Production device of 2-hydroxypyridine-N-oxide

Abstract

The utility model discloses a production device of 2-hydroxypyridine-N-oxide, and belongs to the technical field of chemical production devices. The device comprises an oxidation hydrolysis reaction kettle with a first frequency conversion stirrer, a solid feeding tank, a 2-chloropyridine head tank with a first rotor flow meter, a hydrogen peroxide head tank with a second rotor flow meter, a glacial acetic acid head tank with a third rotor flow meter, a condenser, a waste liquid collecting tank, a DCS (Distributed Control System) and an online pH meter, the device comprises a first frequency conversion stirrer, a feed liquid acidification reaction kettle with a second frequency conversion stirrer, a fourth rotor flow meter, a hydrochloric acid head tank, a first delivery pump, a pressure gauge, a second delivery pump and a two-in-one plate-and-frame filter press. All the devices of the device are connected through pipelines and valves. The amount of hydrogen peroxide and glacial acetic acid and the titration speed are controlled by utilizing a rotor flow meter so as to control the generation amount of peracetic acid in the reaction process, so that the 2-hydroxypyridine-N-oxide achieves high quality and high yield in production, and meanwhile, the potential safety hazard in production is solved.

Description

Technical Field

[0001] This utility model relates to the technical field of chemical production equipment, and in particular to a reaction apparatus for producing 2-hydroxypyridine-N-oxide. Background Technology

[0002] 2-Hydroxypyridine-N-oxide is commonly used as an intermediate in organic synthesis, acting as a catalyst or oxidant in some organic reactions. It can also be used to prepare complexes of metal ions such as copper and iron, and is frequently used in coordination chemistry research. 2-Hydroxypyridine-N-oxide is an important compound, and studies have found that it plays a special role in preventing wood degradation by white-rot fungi.

[0003] 2-Hydroxypyridine-N-oxide (Formula I, abbreviated as HOPO) is an important chemical reagent that can be used as a condensing agent in combination with 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC1). EDC1 activates the carboxylic acid and facilitates condensation and dehydration, while HOPO increases the yield and reduces byproducts. The EDC1 / HOPO combination condensing agent has been widely used in the synthesis of the drug nemateviquid. The high demand for this compound presents new challenges for research and the development of large-scale production processes and equipment. A key challenge is how to produce high-quality, high-yield 2-hydroxypyridine-N-oxide while controlling the formation of peracetic acid to reduce the safety hazards associated with its production. Utility Model Content

[0004] To address the problems existing in the prior art, this utility model provides a production device for 2-hydroxypyridine-N-oxide. By controlling the amount of raw materials added and the dripping rate through a rotor flow meter, the production of 2-hydroxypyridine-N-oxide can achieve high quality and high yield. At the same time, the safety hazards of 2-hydroxypyridine-N-oxide in production can be reduced by controlling the amount of peracetic acid generated.

[0005] The specific technical solution to achieve the above objectives is as follows: a production apparatus for 2-hydroxypyridine-N-oxide, comprising an oxidation hydrolysis apparatus, a feed solution acid precipitation apparatus, and a solid-liquid separation apparatus. The oxidation hydrolysis apparatus includes an oxidation hydrolysis reactor equipped with a first variable frequency stirrer, a solid feed tank, a 2-chloropyridine high-level tank equipped with a first rotor flowmeter, a hydrogen peroxide high-level tank equipped with a second rotor flowmeter, a glacial acetic acid high-level tank equipped with a third rotor flowmeter, a condenser, and a waste liquid collection tank. The feed solution acid precipitation apparatus is equipped with a DCS control system, an online pH meter, a feed solution acid precipitation reactor equipped with a second variable frequency stirrer, a fourth rotor flowmeter, a hydrochloric acid high-level tank, a first feed pump, and a pressure gauge. The solid-liquid separation apparatus includes a second feed pump and a two-in-one plate and frame filter press. All equipment in the oxidation hydrolysis apparatus, feed solution acid precipitation apparatus, and solid-liquid separation apparatus are directly connected via pipelines and valves.

[0006] Furthermore, the 2-chloropyridine high-level tank, hydrogen peroxide high-level tank, and glacial acetic acid high-level tank are connected to the oxidative hydrolysis reactor via valves and a rotor flow meter.

[0007] Furthermore, the oxidative hydrolysis reactor is connected to a condenser and a waste liquid collection tank via valves and pipes.

[0008] Furthermore, the oxidation hydrolysis reactor is equipped with a jacketed heater, and the heat source is either steam or heat transfer oil.

[0009] Furthermore, the feed solution acid precipitation device is equipped with a DCS control system, which enables the online pH meter to be linked with the valve at the bottom of the hydrochloric acid high-level tank.

[0010] Furthermore, the outlet of the oxidation hydrolysis reactor is connected to the inlet of the feed liquid acid precipitation reactor via a first feed pump, and the outlet of the feed liquid acid precipitation reactor is connected to the two-in-one plate and frame filter press via a second feed pump.

[0011] Furthermore, the solid-liquid separation device includes a two-in-one plate and frame filter press.

[0012] The beneficial effects of this invention are as follows: The device connects the 2-chloropyridine high-level tank, hydrogen peroxide high-level tank, and glacial acetic acid high-level tank to the oxidative hydrolysis reactor via a first rotor flow meter, a second rotor flow meter, and a third rotor flow meter, respectively. Compared with traditional production equipment, this invention utilizes rotor flow meters to control the amount of hydrogen peroxide and glacial acetic acid, as well as the titration rate, thereby controlling the amount of peracetic acid generated during the reaction. This results in high-quality and high-yield production of 2-hydroxypyridine-N-oxide, and also eliminates the safety hazards associated with the production of 2-hydroxypyridine-N-oxide. Attached Figure Description

[0013] Figure 1This is a schematic diagram of a reaction apparatus for producing 2-hydroxypyridine-N-oxide;

[0014] In the diagram: 1. 2-Chloroprene high-level tank; 2. Hydrogen peroxide high-level tank; 3. Glacial acetic acid high-level tank; 4. First rotor flow meter; 5. Second rotor flow meter; 6. Third rotor flow meter; 7. Solid feed tank; 8. First variable frequency stirrer; 9. Oxidation hydrolysis reactor; 10. Condenser; 11. Waste liquid collection tank; 12. First feed pump; 13. Pressure gauge; 14. Fourth rotor flow meter; 15. Second variable frequency stirrer; 16. Hydrochloric acid high-level tank; 17. DCS control system; 18. Online pH meter; 19. Feed liquid acid precipitation reactor; 20. Second feed pump; 21. Two-in-one plate and frame filter press. Detailed Implementation

[0015] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0016] Figure 1 A reaction apparatus for producing 2-hydroxypyridine-N-oxide includes an oxidation-hydrolysis unit, a feed solution acid precipitation unit, and a solid-liquid separation unit. The oxidation-hydrolysis unit, used for oxidation and hydrolysis reactions, includes a solid feed tank 7, a 2-chloropyridine high-level tank 1 equipped with a first rotor flowmeter 4, a hydrogen peroxide high-level tank 2 equipped with a second rotor flowmeter 5, a glacial acetic acid high-level tank 3 equipped with a third rotor flowmeter 6, a condenser 10, a waste liquid collection tank 11, and an oxidation-hydrolysis reactor 9 equipped with a first variable frequency stirrer 8. The oxidation-hydrolysis reactor 9 is equipped with a jacketed heater, with the heat source being either steam or heat transfer oil. The feed solution acid precipitation unit is equipped with a DCS control system 17, an online pH meter 18, a feed solution acid precipitation reactor 19 equipped with a second variable frequency stirrer 15, a hydrochloric acid high-level tank 16, a fourth rotor flowmeter 14, a first feed pump 12, and a pressure gauge 13. The solid-liquid separation unit includes a second feed pump 20 and a two-in-one plate and frame filter press 21.

[0017] All equipment in the aforementioned oxidation hydrolysis device, feed liquid acid precipitation device, and solid-liquid separation device are directly connected through pipes and valves.

[0018] The raw materials added to the 2-chloropyridine high-level tank 1, hydrogen peroxide high-level tank 2, and glacial acetic acid high-level tank 3 are controlled by the first rotor flowmeter 4, the second rotor flowmeter 5, and the third rotor flowmeter 6, respectively, and flow to the oxidation hydrolysis reactor 9 through corresponding pipelines. The first variable frequency stirrer 8 stirs the mixture, and hot steam is introduced into the jacket to heat it to a certain temperature for the oxidation reaction. After the reaction is completed, the valve connected to the condenser 10 is opened, and the waste liquid separated by distillation is collected in the waste liquid collection tank 11. After the solution in the oxidation hydrolysis reactor 9 is evaporated to dryness, the jacket is cooled to room temperature by water. Then, caustic soda flakes and a certain amount of other ingredients are added to the oxidation hydrolysis reactor 9 through the solid feed tank 7. A certain amount of water is heated to a certain temperature by hot steam through the jacket to carry out a hydrolysis reaction. The hydrolysis reaction solution is controlled by the fourth rotor flow meter 14 and transported from the outlet of the oxidation hydrolysis reactor 9 to the acid precipitation reactor 19 equipped with the second variable frequency stirrer 15 via the first feed pump 12. The DCS control system 17 enables the online pH meter 18 to be linked with the valve at the bottom of the hydrochloric acid high-level tank 16 to control the hydrochloric acid to enter the acid precipitation reactor 19. After the acid precipitation reaction reaches a certain pH value, the reaction solution is transported to the two-in-one plate and frame filter press 21 via the second feed pump 20 to finally obtain the product 2-hydroxypyridine-N-oxide.

[0019] It will be apparent to those skilled in the art that this invention is not limited to the details of the exemplary embodiments described above, and that it can be implemented in other specific forms without departing from the spirit or essential characteristics of this invention. Therefore, the embodiments should be considered illustrative and non-limiting in all respects, and the scope of this invention is defined by the appended claims rather than the foregoing description. Thus, all variations intended to fall within the meaning and scope of equivalents of the claims are encompassed within this invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0020] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A device for producing 2-hydroxypyridine-N-oxide, comprising an oxidative hydrolysis device, a feed liquid acid separation device, and a solid-liquid separation device, wherein the oxidative hydrolysis device comprises an oxidative hydrolysis reactor (9), a 2-chloropyridine high tank (1), a hydrogen peroxide high tank (2), a glacial acetic acid high tank (3), and a solid feeding tank (7), and the feed liquid acid separation device comprises a feed liquid acid separation reactor (19) and a hydrochloric acid high tank (16), characterized in that: The 2-chloropyridine high tank (1), hydrogen peroxide high tank (2), glacial acetic acid high tank (3) are connected with the oxidation hydrolysis reactor (9) by the first rotor flowmeter (4), the second rotor flowmeter (5), the third rotor flowmeter (6) respectively, the discharge port of the oxidation hydrolysis reactor (9) is connected to the feed inlet of the feed liquid acid separation reactor (19) through the first feed pump (12) and the fourth rotor flowmeter (14), the discharge port of the feed liquid acid separation reactor (19) is connected to the solid-liquid separation device through the second feed pump (20).

2. The production apparatus according to claim 1, characterized by: The oxidation hydrolysis reactor (9) is connected with the condenser (10) and the waste liquid collecting tank (11) through valves and pipelines.

3. The production apparatus according to claim 2, characterized in that: The oxidation hydrolysis reactor (9) is provided with a jacket heater, and the heat source is one of steam and conductive oil.

4. The production apparatus according to claim 3, characterized by: The feed liquid acid separation device is provided with a DCS control system (17), so that the on-line pH meter (18) is linked with the valve at the bottom of the hydrochloric acid high tank.

5. The production apparatus according to claim 4, characterized in that: The solid-liquid separation device comprises a two-in-one plate-and-frame filter press (21).

6. The production apparatus according to claim 5, characterized in that: The oxidation hydrolysis reactor (9) is provided with a first variable frequency stirrer (8), and the feed liquid acid separation reactor (19) is provided with a second variable frequency stirrer (15).

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