Hydrochloride synthesis system

Through the microchannel reactor and temperature control system in the hydrochloride synthesis system, the problem of reaction and decomposition of n-propyl chloroformate and water is solved, and efficient downy Via hydrochloride synthesis is achieved, improving the reaction yield and safety sex.

CN222342823UActive Publication Date: 2025-01-14JIANGYIN SULI CHEM
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Patent Information

Application Number
CN202323669517.3
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2023-12-29
Publication Date
2025-01-14
Estimated Expiration
2033-12-29

AI Technical Summary

Technical Problem

In the existing synthesis method of Downy Via Hydrochloride, n-propyl chloroformate reacts with water to decompose hydrogen chloride, resulting in the formation of hydrogen chloride with N,N-dimethylpropylene diamine, and can no longer be used with n-propyl chloroformate Reaction results in low reaction yield.

Method used

A hydrochloride synthesis system was designed, including mixer, microchannel reactor, propylene diamine raw material pipeline system, deionized water pipeline system and n-propyl ester raw material pipeline system, and the raw material pipeline system was fully utilized through the microchannel reactor. Mix and react, control the reaction temperature, and optimize the reaction conditions using a condenser and temperature control system.

Benefits of technology

The reaction conversion rate is improved to 99%, and the molar yield is increased to 97%, which shortens the reaction time and makes the reaction safer.

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Abstract

The utility model discloses a hydrochloride synthesis system, which comprises a blender used for premixing various received raw materials; the propylene diamine raw material pipeline system is used for storing N, N-dimethyl propylene diamine and can be used for conveying a propylene diamine raw material into the mixer; the deionized water pipeline system is used for storing deionized water and conveying the deionized water into the mixer; the n-propyl ester raw material pipeline system is used for storing n-propyl chloroformate and conveying n-propyl ester raw materials into the mixer for mixing; the micro-channel reactor is communicated with the mixer and is used for providing a reaction place for various raw materials; and the product intermediate storage tank is connected with the micro-channel reactor and is used for storing the intermediate product produced by the micro-channel reactor. Compared with an existing reaction mode, the reaction conversion rate can reach 99%, the molar yield can reach 97%, the reaction yield of propamocarb hydrochloride can be effectively improved, meanwhile, the reaction time can be shortened, and the reaction is safer.
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Description

Technical Field

[0001] The utility model relates to the technical field of chemical synthesis devices, in particular to a hydrochloride synthesis system. Background Art

[0002] Famoxacarb hydrochloride is a toxic fungicide with protective and therapeutic effects. It is harmless to higher animals and can be used to prevent and control downy mildew of cabbage, black root disease of radish, white rust of cabbage, soil-borne diseases of tomatoes, etc.

[0003] At present, the conventional synthesis method of propamocarb hydrochloride is to prepare it by reacting N,N-dimethylpropylenediamine and n-propyl chloroformate. However, the disadvantage of the current conventional method is that n-propyl chloroformate slowly reacts with water to decompose to generate hydrogen chloride during the reaction, and the hydrogen chloride forms a salt with N,N-dimethylpropylenediamine, but cannot react with n-propyl chloroformate to generate a product, resulting in a low reaction yield. Utility Model Content

[0004] The purpose of the utility model is to solve the above problems and provide a hydrochloride synthesis system.

[0005] In order to achieve the above-mentioned purpose, the utility model specifically adopts the following technical solutions:

[0006] A hydrochloride synthesis system comprises: a mixer for premixing a plurality of received raw materials;

[0007] A propylenediamine raw material pipeline system, which is used to store N,N-dimethylpropylenediamine and can transport the propylenediamine raw material to the mixer;

[0008] A deionized water pipeline system, which is used to store deionized water and transport the deionized water to the mixer;

[0009] The n-propyl ester raw material pipeline system is used to store n-propyl chloroformate and transport the n-propyl ester raw material to the mixer for mixing;

[0010] A microchannel reactor is connected to the mixer to provide a reaction site for various raw materials;

[0011] The intermediate product storage tank is connected to the microchannel reactor and is used to store the intermediate product produced by the microchannel reactor.

[0012] As a further description of the above technical solution, the propylene diamine raw material pipeline system includes a propylene diamine storage tank, a pipeline 1 for connecting the propylene diamine storage tank and the mixer;

[0013] A discharge bottom valve 1 is arranged at the bottom of the propylenediamine storage tank, and the discharge bottom valve 1 is used to control the delivery of the propylenediamine raw material in the storage tank.

[0014] As a further description of the above technical solution, a liquid level gauge 1 is provided on the propylenediamine storage tank, and the liquid level gauge 1 is used to display the remaining amount of raw materials in the propylenediamine storage tank.

[0015] As a further description of the above technical solution, the deionized water pipeline system includes a deionized water storage tank, a pipeline 2 for connecting the deionized water storage tank and the mixer;

[0016] A second discharge bottom valve is provided at the bottom of the deionized water storage tank, and the second discharge bottom valve is used to control the delivery of deionized water in the storage tank.

[0017] As a further description of the above technical solution, a second liquid level gauge is provided on the deionized water storage tank.

[0018] As a further description of the above technical solution, the n-propyl ester raw material pipeline system includes an n-propyl ester storage tank, a pipeline three for connecting the n-propyl ester storage tank and the mixer;

[0019] A discharge bottom valve three is arranged at the bottom of the n-propyl ester storage tank, and the discharge bottom valve three is used to control the delivery of the n-propyl ester raw material in the storage tank.

[0020] As a further description of the above technical solution, a liquid level gauge three is provided on the n-propyl ester storage tank.

[0021] As a further description of the above technical solution, condenser one is arranged in pipeline one, condenser two is arranged in pipeline two, and condenser three is arranged in pipeline three.

[0022] As a further description of the above technical solution, the condenser 1, the condenser 2, the condenser 3 and the outside of the microchannel reactor are all provided with a temperature control system.

[0023] As a further description of the above technical solution, the intermediate storage tank of the product is provided with a safety valve and a liquid level gauge.

[0024] The beneficial effects of the utility model are as follows:

[0025] 1. Compared with the conventional reaction mode of propamocarb hydrochloride, the utility model can make the reaction conversion rate reach 99% and the molar yield reach 97%, which can effectively improve the reaction yield of propamocarb hydrochloride, shorten the reaction time and make the reaction safer.

[0026] In order to more clearly illustrate the structural features and functions of the present invention, the present invention is described in detail below in conjunction with the accompanying drawings and specific embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a schematic diagram of the hydrochloride synthesis system.

[0028] Figure numerals: 11, propylene diamine storage tank; 12, pipeline one; 13, discharge bottom valve one; 14, liquid level gauge one; 15, temperature control system one; 16, condenser one; 21, deionized water storage tank; 22, pipeline two; 23, discharge bottom valve two; 24, liquid level gauge two; 25, temperature control system two; 26, condenser two; 31, n-propyl ester storage tank; 32, pipeline three; 33, discharge bottom valve three; 34, liquid level gauge three; 35, temperature control system three; 36, condenser three; 4, mixer; 5, microchannel reactor; 6, product intermediate storage tank; 7, safety valve; 8, liquid level gauge four. DETAILED DESCRIPTION

[0029] In order to make the purpose, technical solution and advantages of the embodiments of the present utility model clearer, the technical solution in the embodiments of the present utility model will be clearly and completely described below in conjunction with the drawings in the embodiments of the present utility model.

[0030] like Figure 1 As shown, in one embodiment, a hydrochloride synthesis system includes a mixer 4, which is used to mix multiple received raw materials, which in this embodiment are N,N-dimethylpropylenediamine, n-propyl chloroformate and deionized water.

[0031] Regarding the supply of N,N-dimethylpropylenediamine, in the embodiment of the present application, it is achieved through a propylenediamine raw material pipeline system, and the propylenediamine raw material pipeline system is connected to the mixer 4, and the N,N-dimethylpropylenediamine can be transported to the mixer 4;

[0032] In the embodiment of the present application, deionized water is supplied through a deionized water pipeline system, which is also connected to the mixer 4 so that the deionized water can be pumped into the mixer 4. It should be noted that the propylene diamine raw material pipeline system and the deionized water pipeline system share an inlet that discharges into the mixer 4.

[0033] Regarding the supply of n-propyl chloroformate, in the embodiment of the present application, the supply is achieved through an n-propyl ester pipeline system, and the n-propyl ester pipeline system is connected to the mixer 4 to pump the n-propyl chloroformate into the mixer 4;

[0034] After the above three raw materials are pumped into the mixer 4, the mixer 4 fully mixes the various materials, and the materials flow into the microchannel reactor 5 through the mixing outlet arranged at the bottom of the mixer 4, and the reaction temperature of the materials in the microchannel reaction is controlled at 0-15°C. The materials are fully entered into the product intermediate storage tank 6 in the microchannel reactor 5 for preliminary storage of the reaction materials.

[0035] By the above technical scheme, compared with the conventional reaction of the existing reaction mode, the general mechanical stirring, the material turbulence effect is not good, the material mixing effect is not good, the reaction speed is low, the residence time of n-propyl chloromethyl in the system is long, and n-propyl chloroformate has a large amount of decomposition to produce n-propyl alcohol and hydrogen chloride, and hydrogen chloride is salified with N, N-dimethylpropylenediamine, and the generated salt can no longer react with n-propyl chloroformate to generate products, resulting in a decrease in yield. When the material is mixed by the mixer in this application and then passed into the microchannel reactor, the material turbulence effect is good, the material mixing is sufficient, the reaction speed is fast, the residence time of n-propyl chloromethyl in the system is short, and the decomposition of n-propyl chloroformate is reduced. The reaction conversion rate can be made to reach 99%, the molar yield is 97%, the reaction yield of cymoxanil hydrochloride can be effectively improved, the reaction time can be shortened, and the reaction is safer.

[0036] The propylenediamine raw material pipeline system, the deionized water pipeline system and the n-propyl ester raw material pipeline system have similar structural compositions. Specifically, the propylenediamine raw material pipeline system includes a propylenediamine storage tank 11 and a pipeline 12 for connecting the propylenediamine storage tank 11 and the mixer 4. A discharge bottom valve 13 is provided at the bottom of the propylenediamine storage tank 11, and the discharge bottom valve 13 is used to control the transportation of the propylenediamine raw material in the storage tank; a liquid level gauge 14 is provided on the propylenediamine storage tank 11, and the liquid level gauge 14 is used to display the remaining amount of raw materials in the propylenediamine storage tank 11, so as to facilitate real-time grasp and timely replenishment of raw materials into the storage tank to ensure the continuity of the reaction process.

[0037] The deionized water pipeline also includes a condenser 16, and the temperature can be controlled by the condenser 16 and the temperature control system 15. In this embodiment, the temperature of the cooling circulating liquid in the condenser 16 is controlled to be -10--5°C.

[0038] The structure of the deionized water pipeline is roughly the same as that of the propylene diamine raw material pipeline: the deionized water pipeline system includes a deionized water storage tank 21, a pipeline 22 for connecting the deionized water storage tank 21 and the mixer 4, a discharge bottom valve 23 is provided at the bottom of the deionized water storage tank 21, and the discharge bottom valve 23 is used to control the delivery of deionized water in the storage tank. A liquid level gauge 24 is provided on the deionized water storage tank 21, and also includes a temperature control system 25 and a condenser 26 to control the temperature. In this embodiment, the temperature of the circulating coolant of the condenser 26 is 0-5°.

[0039] The n-propyl ester raw material pipeline system includes an n-propyl ester storage tank 31, a pipeline three 32 for connecting the n-propyl ester storage tank 31 and the mixer 4, a discharge bottom valve three 33 is provided at the bottom of the n-propyl ester storage tank 31, and the discharge bottom valve three 33 is used to control the transportation of the n-propyl ester raw material in the storage tank. The n-propyl ester storage tank 31 is provided with a liquid level gauge three 34, and is also provided with a temperature control system three 35 and a condenser three 36 to control the internal cooling circulating liquid temperature of the condenser three 36 to -10--5°C.

[0040] At the same time, the deionized water pipeline system, the propylene diamine raw material pipeline system and the n-propyl ester raw material pipeline system all include a pump body, which is a driving device for pumping the raw materials in the pipeline into the mixer 4.

[0041] A safety valve 7 and a liquid level gauge 4 8 are provided on the product intermediate storage tank 6. The safety valve 7 can automatically open when the internal pressure of the storage tank exceeds the design limit to release excess pressure to ensure that the storage tank will not explode or other serious accidents will occur. The liquid level gauge 4 8 provides accurate liquid level information so that the operator can monitor and control the storage volume of the liquid in the storage tank in real time.

[0042] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A hydrochloride synthesis system, characterized in that: include: A mixer, used for premixing the received multiple raw materials; A propylenediamine raw material pipeline system, which is used to store N,N-dimethylpropylenediamine and can transport the propylenediamine raw material to the mixer; A deionized water pipeline system, which is used to store deionized water and transport the deionized water to the mixer; The n-propyl ester raw material pipeline system is used to store n-propyl chloroformate and transport the n-propyl ester raw material to the mixer for mixing; A microchannel reactor is connected to the mixer to provide a reaction site for various raw materials; The intermediate product storage tank is connected to the microchannel reactor and is used to store the intermediate product produced by the microchannel reactor.

2. The hydrochloride synthesis system according to claim 1, characterized in that: The propylene diamine raw material pipeline system includes a propylene diamine storage tank, and a pipeline 1 for connecting the propylene diamine storage tank and the mixer; A discharge bottom valve 1 is arranged at the bottom of the propylenediamine storage tank, and the discharge bottom valve 1 is used to control the delivery of the propylenediamine raw material in the storage tank.

3. The hydrochloride synthesis system according to claim 2, characterized in that: The propylenediamine storage tank is provided with a liquid level gauge 1, and the liquid level gauge 1 is used to display the remaining amount of raw materials in the propylenediamine storage tank.

4. The hydrochloride synthesis system according to claim 2, characterized in that: The deionized water pipeline system includes a deionized water storage tank, and a pipeline 2 for connecting the deionized water storage tank and the mixer; A second discharge bottom valve is provided at the bottom of the deionized water storage tank, and the second discharge bottom valve is used to control the delivery of deionized water in the storage tank.

5. The hydrochloride synthesis system according to claim 4, characterized in that: The deionized water storage tank is provided with a second liquid level gauge.

6. The hydrochloride synthesis system according to claim 4, characterized in that: The n-propyl ester raw material pipeline system includes an n-propyl ester storage tank, and a pipeline three for connecting the n-propyl ester storage tank and the mixer; A discharge bottom valve three is arranged at the bottom of the n-propyl ester storage tank, and the discharge bottom valve three is used to control the delivery of the n-propyl ester raw material in the storage tank.

7. The hydrochloride synthesis system according to claim 6, characterized in that: The n-propyl ester storage tank is provided with a liquid level gauge three.

8. The hydrochloride synthesis system according to claim 6, characterized in that: The pipeline one is provided with a condenser one, the pipeline two is provided with a condenser two, and the pipeline three is provided with a condenser three.

9. The hydrochloride synthesis system according to claim 8, characterized in that: The condenser 1, the condenser 2, the condenser 3 and the outside of the microchannel reactor are all provided with a temperature control system.

10. The hydrochloride synthesis system according to claim 1, characterized in that: The intermediate storage tank of the product is provided with a safety valve and a liquid level gauge.