Synthetic reaction pH adjusting device
By designing a pH adjustment device for drug synthesis reaction, dynamic adjustment of pH value in the reactor is achieved, the problems of inflexible pH adjustment and safety risks in the prior art are solved, and the stability and yield of the reaction are improved.
Patent Information
- Application Number
- CN202420335590.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Priority Date
- 2023-10-30
- Filing Date
- 2024-02-23
- Publication Date
- 2024-12-27
- Estimated Expiration
- 2034-02-23
AI Technical Summary
During the small molecule drug synthesis reaction, it is difficult for the prior art to dynamically adjust the pH value in the reactor, resulting in a deviation from expectations, affecting the precipitation of the target compound, and the operation is cumbersome and safety risks are present.
A synthetic reaction pH adjustment device is designed, including a reactor, a processor, a temperature control device, an acid tank, an alkali tank, a peristaltic pump, an agitator, a temperature sensor and a pH sensor, and the reaction kettle is automatically adjusted through real-time monitoring and automatic adjustment. The pH value of the , realizes dynamic adjustment.
It improves the flexibility and accuracy of pH adjustment of the synthetic reaction, reduces the cumbersomeness and safety risks of personnel operation, ensures the stability of reaction conditions and the effective precipitation of target compounds.
Smart Images
Figure CN222240234U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of pharmaceutical synthesis equipment, in particular to a synthesis reaction pH regulating device. Background Art
[0002] Currently, during the synthesis reaction of small molecule drugs, experimenters need to stably control the pH value in the reactor to meet the expected experimental conditions. The usual practice is to insert a pH meter into the reactor and observe the pH change with the naked eye; and when the pH deviates from the expected value of the reaction, manually add acid / base solvents to the reactor through an acid / base burette to adjust the pH value; the entire adjustment process will continue until the reaction is completed.
[0003] For experimenters, frequent and periodic observation and adjustment are required, which is cumbersome. Moreover, for some experiments that last longer, multiple experimenters may be required to monitor alternately. During the personnel replacement process, there will also be handover risks in the control of experimental reaction conditions.
[0004] In most synthetic experiments, for the safety of the experimental process, the reactor is placed in a closed fume hood; the experimenters need to open the fume hood when making adjustments, which poses certain safety risks.
[0005] At present, there are some solutions in the industry that can add acid and base solvents to the reactor in a timely and quantitative manner. Such solutions are usually preset before the reaction in order to ensure the precipitation of materials in the later stage of the reaction process. Such solutions lack flexibility and dynamic adjustment capabilities, and the pH value may deviate from expectations, resulting in the problem of failure to precipitate the target compound. Utility Model Content
[0006] The main purpose of the utility model is to provide a synthesis reaction pH regulating device, aiming to achieve dynamic regulation of the pH value of the synthesis reaction and improve the flexibility of the pH value regulation of the synthesis reaction.
[0007] To achieve the above-mentioned purpose, the synthetic reaction pH regulating device proposed in the utility model is used to regulate the pH value in the reactor of the synthetic reaction. The synthetic reaction pH regulating device comprises:
[0008] Reactor;
[0009] processor;
[0010] A temperature control device, on which the reactor is disposed, and the temperature control device is communicatively connected with the processor;
[0011] Acid barrels;
[0012] lye barrels;
[0013] A first acid liquid pipe, one end of which is disposed in the acid liquid barrel, and the other end of which is disposed in the reaction kettle; a first peristaltic pump is disposed on the first acid liquid pipe, and the first peristaltic pump is used to add the acid liquid in the acid liquid barrel into the reaction kettle;
[0014] a first alkali liquid pipe, one end of which is arranged in the alkali liquid barrel, and the other end of which is arranged in the reactor; a second peristaltic pump is arranged on the first alkali liquid pipe, and the second peristaltic pump is used to add the alkali liquid in the alkali liquid barrel into the reactor;
[0015] a stirrer, the stirrer being communicatively connected with the processor;
[0016] A fixed frame, one end of the stirrer is arranged on the fixed frame, and the other end of the stirrer is arranged in the reaction kettle;
[0017] A temperature sensor, the temperature sensor is used to obtain the temperature value in the reactor, and the temperature sensor is communicatively connected with the processor; and
[0018] The pH sensor is used to obtain the pH value in the reaction kettle, and the pH sensor is connected to the processor for communication.
[0019] Optionally, the reaction kettle comprises a kettle body and a kettle cover, and the kettle body and the kettle cover are sealed and connected.
[0020] Optionally, the temperature sensor is disposed through the kettle cover and the lower end thereof is located below the reaction liquid surface.
[0021] Optionally, the pH sensor is disposed through the kettle cover and the lower end thereof is located below the reaction liquid surface.
[0022] Optionally, the other end of the first acid liquid pipe passes through the kettle cover and is located above the reaction liquid surface; the other end of the first alkali liquid pipe passes through the kettle cover and is located above the reaction liquid surface.
[0023] Optionally, it also includes:
[0024] a second acid liquid pipe, one end of which is disposed in the acid liquid barrel, and the other end of which is disposed in the reactor; a first injection pump is disposed on the second acid liquid pipe, and the first injection pump is used to add the acid liquid in the acid liquid barrel into the reactor;
[0025] A second alkali liquid pipe, one end of which is arranged in the alkali liquid barrel, and the other end of which is arranged in the reactor; a second injection pump is arranged on the second alkali liquid pipe, and the second injection pump is used to add the alkali liquid in the alkali liquid barrel into the reactor.
[0026] Optionally, the other end of the second acid liquid pipe passes through the kettle cover and is located above the reaction liquid level; the other end of the second alkali liquid pipe passes through the kettle cover and is located above the reaction liquid level.
[0027] Optionally, the reactor package further comprises a sealing assembly for sealing the reactor body and the reactor cover.
[0028] Optionally, the sealing assembly includes a first flange arranged at the upper end of the kettle body, a second flange arranged at the lower end of the kettle cover and abutting against the first flange, a sealing gasket arranged between the first flange and the second flange, and a clamp connecting and fixing the first flange and the second flange.
[0029] Optionally, a camera is also included, and the camera is used to obtain the real-time reaction conditions in the reactor.
[0030] The technical solution of the utility model realizes dynamic adjustment of the pH value of the synthesis reaction through a reaction kettle, a processor, a temperature control device, an acid barrel, an alkali barrel, a first acid pipe, a first peristaltic pump, a first alkali pipe, a second peristaltic pump, a stirrer, a fixing frame, a temperature sensor and a pH sensor, thereby improving the flexibility of adjusting the pH value of the synthesis reaction. BRIEF DESCRIPTION OF THE DRAWINGS
[0031] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the utility model. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying creative work.
[0032] Figure 1 This is a schematic diagram of the structure of an embodiment of a pH regulating device for a synthesis reaction of the utility model;
[0033] Figure 2 for Figure 1 A partial enlarged view of point A in the middle.
[0034] The main component symbols are described as follows:
[0035] Reactor 1, kettle body 11, first flange 111, kettle cover 12, second flange 121, sealing assembly 13, sealing gasket 131, clamp 132, temperature control device 2, acid liquid barrel 31, alkali liquid barrel 41, first acid liquid pipe 32, first peristaltic pump 321, second acid liquid pipe 33, first injection pump 331, first alkali liquid pipe 42, second peristaltic pump 421, second alkali liquid pipe 43, second injection pump 431, agitator 5, fixing bracket 6, temperature sensor 7, pH sensor 8.
[0036] The realization of the purpose, functional features and advantages of the utility model will be further explained in conjunction with embodiments and with reference to the accompanying drawings. DETAILED DESCRIPTION
[0037] The realization of the purpose, functional features and advantages of the utility model will be further explained in conjunction with embodiments and with reference to the accompanying drawings.
[0038] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.
[0039] It should be noted that if the embodiments of the present invention involve directional indications such as up, down, left, right, front, back, etc., then the directional indications are only used to explain the relative position relationship, movement status, etc. between the components in a certain specific posture as shown in the accompanying drawings. If the specific posture changes, the directional indication will also change accordingly.
[0040] In addition, if there are descriptions involving "first", "second", etc. in the embodiments of the utility model, the descriptions of "first", "second", etc. are only used for descriptive purposes and cannot be understood as indicating or suggesting their relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In addition, the technical solutions between the various embodiments can be combined with each other, but they must be based on the ability of ordinary technicians in the field to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection required by the utility model.
[0041] The utility model provides a pH regulating device for a synthesis reaction.
[0042] In the embodiment of the present utility model, Figures 1-2As shown, the synthesis reaction pH regulating device is used to adjust the pH value in the reactor of the drug synthesis reaction, and the synthesis reaction pH regulating device includes a reactor 1, a processor, a temperature control device 2, an acid liquid barrel 31, an alkali liquid barrel 41, a first acid liquid pipe 32, a first alkali liquid pipe 42, an agitator 5, a fixing frame 6, a temperature sensor 7 and a pH sensor 8; the reactor 1 is arranged on the temperature control device 2, and the temperature control device 2 is communicatively connected with the processor; one end of the first acid liquid pipe 32 is arranged in the acid liquid barrel 31, and the other end is arranged in the reactor 1; the first acid liquid pipe 32 is provided with a first peristaltic pump 321, and the first peristaltic pump 321 is used to add the acid in the acid liquid barrel 31 into the reactor 1; the first One end of the alkali liquid pipe 42 is arranged in the alkali liquid barrel 41, and the other end is arranged in the reactor 1; the first alkali liquid pipe 42 is provided with a second peristaltic pump 421, and the second peristaltic pump 421 is used to add the alkali liquid in the alkali liquid barrel 41 into the reactor 1; the agitator 5 is connected to the processor in communication; the agitator 5 includes a stirring rod and a stirring motor driving the stirring rod to rotate, and the stirring motor is connected to the processor in communication; one end of the agitator 5 is arranged on the fixed frame 6, and the other end of the agitator 5 is arranged in the reactor 1; the temperature sensor 7 is used to obtain the temperature value in the reactor 1, and the temperature sensor 7 is connected to the processor in communication; the pH sensor 8 is used to obtain the pH value in the reactor 1, and the pH sensor 8 is connected to the processor in communication. The temperature control device 2 can be a high and low temperature integrated temperature control device; the synthesis reaction pH adjustment device can be used to adjust the pH value of the drug synthesis reaction.
[0043] The technical solution of the utility model realizes dynamic adjustment of the pH value of the synthesis reaction through a reaction kettle 1, a processor, a temperature control device 2, an acid liquid barrel 31, an alkali liquid barrel 41, a first acid liquid pipe 32, a first peristaltic pump 321, a first alkali liquid pipe 42, a second peristaltic pump 421, a stirrer 5, a fixing frame 6, a temperature sensor 7 and a pH sensor 8, thereby improving the flexibility of adjusting the pH value of the synthesis reaction.
[0044] Specifically, in order to facilitate the addition of synthetic drugs, the reactor 1 includes a reactor body 11 and a reactor cover 12, and the reactor body 11 and the reactor cover 12 are sealed and connected. By setting the reactor 11 and the reactor cover 12, and the reactor body 11 and the reactor cover 12 are sealed and connected, the addition of synthetic reactants can be facilitated by opening the reactor cover 12, and the reactor cover 12 is covered after the addition of the synthetic reactants is completed, so as to facilitate the addition of synthetic drug reactants. The reactor can be a split reactor, and the reactor body and the reactor cover can be frosted glass sealed. The reactor cover 12 can be a three-mouth or four-mouth glass reactor cover.
[0045] Specifically, in order to facilitate the fixing of the temperature sensor 7 , the temperature sensor 7 is penetrated through the kettle cover 12 and the lower end thereof is located below the reaction liquid surface.
[0046] Specifically, in order to facilitate the fixation of the pH sensor 8, the pH sensor 8 is penetrated through the kettle cover 12 and the lower end thereof is located below the reaction liquid surface.
[0047] Specifically, in order to facilitate the fixation of the first acid liquid pipe 32 and the first alkali liquid pipe 42, the other end of the first acid liquid pipe 32 passes through the kettle cover 12 and the other end of the first acid liquid pipe 32 is located above the reaction liquid surface; the other end of the first alkali liquid pipe 42 passes through the kettle cover 12 and the other end of the first alkali liquid pipe 42 is located above the reaction liquid surface.
[0048] Specifically, in order to achieve more accurate control of the pH value of the synthesis reaction, improve the yield of the synthesis reaction, and achieve the precipitation of the target compound. The synthesis reaction pH adjustment device also includes a second acid liquid pipe 33 and a second alkali liquid pipe 43; one end of the second acid liquid pipe 33 is arranged in the acid liquid barrel 31, and the other end is arranged in the reactor 1; the second acid liquid pipe 33 is provided with a first injection pump 331, and the first injection pump 331 is used to add the acid liquid in the acid liquid barrel 31 to the reactor 1; one end of the second alkali liquid pipe 43 is arranged in the alkali liquid barrel 41, and the other end is arranged in the reactor 1; the second alkali liquid pipe 43 is provided with a second injection pump 431, and the second injection pump 431 is used to add the alkali liquid in the alkali liquid barrel 41 to the reactor 1. By means of the reactor 1, the processor, the temperature control device 2, the acid liquid barrel 31, the alkali liquid barrel 41, the first acid liquid pipe 32, the first peristaltic pump 321, the second acid liquid pipe 33, the first injection pump 331, the first alkali liquid pipe 42, the second peristaltic pump 421, the second alkali liquid pipe 43, the second injection pump 431, the agitator 5, the fixing frame 6, the temperature sensor 7 and the pH sensor 8, the pH value of the synthesis reaction can be more accurately controlled, the yield of the synthesis reaction can be improved, and the precipitation of the target compound can be achieved.
[0049] The pH value of the synthesis reaction can be precisely controlled by accurately adding the acid in the acid barrel 31 into the reactor 1 through the first injection pump 331 and accurately adding the alkali in the alkali barrel 41 into the reactor 1 through the second injection pump 431.
[0050] Specifically, in order to facilitate the fixation of the second acid liquid pipe 33 and the second alkali liquid pipe 43, the other end of the second acid liquid pipe 33 passes through the kettle cover 12 and the other end of the second acid liquid pipe 33 is located above the reaction liquid surface; the other end of the second alkali liquid pipe 43 passes through the kettle cover 12 and the other end of the second alkali liquid pipe 43 is located above the reaction liquid surface.
[0051] Specifically, in order to better seal the kettle body 11 and the kettle cover 12 , the reactor 1 further includes a sealing component 13 for sealing the kettle body 11 and the kettle cover 12 .
[0052] Specifically, in order to further seal the kettle body 11 and the kettle cover 12, the sealing assembly 13 includes a first flange 111 arranged at the upper end of the kettle body, a second flange 121 arranged at the lower end of the kettle cover and abutting against the first flange 111, a sealing gasket 131 arranged between the first flange 111 and the second flange 121, and a clamp 132 connecting and fixing the first flange 111 and the second flange 121.
[0053] Specifically, in order to monitor the reaction conditions inside the reactor, a camera is also included, and the camera is used to obtain the real-time reaction conditions inside the reactor.
[0054] The working principle of the practical synthesis reaction pH regulating device is as follows: after adding reactants to the kettle body 11, the kettle cover 12 is closed, the temperature control device 2 is turned on and the agitator 5 is started through the processor; according to the reaction temperature of the drug synthesis reaction, the reaction temperature range of the temperature control device 2 is set through the processor. After the drug synthesis reaction starts, the optimal reaction pH range is determined according to the optimal reaction pH value of the drug synthesis reaction, and the first peristaltic pump 321 and the first injection pump 331 are used to extract the acid in the acid barrel 31 and the second peristaltic pump 421 and the second injection pump 431 are used to extract the alkali in the alkali barrel 41 to control the reaction solution in the reactor 1 within the optimal reaction pH range. After the staff or the processor determines through the camera that the drug synthesis reaction in the reactor is completed, the staff turns off the temperature control device 2 or the processor controls the temperature control device 2 to turn off.
[0055] When the pH sensor 8 detects that the pH value of the solution is much lower than the minimum pH value of the optimal reaction pH range, the pH sensor 8 sends the real-time pH value to the processor. After the processor determines that the real-time pH value is much lower than the minimum pH value of the optimal reaction pH range, the processor controls the second peristaltic pump 421 to add alkali solution to the reactor through the first alkali solution pipe 42. When the processor obtains that the real-time pH value of the pH sensor 8 is the optimal reaction pH value, the processor controls the second peristaltic pump 421 to turn off. When the pH sensor 8 detects that the pH value of the solution is much higher than the maximum pH value of the optimal reaction pH range, the pH sensor 8 sends the real-time pH value to the processor. After the processor determines that the real-time pH value is much higher than the maximum pH value of the optimal reaction pH range, the processor controls the first peristaltic pump 321 to add acid solution to the reactor through the first acid solution pipe 22. When the processor obtains that the real-time pH value of the pH sensor 8 is the optimal reaction pH value, the processor controls the second peristaltic pump 421 to turn off. When the pH sensor 8 detects that the real-time pH value of the solution is greater than the maximum pH value in the optimal reaction pH range, the pH sensor 8 sends the real-time pH value to the processor. After the processor determines that the real-time pH value is greater than the maximum pH value in the optimal reaction pH range, the processor controls the second peristaltic pump 421 to close and controls the first injection pump 331 to add acid to the reactor through the second acid pipe 33. When the processor obtains that the real-time pH value of the pH sensor 8 is the optimal reaction pH value, the processor controls the first injection pump 331 to close; when the pH sensor 8 detects that the pH value of the solution is less than the minimum pH value in the optimal reaction pH range, the pH sensor 8 sends the real-time pH value to the processor. After the processor determines that the real-time pH value is less than the minimum pH value in the optimal reaction pH range, the processor controls the second injection pump 431 to add alkali solution to the reactor through the first alkali solution pipe 42. When the processor obtains that the real-time pH value of the pH sensor 8 is the optimal reaction pH value, the processor controls the second injection pump 431 to close. For example, the reaction pH of the drug synthesis reaction is 5, and the optimal reaction pH range is 4-7; when the pH sensor 8 detects that the pH value of the solution is 2, after the processor determines that 2 is much smaller than 4, the processor controls the second peristaltic pump 421 to add alkali solution into the reactor through the first alkali solution pipe 42; when the pH sensor 8 detects that the pH value of the solution is 10, after the processor determines that 10 is much larger than 7, the processor controls the first peristaltic pump 321 to add acid into the reactor through the first acid solution pipe 32; when the pH sensor 8 detects that the real-time pH value of the solution is 7.5, after the processor determines that 7.5 is greater than 7, the processor controls the second peristaltic pump 411 to close and controls the first injection pump 331 to add acid into the reactor through the second acid solution pipe 33, and when the processor obtains the real-time pH value of the pH sensor 8 as 4.5; after the processor determines that 4.5 is less than 4, the processor controls the second peristaltic pump 411 to add alkali solution into the reactor through the first alkali solution pipe 42.
[0056] The above are only preferred embodiments of the present invention, and do not limit the patent scope of the present invention. All equivalent structural changes made by using the contents of the present invention specification and drawings under the concept of the present invention, or directly / indirectly applied in other related technical fields are included in the patent protection scope of the present invention.
Claims
1. A synthesis reaction pH adjustment device, characterized in that: Used to adjust the pH value in the reactor of the synthesis reaction, the synthesis reaction pH adjustment device comprises: Reactor (1); processor; A temperature control device (2), the reaction kettle (1) is arranged on the temperature control device (2), and the temperature control device (2) is communicatively connected with the processor; Acid barrel (31); Lye barrel (41); a first acid liquid pipe (32), one end of the first acid liquid pipe (32) being arranged in the acid liquid barrel (31), and the other end of the first acid liquid pipe (32) being arranged in the reaction kettle (1); a first peristaltic pump (321) being arranged on the first acid liquid pipe (32), and the first peristaltic pump (321) being used to add the acid liquid in the acid liquid barrel (31) into the reaction kettle (1); a first alkali liquid pipe (42), one end of the first alkali liquid pipe (42) being arranged in the alkali liquid barrel (41), and the other end of the first alkali liquid pipe (42) being arranged in the reaction kettle (1); a second peristaltic pump (421) being arranged on the first alkali liquid pipe (42), and the second peristaltic pump (421) being used for adding the alkali liquid in the alkali liquid barrel (41) into the reaction kettle (1); a stirrer (5), the stirrer (5) being communicatively connected to the processor; A fixed frame (6), one end of the stirrer (5) is arranged on the fixed frame (6), and the other end of the stirrer (5) is arranged in the reaction kettle (1); a temperature sensor (7), the temperature sensor (7) being used to obtain the temperature value in the reaction kettle (1), the temperature sensor (7) being communicatively connected to the processor; and A pH sensor (8), the pH sensor (8) is used to obtain the pH value in the reaction kettle (1), and the pH sensor (8) is communicatively connected to the processor.
2. A synthesis reaction pH regulating device according to claim 1, characterized in that: The reaction kettle (1) comprises a kettle body (11) and a kettle cover (12), and the kettle body (11) and the kettle cover (12) are sealed and connected.
3. A synthesis reaction pH regulating device according to claim 2, characterized in that: The temperature sensor (7) is disposed through the kettle cover (12) and the lower end thereof is located below the reaction liquid surface.
4. A synthesis reaction pH regulating device according to claim 2, characterized in that: The pH sensor (8) is disposed through the kettle cover (12) and the lower end thereof is located below the reaction liquid surface.
5. A synthesis reaction pH regulating device according to claim 2, characterized in that: The other end of the first acid liquid pipe (32) passes through the kettle cover (12) and is located above the reaction liquid surface; the other end of the first alkali liquid pipe (42) passes through the kettle cover (12) and is located above the reaction liquid surface.
6. A synthesis reaction pH regulating device according to claim 2, characterized in that: Also includes: a second acid liquid pipe (33), one end of the second acid liquid pipe (33) being arranged in the acid liquid barrel (31), and the other end of the second acid liquid pipe (33) being arranged in the reaction kettle (1); a first injection pump (331) being arranged on the second acid liquid pipe (33), and the first injection pump (331) being used to add the acid liquid in the acid liquid barrel (31) into the reaction kettle (1); A second alkali liquid pipe (43), one end of the second alkali liquid pipe (43) is arranged in the alkali liquid barrel (41), and the other end is arranged in the reactor (1); a second injection pump (431) is arranged on the second alkali liquid pipe (43), and the second injection pump (431) is used to add the alkali liquid in the alkali liquid barrel (41) into the reactor (1).
7. A synthesis reaction pH regulating device according to claim 6, characterized in that: The other end of the second acid liquid pipe (33) passes through the kettle cover (12) and the other end of the second acid liquid pipe (33) is located above the reaction liquid surface; the other end of the second alkali liquid pipe (43) passes through the kettle cover (12) and the other end of the second alkali liquid pipe (43) is located above the reaction liquid surface.
8. A synthesis reaction pH regulating device according to claim 2, characterized in that: The reactor (1) further comprises a sealing assembly (13) for sealing the reactor body (11) and the reactor cover (12).
9. A synthesis reaction pH regulating device according to claim 8, characterized in that: The sealing assembly (13) comprises a first flange (111) arranged at the upper end of the kettle body, a second flange (121) arranged at the lower end of the kettle cover and abutting against the first flange (111), a sealing gasket (131) arranged between the first flange (111) and the second flange (121), and a clamp (132) connecting and fixing the first flange (111) and the second flange (121).
10. A synthesis reaction pH adjustment device according to claim 1, characterized in that: It also comprises a camera, which is used to obtain the real-time reaction conditions in the reaction kettle (1).