Enzyme catalysis reaction device

By designing an enzyme-catalyzed reaction device and utilizing nitrogen bubbling and pH control, the problems of low purity and yield in enzyme-catalyzed reactions were solved, enabling the preparation of high-purity, high-yield 4-aminopiperidine compounds, thus reducing costs and time.

CN224243095UActive Publication Date: 2026-05-15SULI PHARMA TECH JIANGYIN
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
SULI PHARMA TECH JIANGYIN
Filing Date
2025-04-30
Publication Date
2026-05-15

AI Technical Summary

Technical Problem

Existing enzyme-catalyzed reaction devices suffer from problems such as low enzyme purity, low yield, and high impurity content when preparing 4-aminopiperidine compounds.

Method used

An enzyme catalytic reaction device was designed, comprising a reaction vessel, a nitrogen pipeline, a pH sensor, and a PLC control system. The pH value inside the reaction vessel is maintained between 9.0 and 10.0 by using nitrogen bubbling and pH control. Byproducts are blown away by nitrogen and the reaction process is controlled.

Benefits of technology

It improved the purity and yield of enzyme catalysis, reduced reaction costs and time, and enhanced product quality and production capacity.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to an enzyme catalysis reaction device which comprises a reaction kettle, an inlet of the reaction kettle is connected with a high-position dripping tank positioned above the reaction kettle through a pneumatic valve, the reaction kettle and the high-position dripping tank are respectively connected with a diaphragm pump, a nitrogen pipe connected to a circular pipeline at the bottom of the kettle is arranged in the reaction kettle, and small holes are distributed on the circular pipeline. A pH sensor is also arranged in the reaction kettle; and the pneumatic valve and the pH sensor are both connected with a PLC (Programmable Logic Controller). According to the reaction device disclosed by the utility model, nitrogen is introduced under liquid in the reaction kettle for bubbling, the nitrogen is more uniformly distributed in a system through the small holes in the circular pipeline at the bottom of the kettle, and a byproduct acetone is blown away from the system, so that the reaction can be carried out in the forward direction, the pH sensor and the pneumatic valve are connected with the PLC, and the pH in the reaction kettle is kept at 9-10 by controlling the opening and closing of the pneumatic valve; the yield is greatly improved, the reaction time and cost are saved, and the product quality is improved.
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Description

Technical Field

[0001] This utility model belongs to the field of pharmaceutical fine chemical technology, specifically relating to an enzyme-catalyzed reaction device. Background Technology

[0002] 4-Aminopiperidine compounds are important pharmaceutical intermediates in the chemical industry. Their preparation typically involves reacting 4-piperidinone compounds as raw materials. A common method is to directly convert 4-piperidinone compounds into 4-aminopiperidine compounds using transaminases.

[0003] The process involves adding isopropylamine, triethanolamine, and pyridoxal 5-phosphate monohydrate to dilute hydrochloric acid to prepare a buffer solution; adding a dimethyl sulfoxide solution of a 4-piperidinone compound to the buffer solution, and then adding transaminase. Because enzyme-catalyzed reactions are mild, energy-efficient, and have relatively low operating and reaction costs, and because enzyme-catalyzed reactions exhibit high stereoselectivity, reacting only with a specific isomer or conformational substrate, this is extremely useful for synthesizing compounds with specific structures. Summary of the Invention

[0004] The purpose of this invention is to provide an enzyme-catalyzed reaction device that produces enzymes with high purity, high yield, and low impurities in other configurations.

[0005] The technical solution adopted by this utility model to solve the above problems is as follows: an enzyme-catalyzed reaction device, including a reaction vessel, the inlet of the reaction vessel is connected to a high-level dropping tank located above the reaction vessel via a pneumatic valve, the inlet of the reaction vessel is also connected to a first diaphragm pump, the inlet of the high-level dropping tank is also connected to a second diaphragm pump, a nitrogen pipe extending to the bottom of the reaction vessel is provided inside the reaction vessel, a circular pipe with many small holes is also provided at the bottom of the reaction vessel, and a pH sensor is also provided inside the reaction vessel.

[0006] Preferably, the inlet of the reactor is connected in sequence to a high-level dropping tank located above the reactor via a feed valve, a flow meter, and a pneumatic valve.

[0007] Preferably, a balance pipe is also provided between the reaction vessel and the high-level dropping tank.

[0008] Preferably, the reactor is equipped with a jacket that allows for the flow of refrigerant or hot water to ensure the temperature of the reaction system.

[0009] Preferably, the reactor is equipped with a stirring mechanism, which includes a stirring shaft and stirring blades connected to the stirring shaft.

[0010] Preferably, both the reaction vessel and the high-level dropping tank are connected to a nitrogen storage tank via nitrogen pipes.

[0011] Preferably, the high-level dripping tank is also equipped with a level gauge.

[0012] Preferably, the pH sensor is connected to a PLC controller, and the PLC controller is also connected to a pneumatic valve.

[0013] Preferably, the orifice is circular, elliptical, or rectangular, and the orifice is evenly distributed on the circular pipe.

[0014] Preferably, the inlet and outlet pipes of the reactor are equipped with regulating valves.

[0015] Preferably, the circular pipe is welded to the reactor via four supports, and the four supports are evenly distributed in a ring along the circular pipe.

[0016] Preferably, the outer diameter of the circular pipe is smaller than the inner diameter of the reactor.

[0017] Compared with the prior art, the advantages of this utility model are:

[0018] This invention relates to an enzyme-catalyzed reaction apparatus that uses nitrogen gas to bubble through the liquid in the reaction vessel. Specifically, small holes in the circular pipe at the bottom of the vessel ensure a more even distribution of nitrogen gas within the system. This process blows away the acetone byproduct from the reaction, promoting a forward reaction. Simultaneously, isopropylamine is also blown away from the system, lowering the pH. A pH sensor inside the reaction vessel and a pneumatic valve under the high-level isopropylamine dropper are connected to a PLC controller. By controlling the opening and closing of the pneumatic valve, the pH inside the reaction vessel can be maintained between 9.0 and 10.0, significantly improving yield, saving reaction time and costs, and enhancing product quality and production capacity. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the enzyme-catalyzed reaction device in an embodiment of the present invention.

[0020] Figure 2 This is a schematic diagram of the circular pipe and nitrogen pipe in the reaction device in this embodiment of the present invention.

[0021] Wherein: 1 is the reaction vessel, 1.1 is the circular pipe, 1.1.1 is the support, 1.2 is the stirring mechanism, 2 is the pneumatic valve, 3 is the high-level dripping tank, 3.1 is the level gauge, 4.1 is the first diaphragm pump, 4.2 is the second diaphragm pump, 5 is the nitrogen pipe, 6 is the pH sensor, 7 is the flow meter, and 8 is the balance pipe. Detailed Implementation

[0022] The present invention will be further described in detail below with reference to the accompanying drawings and embodiments.

[0023] like Figure 1The diagram shown is a schematic representation of the enzyme-catalyzed reaction apparatus in this embodiment.

[0024] An enzyme-catalyzed reaction apparatus includes a reaction vessel 1, which is equipped with a jacket for passing coolant or hot water to ensure that the temperature of the reaction system is maintained within a certain range. The reaction vessel 1 is equipped with a stirring mechanism 1.2, which includes a stirring shaft and stirring blades connected to the stirring shaft. The inlet and outlet pipes of the reaction vessel 1 are equipped with regulating valves.

[0025] The inlet of reactor 1 is connected to a high-level dropping tank 3 located above reactor 1 via a feed valve, a flow meter 7, and a pneumatic valve 2. A balance pipe 8 is also provided between reactor 1 and the high-level dropping tank 3. Both reactor 1 and the high-level dropping tank 3 are connected to a nitrogen storage tank via nitrogen pipes. The high-level dropping tank 3 is also equipped with a level gauge 3.1. The inlet of reactor 1 is also connected to a first diaphragm pump 4.1, and the inlet of the high-level dropping tank 3 is also connected to a second diaphragm pump 4.2.

[0026] like Figure 2 The diagram shown is a schematic representation of the circular pipe and nitrogen pipe in the reaction apparatus in this embodiment.

[0027] The reactor 1 is equipped with a nitrogen pipe 5 extending to the bottom of the reactor. The bottom of the reactor 1 is also equipped with a circular pipe 1.1 covered with small holes. Several small holes are evenly arranged on the circumference of the circular pipe 1.1. The outer diameter of the circular pipe 1.1 is smaller than the inner diameter of the reactor 1. The circular pipe 1.1 is welded to the reactor 1 via four supports 1.1.1. The four supports 1.1.1 are evenly distributed in a ring along the circular pipe 1.1. The small holes are evenly distributed on the circular pipe 1.1. The small holes are circular in shape. The reactor 1 is also equipped with a pH sensor 6. The pH sensor 6 is connected to a PLC controller. The PLC controller is also connected to a pneumatic valve 2. That is, the pH sensor 6 and the pneumatic valve 2 are both connected to and controlled by the PLC controller.

[0028] The working process of this embodiment will be described in detail below with reference to the accompanying drawings:

[0029] First, nitrogen from the nitrogen storage tank is introduced into the reactor 1 and the high-level dropping tank 3 via nitrogen pipe 5, creating a nitrogen atmosphere in both reactor 1 and the high-level dropping tank 3. Then, a prepared buffer solution and a dimethyl sulfoxide solution of 4-piperidinone compounds are pumped in through the first diaphragm pump 4.1. Transaminase is added through the inlet (manhole cover) of reactor 1. Nitrogen is then introduced into the system inside the reactor via nitrogen pipe 5, which extends to the bottom of reactor 1. Small holes on the circular pipe 1.1 at the bottom of the reactor distribute the nitrogen more evenly within the system. The acetone byproduct generated in the reaction is blown out of the system and pumped into the high-level dropping tank 3 by the second diaphragm pump 4.2. The feed valve below the flow meter 7, the flow meter 7, and the pneumatic valve 2 are then opened. Isopropylamine is introduced into reactor 1. The pH sensor 6 inside reactor 1 monitors the pH of reactor 1 in real time and transmits the pH detection result to the PLC controller. When the pH value of the material in reactor 1 is 9~10, the PLC controller controls the pneumatic valve 2 to close. When the pH value of the material in reactor 1 is less than 9, the PLC controller controls the pneumatic valve 2 to open and add isopropylamine from the high-level dropping tank 2 into reactor 1. Through the interaction of pH sensor 6, PLC controller and pneumatic valve 2, the pH value of the reaction system is ensured to be 9~10. After the reaction is completed, the reactants flow out through the discharge port at the lower end of reactor 1 for post-processing to obtain enzyme catalysis.

[0030] In addition to the above embodiments, this utility model also includes other implementation methods. All technical solutions formed by equivalent transformation or equivalent substitution should fall within the protection scope of the claims of this utility model.

Claims

1. An enzyme-catalyzed reaction apparatus, characterized in that: The reactor includes a reaction vessel (1), the inlet of which is connected via a pneumatic valve (2) to a high-level dropping tank (3) located above the reaction vessel (1). The inlet of the reaction vessel (1) is also connected to a first diaphragm pump (4.1), and the inlet of the high-level dropping tank (3) is also connected to a second diaphragm pump (4.2). The reaction vessel (1) is provided with a nitrogen pipe (5) extending to the bottom of the vessel. The bottom of the reaction vessel (1) is also provided with a circular pipe (1.1) filled with small holes. The reaction vessel (1) is also provided with a pH sensor (6). The pneumatic valve (2) and the pH sensor (6) are both connected to a PLC controller.

2. The enzyme-catalyzed reaction apparatus according to claim 1, characterized in that: The inlet of the reactor (1) is connected in sequence to the high-level dripping tank (3) located above the reactor (1) via the feed valve, flow meter (7) and pneumatic valve (2).

3. The enzyme-catalyzed reaction apparatus according to claim 1, characterized in that: A balance pipe (8) is also provided between the reactor (1) and the high-level dripping tank (3).

4. The enzyme-catalyzed reaction apparatus according to claim 1, characterized in that: The reactor (1) is equipped with a jacket that allows for the flow of cooling medium or hot water to ensure the temperature of the reaction system.

5. The enzyme-catalyzed reaction apparatus according to claim 1, characterized in that: The reactor (1) is equipped with a stirring mechanism (1.2), which includes a stirring shaft and stirring blades connected to the stirring shaft.

6. The enzyme-catalyzed reaction apparatus according to claim 1, characterized in that: Both the reactor (1) and the high-level dripping tank (3) are connected to nitrogen storage tanks.

7. The enzyme-catalyzed reaction apparatus according to claim 1, characterized in that: The high-level dripping tank (3) is also equipped with a level gauge (3.1).

8. The enzyme-catalyzed reaction apparatus according to claim 1, characterized in that: The small holes are circular, elliptical, or rectangular in shape, and are evenly distributed on the circular pipe (1.1).

9. The enzyme-catalyzed reaction apparatus according to claim 1, characterized in that: The inlet and outlet pipes of the reactor (1) are equipped with regulating valves.

10. The enzyme-catalyzed reaction apparatus according to claim 1, characterized in that: The circular pipe (1.1) is welded to the reactor (1) via four supports (1.1.1), which are evenly distributed in a ring along the circular pipe.