidine, is similar to ranitidine but has little side effect and high oral bioavailability.
Nizatidine basically adopts two synthetic routes in China, and the structure of nizatidine can be divided into two parts of a main ring [ 2-dimethylaminomethyl-4-chloromethyl thiazole salt ] and a side chain [ N- (2-Thiourethyl) -N' -methyl-2-nitro-1, 1-ethylene diamine ]. The synthesis can be carried out by synthesizing the main ring and then gradually lengthening the side chain, or by direct condensation of the main ring and the side chain under alkaline conditions according to the synthesis method of ranitidine. The existing process belongs to a process method for synthesizing a main ring and then partially lengthening a side chain, but the main ring structure is not [ 2-dimethylaminomethyl-4-chloromethyl thiazole salt, but [ 2-dimethylaminomethyl-4-hydroxymethyl thiazole ], the process has certain pollution to the environment, and the quality of an intermediate in the production process is not easy to control.
SUMMERY OF THE UTILITY MODEL
The utility model provides a drug intermediate apparatus for producing combination, the use of this equipment can reduce prior art to the pollution of environment, improves product quality, reduction in production cost.
In order to achieve the above object, the utility model provides a following technical scheme: a drug intermediate production device combination comprises a first intermediate production device combination, a second intermediate production device combination and a finished product production device combination, wherein a chloroform metering tank is arranged at the front end of the first intermediate production device combination, the rear end of the chloroform metering tank is connected with a first condensation reaction kettle through a pipeline, the rear end of the first condensation reaction kettle is connected with a first filter through a pipeline, the rear end of the first filter is connected with a salifying extraction kettle through a pipeline, a first alkali tank is further connected onto the salifying extraction kettle, the rear end of the salifying extraction kettle is connected with a first distillation kettle through a pipeline, the rear end of the first distillation kettle is connected with a first reduced pressure distillation kettle through a pipeline, a first condenser is installed on the pipeline at the rear end of the first reduced pressure distillation kettle, a first intermediate receiving tank is connected onto the pipeline at the rear end of the first condenser, the rear end of the first intermediate receiving tank is connected with a second, the upper part of the second condensation reaction kettle is also connected with a hydrochloric acid head tank; the rear end of the second condensation reaction kettle is connected with a first extraction kettle through a pipeline, the upper part of the first extraction kettle is also provided with a second alkali tank, the rear end of the first extraction kettle is connected with a second distillation kettle through a pipeline, the rear end of the second distillation kettle is connected with a second reduced pressure distillation kettle through a pipeline, a second condenser is arranged on the pipeline at the rear end of the second reduced pressure distillation kettle, a second intermediate receiving tank is arranged on the pipeline at the rear end of the second condenser, the rear end of the second intermediate receiving tank is connected with a third condensation reaction kettle, the rear end of the third condensation reaction kettle is connected with a crude product crystallization kettle through a pipeline, the rear end of the crude product crystallization kettle is provided with a first centrifugal machine, and the rear end of the first centrifugal machine is connected with a first crude; second midbody receiving tank rear end has the crude product to dissolve the cauldron through the tube coupling, the crude product dissolves the cauldron rear end and has the recrystallization cauldron through the tube coupling, second centrifuge is installed to recrystallization cauldron rear end, second crude product acetone mother liquor geosyncline is installed to second centrifuge rear end, recrystallization dissolution kettle installs in the second centrifuge rear end recrystallization dissolution kettle, recrystallization dissolution kettle rear end has the fourth filter through the tube coupling, fourth filter rear end is connected with finished product crystallization kettle, finished product crystallization kettle rear end is connected with third centrifuge, third centrifuge rear end is connected with finished product acetone mother liquor geosyncline.
Preferably, a second filter is arranged at the rear end of the second condensation reaction kettle.
Preferably, a first long visual cup is further mounted on a pipeline between the salifying extraction kettle and the first distillation kettle.
Preferably, the rear end of the second condensation reaction kettle is also connected with a gas storage barrel.
Preferably, a third filter is further arranged on a pipeline between the third condensation reaction kettle and the crude product crystallization kettle.
Preferably, a second visual cup is further arranged on the pipeline between the first extraction kettle and the second distillation kettle.
Preferably, a double-cone dryer is further connected to the rear end of the third centrifuge.
Compared with the prior art, the beneficial effects of the utility model are that:
the process improvement omits the use of raw materials of thionyl chloride, reduces the pollution influence of the process on the environment and people to a certain extent, and simultaneously, the first intermediate and the second intermediate both adopt a high-temperature reduced pressure distillation method, thereby improving the quality of the intermediate product, which is the premise of stable quality of the final product. In particular, the 1, 3-dichloroacetone, the dimethylamino thioacetamide and other skeleton raw materials are all produced from the beginning, and the method has very direct and important significance on the quality control of the main raw materials and the production cost of products.
Other features of the present disclosure and advantages thereof will become apparent from the following detailed description of exemplary embodiments thereof, which proceeds with reference to the accompanying drawings.
Drawings
In order to more clearly illustrate the embodiments of the present disclosure or technical solutions in related arts, the drawings used in the description of the embodiments or related arts will be briefly introduced below, it is obvious that the drawings in the following description are only embodiments of the present disclosure, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic view of the production apparatus of the present invention;
FIG. 2 is a view showing the assembly of the production apparatus of the present invention in FIG. 2;
FIG. 3 is a view showing the assembly of the production apparatus of the present invention;
in the figure: 1. a first intermediate production device combination, a second intermediate production device combination, a 3 finished product production device combination, a 11 chloroform metering tank, a 12 first condensation reaction kettle, a 13 first filter, a 14 salifying extraction kettle, a 15 first alkali tank, a 16 first distillation kettle, a 17 first reduced pressure distillation kettle, a 18 first condenser, a 19 first intermediate receiving tank, a 110 second condensation reaction kettle, a 111 hydrochloric acid head tank, a 112 second filter, a 113 first long sight glass, a 114 gas storage barrel, a 21 first extraction kettle, a 22 second alkali tank, a 23 second distillation kettle, a 24 second reduced pressure distillation kettle, a 25 second condenser, a 26 second intermediate, a 27 third condensation reaction kettle, a 28 crude product crystallization kettle, a 29 first centrifuge, a 210 first crude product acetone mother liquor receiving tank, a 211, a third filter, a 212, A second long visual cup, 31, a crude product dissolving kettle, 32, a recrystallization kettle, 33, a second centrifuge, 34, a second crude product acetone mother liquor ground groove, 35, a recrystallization dissolving kettle, 36, a fourth filter, 37, a finished product crystallization kettle, 38, a third centrifuge, 39, a double-cone dryer, 310 and a finished product acetone mother liquor ground groove.
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. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. 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.
Unless specifically stated otherwise, the relative arrangement of the components and steps, the numerical expressions, and numerical values set forth in these embodiments do not limit the scope of the present invention. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
Spatially relative terms, such as "above … …," "above … …," "above … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial relationship to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is turned over, devices described as "above" or "on" other devices or configurations would then be oriented "below" or "under" the other devices or configurations. Thus, the exemplary term "above … …" can include both an orientation of "above … …" and "below … …". The device may be otherwise variously oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
Referring to fig. 1-3, the present invention provides a technical solution: a pharmaceutical intermediate production device combination comprises a first intermediate production device combination 1, a second intermediate production device combination 2 and a finished product production device combination 3, wherein a chloroform metering tank 11 is arranged at the front end of the first intermediate production device combination 1, the rear end of the chloroform metering tank is connected with a first condensation reaction kettle 12 through a pipeline, the rear end of the first condensation reaction kettle is connected with a first filter 13 through a pipeline, the rear end of the first filter is connected with a salifying extraction kettle 14 through a pipeline, the salifying extraction kettle is also connected with a first alkali tank 15, the rear end of the salifying extraction kettle is connected with a first distillation kettle 16 through a pipeline, the rear end of the first distillation kettle is connected with a first reduced pressure distillation kettle 17 through a pipeline, a first condenser 18 is arranged on the pipeline at the rear end of the first reduced pressure distillation kettle, a first intermediate 19 is connected on the pipeline at the rear end of the first condenser, a second intermediate receiving tank is connected with a second condensation reaction kettle 110, the upper part of the second condensation reaction kettle is also connected with a hydrochloric acid head tank 111; the rear end of the second condensation reaction kettle is connected with a first extraction kettle 21 through a pipeline, the upper part of the first extraction kettle is also provided with a second alkali tank 22, the rear end of the first extraction kettle is connected with a second distillation kettle 23 through a pipeline, the rear end of the second distillation kettle is connected with a second reduced pressure distillation kettle 24 through a pipeline, the pipeline at the rear end of the second reduced pressure distillation kettle is provided with a second condenser 25, the pipeline at the rear end of the second condenser is provided with a second intermediate receiving tank 26, the rear end of the second intermediate receiving tank is connected with a third condensation reaction kettle 27, the rear end of the third condensation reaction kettle is connected with a crude product crystallization kettle 28 through a pipeline, the rear end of the crude product crystallization kettle is provided with a first centrifuge 29, and the rear end of the first centrifuge is connected with a first crude product acetone; second midbody receiving groove 26 rear end has crude product dissolving kettle 31 through the tube coupling, crude product dissolving kettle rear end has recrystallization cauldron 32 through the tube coupling, second centrifuge 33 is installed to recrystallization cauldron rear end, second crude product acetone mother liquor geosyncline 34 is installed to second centrifuge rear end, recrystallization dissolving kettle 35 is installed to second centrifuge rear end, recrystallization dissolving kettle rear end has fourth filter 36 through the tube coupling, fourth filter rear end is connected with finished product crystallization cauldron 37, finished product crystallization cauldron rear end is connected with third centrifuge 38, third centrifuge rear end is connected with finished product acetone mother liquor geosyncline 310. The second condensation reaction vessel 110 is provided at the rear end thereof with a second filter 112. A first long visual cup 113 is also arranged on the pipeline between the salifying extraction kettle 14 and the first distillation kettle 16. The rear end of the second condensation reaction kettle 110 is also connected with a gas storage barrel 114. A third filter 211 is also installed on the pipeline between the third condensation reaction kettle 27 and the crude product crystallization kettle 28. A second visual cup 212 is also arranged on the pipeline between the first extraction kettle 21 and the second distillation kettle 23. A double cone dryer 39 is also connected to the rear end of the third centrifuge 38.
During production, a certain amount of chloroform, thioacetamide, sodium bicarbonate and 1.3-dichloroacetone are added into a first condensation reaction kettle 12, potassium hydroxide is dropwise added through a first alkali tank 15 at the condensation temperature of 50-55 ℃ and the condensation temperature of 20-25 ℃, the mixture is subjected to static layering and extraction, and a chloroform layer is combined for normal pressure recovery; and after finishing, carrying out reduced pressure distillation on the first distillation kettle to obtain a first intermediate.
Adding quantitative cysteine and hydrochloric acid into a second condensation reaction kettle, pumping the first intermediate into the second condensation reaction kettle, heating to 108-; pumping quantitative chloroform for extraction, combining the extract liquid, distilling at normal pressure and recovering the chloroform; and (5) decompressing and rectifying to obtain a second intermediate.
Adding quantitative purified water, a second intermediate, nitrovinylamine and a methyl mercaptan absorption system into a third condensation reaction kettle 27, and reacting at 50 ℃ for 18 hours; pumping quantitative acetone and active carbon, heating and refluxing for 4 hours, obtaining a crude product of nizatidine through pressure filtration, cooling and centrifugation, dissolving the crude product in acetone reflux at 58-64 ℃, performing cold separation at 0-5 ℃ to obtain a recrystallized crude product, performing acetone reflux solution at 58-64 ℃, filtering, performing cold separation at 0-5 ℃, and drying to obtain a finished product of nizatidine.
Example 1:
a pharmaceutical intermediate production device combination comprises a first intermediate production device combination 1, a second intermediate production device combination 2 and a finished product production device combination 3, wherein a chloroform metering tank 11 is arranged at the front end of the first intermediate production device combination 1, the rear end of the chloroform metering tank is connected with a first condensation reaction kettle 12 through a pipeline, the rear end of the first condensation reaction kettle is connected with a first filter 13 through a pipeline, the rear end of the first filter is connected with a salifying extraction kettle 14 through a pipeline, the salifying extraction kettle is also connected with a first alkali tank 15, the rear end of the salifying extraction kettle is connected with a first distillation kettle 16 through a pipeline, the rear end of the first distillation kettle is connected with a first reduced pressure distillation kettle 17 through a pipeline, a first condenser 18 is arranged on the pipeline at the rear end of the first reduced pressure distillation kettle, a first intermediate 19 is connected on the pipeline at the rear end of the first condenser, a second intermediate receiving tank is connected with a second condensation reaction kettle 110, the upper part of the second condensation reaction kettle is also connected with a hydrochloric acid head tank 111; the rear end of the second condensation reaction kettle is connected with a first extraction kettle 21 through a pipeline, the upper part of the first extraction kettle is also provided with a second alkali tank 22, the rear end of the first extraction kettle is connected with a second distillation kettle 23 through a pipeline, the rear end of the second distillation kettle is connected with a second reduced pressure distillation kettle 24 through a pipeline, the pipeline at the rear end of the second reduced pressure distillation kettle is provided with a second condenser 25, the pipeline at the rear end of the second condenser is provided with a second intermediate receiving tank 26, the rear end of the second intermediate receiving tank is connected with a third condensation reaction kettle 27, the rear end of the third condensation reaction kettle is connected with a crude product crystallization kettle 28 through a pipeline, the rear end of the crude product crystallization kettle is provided with a first centrifuge 29, and the rear end of the first centrifuge is connected with a first crude product acetone; second midbody receiving groove 26 rear end has crude product dissolving kettle 31 through the tube coupling, crude product dissolving kettle rear end has recrystallization cauldron 32 through the tube coupling, second centrifuge 33 is installed to recrystallization cauldron rear end, second crude product acetone mother liquor geosyncline 34 is installed to second centrifuge rear end, recrystallization dissolving kettle 35 is installed to second centrifuge rear end, recrystallization dissolving kettle rear end has fourth filter 36 through the tube coupling, fourth filter rear end is connected with finished product crystallization cauldron 37, finished product crystallization cauldron rear end is connected with third centrifuge 38, third centrifuge rear end is connected with finished product acetone mother liquor geosyncline 310.
Example 2:
a pharmaceutical intermediate production device combination comprises a first intermediate production device combination 1, a second intermediate production device combination 2 and a finished product production device combination 3, wherein a chloroform metering tank 11 is arranged at the front end of the first intermediate production device combination 1, the rear end of the chloroform metering tank is connected with a first condensation reaction kettle 12 through a pipeline, the rear end of the first condensation reaction kettle is connected with a first filter 13 through a pipeline, the rear end of the first filter is connected with a salifying extraction kettle 14 through a pipeline, the salifying extraction kettle is also connected with a first alkali tank 15, the rear end of the salifying extraction kettle is connected with a first distillation kettle 16 through a pipeline, the rear end of the first distillation kettle is connected with a first reduced pressure distillation kettle 17 through a pipeline, a first condenser 18 is arranged on the pipeline at the rear end of the first reduced pressure distillation kettle, a first intermediate 19 is connected on the pipeline at the rear end of the first condenser, a second intermediate receiving tank is connected with a second condensation reaction kettle 110, the upper part of the second condensation reaction kettle is also connected with a hydrochloric acid head tank 111; the rear end of the second condensation reaction kettle is connected with a first extraction kettle 21 through a pipeline, the upper part of the first extraction kettle is also provided with a second alkali tank 22, the rear end of the first extraction kettle is connected with a second distillation kettle 23 through a pipeline, the rear end of the second distillation kettle is connected with a second reduced pressure distillation kettle 24 through a pipeline, the pipeline at the rear end of the second reduced pressure distillation kettle is provided with a second condenser 25, the pipeline at the rear end of the second condenser is provided with a second intermediate receiving tank 26, the rear end of the second intermediate receiving tank is connected with a third condensation reaction kettle 27, the rear end of the third condensation reaction kettle is connected with a crude product crystallization kettle 28 through a pipeline, the rear end of the crude product crystallization kettle is provided with a first centrifuge 29, and the rear end of the first centrifuge is connected with a first crude product acetone; second midbody receiving groove 26 rear end has crude product dissolving kettle 31 through the tube coupling, crude product dissolving kettle rear end has recrystallization cauldron 32 through the tube coupling, second centrifuge 33 is installed to recrystallization cauldron rear end, second crude product acetone mother liquor geosyncline 34 is installed to second centrifuge rear end, recrystallization dissolving kettle 35 is installed to second centrifuge rear end, recrystallization dissolving kettle rear end has fourth filter 36 through the tube coupling, fourth filter rear end is connected with finished product crystallization cauldron 37, finished product crystallization cauldron rear end is connected with third centrifuge 38, third centrifuge rear end is connected with finished product acetone mother liquor geosyncline 310. The second condensation reaction vessel 110 is provided at the rear end thereof with a second filter 112.
Example 3:
a pharmaceutical intermediate production device combination comprises a first intermediate production device combination 1, a second intermediate production device combination 2 and a finished product production device combination 3, wherein a chloroform metering tank 11 is arranged at the front end of the first intermediate production device combination 1, the rear end of the chloroform metering tank is connected with a first condensation reaction kettle 12 through a pipeline, the rear end of the first condensation reaction kettle is connected with a first filter 13 through a pipeline, the rear end of the first filter is connected with a salifying extraction kettle 14 through a pipeline, the salifying extraction kettle is also connected with a first alkali tank 15, the rear end of the salifying extraction kettle is connected with a first distillation kettle 16 through a pipeline, the rear end of the first distillation kettle is connected with a first reduced pressure distillation kettle 17 through a pipeline, a first condenser 18 is arranged on the pipeline at the rear end of the first reduced pressure distillation kettle, a first intermediate 19 is connected on the pipeline at the rear end of the first condenser, a second intermediate receiving tank is connected with a second condensation reaction kettle 110, the upper part of the second condensation reaction kettle is also connected with a hydrochloric acid head tank 111; the rear end of the second condensation reaction kettle is connected with a first extraction kettle 21 through a pipeline, the upper part of the first extraction kettle is also provided with a second alkali tank 22, the rear end of the first extraction kettle is connected with a second distillation kettle 23 through a pipeline, the rear end of the second distillation kettle is connected with a second reduced pressure distillation kettle 24 through a pipeline, the pipeline at the rear end of the second reduced pressure distillation kettle is provided with a second condenser 25, the pipeline at the rear end of the second condenser is provided with a second intermediate receiving tank 26, the rear end of the second intermediate receiving tank is connected with a third condensation reaction kettle 27, the rear end of the third condensation reaction kettle is connected with a crude product crystallization kettle 28 through a pipeline, the rear end of the crude product crystallization kettle is provided with a first centrifuge 29, and the rear end of the first centrifuge is connected with a first crude product acetone; second midbody receiving groove 26 rear end has crude product dissolving kettle 31 through the tube coupling, crude product dissolving kettle rear end has recrystallization cauldron 32 through the tube coupling, second centrifuge 33 is installed to recrystallization cauldron rear end, second crude product acetone mother liquor geosyncline 34 is installed to second centrifuge rear end, recrystallization dissolving kettle 35 is installed to second centrifuge rear end, recrystallization dissolving kettle rear end has fourth filter 36 through the tube coupling, fourth filter rear end is connected with finished product crystallization cauldron 37, finished product crystallization cauldron rear end is connected with third centrifuge 38, third centrifuge rear end is connected with finished product acetone mother liquor geosyncline 310. A first long visual cup 113 is also arranged on the pipeline between the salifying extraction kettle 14 and the first distillation kettle 16.
Example 4:
a pharmaceutical intermediate production device combination comprises a first intermediate production device combination 1, a second intermediate production device combination 2 and a finished product production device combination 3, wherein a chloroform metering tank 11 is arranged at the front end of the first intermediate production device combination 1, the rear end of the chloroform metering tank is connected with a first condensation reaction kettle 12 through a pipeline, the rear end of the first condensation reaction kettle is connected with a first filter 13 through a pipeline, the rear end of the first filter is connected with a salifying extraction kettle 14 through a pipeline, the salifying extraction kettle is also connected with a first alkali tank 15, the rear end of the salifying extraction kettle is connected with a first distillation kettle 16 through a pipeline, the rear end of the first distillation kettle is connected with a first reduced pressure distillation kettle 17 through a pipeline, a first condenser 18 is arranged on the pipeline at the rear end of the first reduced pressure distillation kettle, a first intermediate 19 is connected on the pipeline at the rear end of the first condenser, a second intermediate receiving tank is connected with a second condensation reaction kettle 110, the upper part of the second condensation reaction kettle is also connected with a hydrochloric acid head tank 111; the rear end of the second condensation reaction kettle is connected with a first extraction kettle 21 through a pipeline, the upper part of the first extraction kettle is also provided with a second alkali tank 22, the rear end of the first extraction kettle is connected with a second distillation kettle 23 through a pipeline, the rear end of the second distillation kettle is connected with a second reduced pressure distillation kettle 24 through a pipeline, the pipeline at the rear end of the second reduced pressure distillation kettle is provided with a second condenser 25, the pipeline at the rear end of the second condenser is provided with a second intermediate receiving tank 26, the rear end of the second intermediate receiving tank is connected with a third condensation reaction kettle 27, the rear end of the third condensation reaction kettle is connected with a crude product crystallization kettle 28 through a pipeline, the rear end of the crude product crystallization kettle is provided with a first centrifuge 29, and the rear end of the first centrifuge is connected with a first crude product acetone; second midbody receiving groove 26 rear end has crude product dissolving kettle 31 through the tube coupling, crude product dissolving kettle rear end has recrystallization cauldron 32 through the tube coupling, second centrifuge 33 is installed to recrystallization cauldron rear end, second crude product acetone mother liquor geosyncline 34 is installed to second centrifuge rear end, recrystallization dissolving kettle 35 is installed to second centrifuge rear end, recrystallization dissolving kettle rear end has fourth filter 36 through the tube coupling, fourth filter rear end is connected with finished product crystallization cauldron 37, finished product crystallization cauldron rear end is connected with third centrifuge 38, third centrifuge rear end is connected with finished product acetone mother liquor geosyncline 310. The rear end of the second condensation reaction kettle 110 is also connected with a gas storage barrel 114.
Example 5:
a pharmaceutical intermediate production device combination comprises a first intermediate production device combination 1, a second intermediate production device combination 2 and a finished product production device combination 3, wherein a chloroform metering tank 11 is arranged at the front end of the first intermediate production device combination 1, the rear end of the chloroform metering tank is connected with a first condensation reaction kettle 12 through a pipeline, the rear end of the first condensation reaction kettle is connected with a first filter 13 through a pipeline, the rear end of the first filter is connected with a salifying extraction kettle 14 through a pipeline, the salifying extraction kettle is also connected with a first alkali tank 15, the rear end of the salifying extraction kettle is connected with a first distillation kettle 16 through a pipeline, the rear end of the first distillation kettle is connected with a first reduced pressure distillation kettle 17 through a pipeline, a first condenser 18 is arranged on the pipeline at the rear end of the first reduced pressure distillation kettle, a first intermediate 19 is connected on the pipeline at the rear end of the first condenser, a second intermediate receiving tank is connected with a second condensation reaction kettle 110, the upper part of the second condensation reaction kettle is also connected with a hydrochloric acid head tank 111; the rear end of the second condensation reaction kettle is connected with a first extraction kettle 21 through a pipeline, the upper part of the first extraction kettle is also provided with a second alkali tank 22, the rear end of the first extraction kettle is connected with a second distillation kettle 23 through a pipeline, the rear end of the second distillation kettle is connected with a second reduced pressure distillation kettle 24 through a pipeline, the pipeline at the rear end of the second reduced pressure distillation kettle is provided with a second condenser 25, the pipeline at the rear end of the second condenser is provided with a second intermediate receiving tank 26, the rear end of the second intermediate receiving tank is connected with a third condensation reaction kettle 27, the rear end of the third condensation reaction kettle is connected with a crude product crystallization kettle 28 through a pipeline, the rear end of the crude product crystallization kettle is provided with a first centrifuge 29, and the rear end of the first centrifuge is connected with a first crude product acetone; second midbody receiving groove 26 rear end has crude product dissolving kettle 31 through the tube coupling, crude product dissolving kettle rear end has recrystallization cauldron 32 through the tube coupling, second centrifuge 33 is installed to recrystallization cauldron rear end, second crude product acetone mother liquor geosyncline 34 is installed to second centrifuge rear end, recrystallization dissolving kettle 35 is installed to second centrifuge rear end, recrystallization dissolving kettle rear end has fourth filter 36 through the tube coupling, fourth filter rear end is connected with finished product crystallization cauldron 37, finished product crystallization cauldron rear end is connected with third centrifuge 38, third centrifuge rear end is connected with finished product acetone mother liquor geosyncline 310. A third filter 211 is also installed on the pipeline between the third condensation reaction kettle 27 and the crude product crystallization kettle 28.
Example 6:
a pharmaceutical intermediate production device combination comprises a first intermediate production device combination 1, a second intermediate production device combination 2 and a finished product production device combination 3, wherein a chloroform metering tank 11 is arranged at the front end of the first intermediate production device combination 1, the rear end of the chloroform metering tank is connected with a first condensation reaction kettle 12 through a pipeline, the rear end of the first condensation reaction kettle is connected with a first filter 13 through a pipeline, the rear end of the first filter is connected with a salifying extraction kettle 14 through a pipeline, the salifying extraction kettle is also connected with a first alkali tank 15, the rear end of the salifying extraction kettle is connected with a first distillation kettle 16 through a pipeline, the rear end of the first distillation kettle is connected with a first reduced pressure distillation kettle 17 through a pipeline, a first condenser 18 is arranged on the pipeline at the rear end of the first reduced pressure distillation kettle, a first intermediate 19 is connected on the pipeline at the rear end of the first condenser, a second intermediate receiving tank is connected with a second condensation reaction kettle 110, the upper part of the second condensation reaction kettle is also connected with a hydrochloric acid head tank 111; the rear end of the second condensation reaction kettle is connected with a first extraction kettle 21 through a pipeline, the upper part of the first extraction kettle is also provided with a second alkali tank 22, the rear end of the first extraction kettle is connected with a second distillation kettle 23 through a pipeline, the rear end of the second distillation kettle is connected with a second reduced pressure distillation kettle 24 through a pipeline, the pipeline at the rear end of the second reduced pressure distillation kettle is provided with a second condenser 25, the pipeline at the rear end of the second condenser is provided with a second intermediate receiving tank 26, the rear end of the second intermediate receiving tank is connected with a third condensation reaction kettle 27, the rear end of the third condensation reaction kettle is connected with a crude product crystallization kettle 28 through a pipeline, the rear end of the crude product crystallization kettle is provided with a first centrifuge 29, and the rear end of the first centrifuge is connected with a first crude product acetone; second midbody receiving groove 26 rear end has crude product dissolving kettle 31 through the tube coupling, crude product dissolving kettle rear end has recrystallization cauldron 32 through the tube coupling, second centrifuge 33 is installed to recrystallization cauldron rear end, second crude product acetone mother liquor geosyncline 34 is installed to second centrifuge rear end, recrystallization dissolving kettle 35 is installed to second centrifuge rear end, recrystallization dissolving kettle rear end has fourth filter 36 through the tube coupling, fourth filter rear end is connected with finished product crystallization cauldron 37, finished product crystallization cauldron rear end is connected with third centrifuge 38, third centrifuge rear end is connected with finished product acetone mother liquor geosyncline 310. A second visual cup 212 is also arranged on the pipeline between the first extraction kettle 21 and the second distillation kettle 23.
Example 7:
a pharmaceutical intermediate production device combination comprises a first intermediate production device combination 1, a second intermediate production device combination 2 and a finished product production device combination 3, wherein a chloroform metering tank 11 is arranged at the front end of the first intermediate production device combination 1, the rear end of the chloroform metering tank is connected with a first condensation reaction kettle 12 through a pipeline, the rear end of the first condensation reaction kettle is connected with a first filter 13 through a pipeline, the rear end of the first filter is connected with a salifying extraction kettle 14 through a pipeline, the salifying extraction kettle is also connected with a first alkali tank 15, the rear end of the salifying extraction kettle is connected with a first distillation kettle 16 through a pipeline, the rear end of the first distillation kettle is connected with a first reduced pressure distillation kettle 17 through a pipeline, a first condenser 18 is arranged on the pipeline at the rear end of the first reduced pressure distillation kettle, a first intermediate 19 is connected on the pipeline at the rear end of the first condenser, a second intermediate receiving tank is connected with a second condensation reaction kettle 110, the upper part of the second condensation reaction kettle is also connected with a hydrochloric acid head tank 111; the rear end of the second condensation reaction kettle is connected with a first extraction kettle 21 through a pipeline, the upper part of the first extraction kettle is also provided with a second alkali tank 22, the rear end of the first extraction kettle is connected with a second distillation kettle 23 through a pipeline, the rear end of the second distillation kettle is connected with a second reduced pressure distillation kettle 24 through a pipeline, the pipeline at the rear end of the second reduced pressure distillation kettle is provided with a second condenser 25, the pipeline at the rear end of the second condenser is provided with a second intermediate receiving tank 26, the rear end of the second intermediate receiving tank is connected with a third condensation reaction kettle 27, the rear end of the third condensation reaction kettle is connected with a crude product crystallization kettle 28 through a pipeline, the rear end of the crude product crystallization kettle is provided with a first centrifuge 29, and the rear end of the first centrifuge is connected with a first crude product acetone; second midbody receiving groove 26 rear end has crude product dissolving kettle 31 through the tube coupling, crude product dissolving kettle rear end has recrystallization cauldron 32 through the tube coupling, second centrifuge 33 is installed to recrystallization cauldron rear end, second crude product acetone mother liquor geosyncline 34 is installed to second centrifuge rear end, recrystallization dissolving kettle 35 is installed to second centrifuge rear end, recrystallization dissolving kettle rear end has fourth filter 36 through the tube coupling, fourth filter rear end is connected with finished product crystallization cauldron 37, finished product crystallization cauldron rear end is connected with third centrifuge 38, third centrifuge rear end is connected with finished product acetone mother liquor geosyncline 310. A double cone dryer 39 is also connected to the rear end of the third centrifuge 38.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A pharmaceutical intermediate production device assembly comprising a first intermediate production device assembly (1), a second intermediate production device assembly (2) and a finished product production device assembly (3), characterized in that: the front end of the first intermediate production device combination (1) is provided with a chloroform metering tank (11), the rear end of the chloroform metering tank is connected with a first condensation reaction kettle (12) through a pipeline, the rear end of the first condensation reaction kettle is connected with a first filter (13) through a pipeline, the rear end of the first filter is connected with a salification extraction kettle (14) through a pipeline, the salification extraction kettle is also connected with a first alkali tank (15), the rear end of the salification extraction kettle is connected with a first distillation kettle (16) through a pipeline, the rear end of the first distillation kettle is connected with a first reduced pressure distillation kettle (17) through a pipeline, the pipeline at the rear end of the first reduced pressure distillation kettle is provided with a first condenser (18), the pipeline at the rear end of the first condenser is connected with a first intermediate receiving tank (19), the rear end of the first intermediate receiving tank is connected with a second condensation reaction kettle (110), and the upper part of the second; the rear end of the second condensation reaction kettle is connected with a first extraction kettle (21) through a pipeline, the upper part of the first extraction kettle is also provided with a second alkali tank (22), the rear end of the first extraction kettle is connected with a second distillation kettle (23) through a pipeline, the rear end of the second distillation kettle is connected with a second reduced pressure distillation kettle (24) through a pipeline, the pipeline at the rear end of the second reduced pressure distillation kettle is provided with a second condenser (25), the pipeline at the rear end of the second condenser is provided with a second intermediate receiving tank (26), the rear end of the second intermediate receiving tank is connected with a third condensation reaction kettle (27), the rear end of the third condensation reaction kettle is connected with a crude product crystallization kettle (28) through a pipeline, the rear end of the crude product crystallization kettle is provided with a first centrifuge (29), and the rear end of the first centrifuge is connected with a first crude; second midbody receiving tank (26) rear end has crude product to dissolve cauldron (31) through the tube coupling, crude product dissolves cauldron rear end has recrystallization cauldron (32) through the tube coupling, second centrifuge (33) is installed to recrystallization cauldron rear end, second crude product acetone mother liquor geosyncline (34) is installed to second centrifuge rear end, recrystallization dissolves cauldron (35) is installed to second centrifuge rear end, recrystallization dissolves cauldron rear end has fourth filter (36) through the tube coupling, fourth filter rear end is connected with finished product crystallization cauldron (37), finished product crystallization cauldron rear end is connected with third centrifuge (38), third centrifuge rear end is connected with finished product acetone mother liquor geosyncline (310).
2. A pharmaceutical intermediate production device assembly according to claim 1, wherein: and a second filter (112) is arranged at the rear end of the second condensation reaction kettle (110).
3. A pharmaceutical intermediate production device assembly according to claim 1, wherein: a first long sight cup (113) is also arranged on a pipeline between the salifying extraction kettle (14) and the first distillation kettle (16).
4. A pharmaceutical intermediate production device assembly according to claim 1, wherein: the rear end of the second condensation reaction kettle (110) is also connected with a gas storage barrel (114).
5. A pharmaceutical intermediate production device assembly according to claim 1, wherein: and a third filter (211) is also arranged on a pipeline between the third condensation reaction kettle (27) and the crude product crystallization kettle (28).
6. A pharmaceutical intermediate production device assembly according to claim 1, wherein: a second long sight cup (212) is also arranged on a pipeline between the first extraction kettle (21) and the second distillation kettle (23).
7. A pharmaceutical intermediate production device assembly according to claim 1, wherein: the rear end of the third centrifugal machine (38) is also connected with a double-cone dryer (39).
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| CN113773267A (en) * | 2021-09-06 | 2021-12-10 | 安徽美诺华药物化学有限公司 | Method for recovering methyl ester from valsartan mother liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113773267A (en) * | 2021-09-06 | 2021-12-10 | 安徽美诺华药物化学有限公司 | Method for recovering methyl ester from valsartan mother liquor |
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