A metanilamide hydrochloride device

Abstract

The utility model relates to the field of organic chemical synthesis equipment discloses a kind of m-acetylaminoaniline hydrochloride device, including generation cauldron, the right side upper portion of generation cauldron is connected with synthesis cauldron by dosing assembly a, the outside fixed connection of synthesis cauldron has dosing assembly b, the left side upper portion fixed connection of synthesis cauldron has venturi tube, the lower portion fixed connection of venturi tube inside close to synthesis cauldron has auxiliary assembly, the outside fixed connection of venturi tube has connecting pipe b, the lower portion fixed connection of connecting pipe b is in synthesis cauldron lower portion, the inner wall communication of connecting pipe b has conveying pump. In the utility model, by using hydrogen chloride gas to replace traditional hydrochloric acid to carry out salting reaction, in combination with mother liquor circulation, avoid the problem of excessive mother liquor caused by the large amount of water brought by hydrochloric acid, realize mother liquor zero discharge, solve the problem of high wastewater treatment cost in traditional process from the root, meet green environmental protection production requirement.

Description

Technical Field

[0001] This utility model relates to the field of organic chemical synthesis equipment, and in particular to a device for m-acetaminoaniline hydrochloride. Background Technology

[0002] m-Acetaminoaniline hydrochloride is an important organic chemical intermediate, widely used in the synthesis and production of dyes, pharmaceuticals, pesticides, and other fields. In its traditional preparation process, a "one-pot" method is commonly used, where m-phenylenediamine, hydrochloric acid, and glacial acetic acid are directly added to a reaction vessel to carry out the salt formation reaction.

[0003] In traditional processes, m-phenylenediamine, hydrochloric acid, and glacial acetic acid are added simultaneously in a one-pot method. Hydrochloric acid is used for salt formation. However, hydrochloric acid contains a large amount of water (70%), resulting in a large amount of mother liquor generated during the process. This amount may even exceed the required amount for recycling, necessitating the discharge of some mother liquor. This leads to a large amount of wastewater and increased wastewater treatment costs. Furthermore, discharging the mother liquor as wastewater wastes some of the raw materials in the mother liquor, further increasing costs. Therefore, a m-acetaminophen hydrochloride device is proposed to solve the above problems. Utility Model Content

[0004] To overcome the above deficiencies, this utility model provides a device for methizamine hydrochloride, which aims to solve the problem in the prior art that "the traditional process uses hydrochloric acid for salt formation reaction, and the hydrochloric acid contains a large amount of water, which leads to the generation of a large amount of mother liquor. When the amount exceeds the circulation requirements, it has to be discharged, which generates a large amount of wastewater, increases the cost of sewage treatment, and wastes the raw materials in the mother liquor, increasing the production cost".

[0005] To achieve the above objectives, the present invention adopts the following technical solution: a m-acetaminophen hydrochloride device, comprising a generating vessel, a synthesis vessel connected to the upper right side of the generating vessel via a dosing component a, a dosing component b fixedly connected to the outer side of the synthesis vessel, a venturi tube fixedly connected to the upper left side of the synthesis vessel, an auxiliary component fixedly connected to the lower part of the venturi tube near the interior of the synthesis vessel, a connecting pipe b fixedly connected to the outer side of the venturi tube, the lower part of the connecting pipe b fixedly connected to the lower part of the synthesis vessel, a delivery pump communicating with the inner wall of the connecting pipe b, a three-way valve fixedly connected to the right side of the lower part of the connecting pipe b, and a filter fixedly connected to the right side of the three-way valve.

[0006] As a further description of the above technical solution: The dosing assembly a includes a support frame a, which is fixedly connected to the outside of the generating vessel. A hydrochloric acid storage tank and a sulfuric acid storage tank are fixedly connected to the upper part of the support frame a. The hydrochloric acid storage tank and the sulfuric acid storage tank are respectively connected to the inner wall of the generating vessel through a delivery pipe a. A metering pump a is fixedly connected to the outside of the delivery pipe a. A connecting pipe a is fixedly connected to the upper right side of the generating vessel. The right end of the connecting pipe a is fixedly connected to the upper part of a venturi tube. A one-way valve is fixedly connected to the inner wall of the connecting pipe a.

[0007] As a further description of the above technical solution: The dosing assembly b includes a support frame b, on the upper part of which a storage tank c, a storage tank d, and a mother liquor tank are fixedly connected. The storage tank c, storage tank d, and mother liquor tank are connected to the inside of the synthesis reactor through multiple sets of delivery pipes b, and a metering pump b is provided on the outside of the delivery pipes b.

[0008] As a further description of the above technical solution: The auxiliary components include a gas supply pipe and a gas supply ring pipe. The gas supply pipe is fixedly connected to the inner wall of the reactor and communicates with the inside of the Venturi tube. The gas supply ring pipe is arranged around the inner wall of the reactor.

[0009] As a further description of the above technical solution: The gas delivery ring pipe is surrounded by a discharge hole.

[0010] As a further description of the above technical solution: The one-way valve is provided in multiple sets, and the multiple sets of one-way valves are respectively installed on the inner wall of the delivery pipe a, the connecting pipe b, and the delivery pipe b.

[0011] As a further description of the above technical solution: The inner walls of both the generating vessel and the synthesis vessel are lined with enamel glass.

[0012] As a further description of the above technical solution: The Venturi tube, conveying pipe a, connecting pipe b, and conveying pipe b are all made of polytetrafluoroethylene.

[0013] This utility model has the following beneficial effects: 1. In this utility model, hydrogen chloride gas is used to replace traditional hydrochloric acid for the salt formation reaction. Combined with mother liquor recycling, the problem of excessive mother liquor caused by the large amount of water introduced by hydrochloric acid is avoided, and zero discharge of mother liquor is achieved. This solves the problem of high wastewater treatment cost in traditional processes from the root, and meets the requirements of green and environmentally friendly production.

[0014] 2. In this invention, the mother liquor is recovered by a filter and recycled for the next batch of reaction, avoiding the waste of raw materials caused by the discharge of mother liquor in the traditional process and significantly improving the utilization rate of raw materials; at the same time, 90% of the sulfuric acid generated in the hydrogen chloride generation kettle can be recycled for the dye manufacturing process, realizing the secondary utilization of resources and further reducing production energy consumption and raw material costs.

[0015] 3. In this utility model, the cooperation of the venturi tube and auxiliary components enables the hydrogen chloride gas to be fully mixed with the materials in the synthesis reactor, thereby improving the efficiency of the salt formation reaction. The setting of multiple one-way valves effectively prevents material backflow, ensures that the medium in each pipeline is stably transported in the set direction, reduces the risk of equipment corrosion and material contamination, and improves the operational stability of the device. Attached Figure Description

[0016] Figure 1 This is a three-dimensional structural diagram of the overall device in this utility model; Figure 2 This is a three-dimensional structural disassembly diagram of the drug delivery component b in this utility model; Figure 3 This is a three-dimensional structural diagram of the auxiliary component in this utility model.

[0017] Legend: 1. Generating vessel; 2. Dosing assembly a; 21. Support frame a; 22. Delivery pipe a; 23. Hydrochloric acid storage tank; 24. Sulfuric acid storage tank; 25. Metering pump a; 26. Connecting pipe a; 27. Check valve; 3. Synthesis vessel; 4. Dosing assembly b; 41. Support frame b; 42. Delivery pipe b; 43. Storage tank c; 44. Storage tank d; 45. Mother liquor tank; 46. Metering pump b; 5. Venturi tube; 6. Connecting pipe b; 7. Delivery pump; 8. Three-way valve; 9. Filter; 10. Auxiliary components; 101. Gas delivery pipe; 102. Gas delivery ring pipe. Detailed Implementation

[0018] 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.

[0019] Reference Figure 1 - Figure 3One embodiment of this utility model provides: a m-acetaminoaniline hydrochloride device includes a generating vessel 1, which serves as the preparation site for hydrogen chloride gas and is equipped with a stirring function. Hydrochloric acid and concentrated sulfuric acid are received through a dosing component a2. A reaction occurs in the vessel to generate hydrogen chloride gas. 98% of the concentrated sulfuric acid absorbs the water in 30% of the hydrochloric acid and releases HCl gas at the same time. 90% of the sulfuric acid produced after the reaction can be recycled for use in the dye manufacturing process. Its inner wall is lined with enamel glass, which is resistant to strong acid corrosion and ensures reaction stability. The upper right side of the generating vessel 1 is connected to the synthesis vessel 3 via a dosing assembly a2. This synthesis vessel 3 serves as the core container for the salt formation reaction, equipped with stirring and heating functions. It receives the mother liquor, m-phenylenediamine, and glacial acetic acid, and reacts with hydrogen chloride gas supplied from the generating vessel 1 to produce m-acetaminoaniline hydrochloride. Its inner wall is also lined with enamel glass, which is resistant to acid corrosion. A dosing assembly b4 is fixedly connected to the outside of the synthesis vessel 3, and a Venturi tube 5 is fixedly connected to the upper left side of the synthesis vessel 3, connecting the generating vessel 1 and the synthesis vessel 3. Utilizing fluid dynamics principles, the hydrogen chloride gas is forcibly mixed with the materials inside the synthesis vessel 3, improving mass transfer efficiency and ensuring that HCl gas fully participates in the salt formation reaction. The material is polytetrafluoroethylene, which has strong corrosion resistance.

[0020] Furthermore, an auxiliary component 10 is fixedly connected to the lower part of the Venturi tube 5 near the interior of the synthesis vessel 3. A connecting pipe b6 is fixedly connected to the outer side of the Venturi tube 5, connecting the input end of the Venturi tube 5 to the lower part of the synthesis vessel 3, and serving as a conveying channel for the reacted materials. The lower part of the connecting pipe b6 is fixedly connected to the lower part of the synthesis vessel 3, and a conveying pump 7 is connected to the inner wall of the connecting pipe b6 to provide power to pump the reactants in the synthesis vessel 3 into the Venturi tube 5 through the connecting pipe b6, forcibly mixing the hydrogen chloride gas with the materials in the synthesis vessel 3. A three-way valve 8 is fixedly connected to the right side of the lower part of the connecting pipe b6. A filter 9 is fixedly connected to the side to perform solid-liquid separation on the reacted material, separating the m-acetaminoaniline hydrochloride product and recovering the mother liquor. A pipe can be fixedly connected between the liquid output port of the filter 9 and the input end of the mother liquor tank 45 to continuously add the mother liquor to the mother liquor tank 45, realizing the recycling of the mother liquor. The filter plates and filter cloths in contact with the material are made of corrosion-resistant materials, such as reinforced polypropylene and polytetrafluoroethylene, to ensure separation efficiency and mother liquor purity. The filter 9 is an existing structure and can be implemented by those skilled in the art. Since it is existing technology, it will not be described in detail in this case.

[0021] Reference Figure 1 and Figure 2The dosing assembly a2 includes a support frame a21, which is fixedly connected to the outside of the generating vessel 1, providing stable support for the hydrochloric acid storage tank 23 and the sulfuric acid storage tank 24. The upper part of the support frame a21 is fixedly connected to the hydrochloric acid storage tank 23 and the sulfuric acid storage tank 24. The hydrochloric acid storage tank 23 stores 30% hydrochloric acid and is supplied to the generating vessel 1 via a conveying pipe a22. The sulfuric acid storage tank 24 stores 98% concentrated sulfuric acid and is supplied to the generating vessel 1 via the conveying pipe a22. The hydrochloric acid storage tank 23 and the sulfuric acid storage tank 24 are respectively connected to the inner wall of the generating vessel 1 via the conveying pipe a22. The conveying pipe a22 is made of polytetrafluoroethylene (PTFE), which is corrosion-resistant, and is used to transport hydrochloric acid and concentrated sulfuric acid from the storage tanks to the generating vessel 1. A metering pump a25 is fixedly connected to the outside of support frame a21. The metering pump a25 is fixedly connected to the outside of support frame a21 to precisely control the delivery of hydrochloric acid and concentrated sulfuric acid, ensuring that the two react in proportion and guaranteeing the efficiency of HCl gas generation. The metering pumps are controlled and powered by external control equipment. A connecting pipe a26 is fixedly connected to the upper right side of generator 1 to transport the hydrogen chloride gas generated in generator 1 to venturi tube 5. The material is suitable for acidic gas environment. The right end of connecting pipe a26 is fixedly connected to the upper part of venturi tube 5. A one-way valve 27 is fixedly connected to the inner wall of connecting pipe a26 to prevent gas or liquid backflow. If the pressure in generator 1 is too high, it will prevent acid from flowing back into the storage tank or hydrogen chloride gas from flowing backward, thus protecting the pipeline and equipment.

[0022] Reference Figure 1 and Figure 2 The dosing assembly b4 includes a support frame b41, which securely supports storage tanks c43 and d44, and mother liquor tank 45 to ensure stable dosing. Level gauges are installed on the outside of each storage tank for easy worker observation. Storage tanks c43, d44, and mother liquor tank 45 are fixedly connected to the upper part of the support frame b41. Storage tank c43 stores m-phenylenediamine raw material and is supplied to the synthesis reactor 3 via conveying pipe b42. Storage tank d44 stores glacial acetic acid raw material and is supplied to the synthesis reactor 3 via conveying pipe b42. Mother liquor tank 45 stores the mother liquor recovered from the previous batch of filtration. The mother liquor is circulated to the synthesis reactor 3 through the conveying pipe b42, achieving zero discharge. Storage tanks c43, d44, and 45 are connected to the inside of the synthesis reactor 3 through multiple sets of conveying pipes b42. They are made of polytetrafluoroethylene, which is corrosion resistant, and are used to transport m-phenylenediamine, glacial acetic acid, and mother liquor to the synthesis reactor 3. A metering pump b46 is installed on the outside of the conveying pipe b42 to accurately control the amount of raw materials and mother liquor added, ensuring a stable synthesis reaction ratio and improving product purity. It is controlled and powered by an external control device. The metering pump b46 is fixedly connected to the outside of the support frame b41.

[0023] Reference Figure 1 - Figure 3The auxiliary component 10 includes a gas delivery pipe 101 and a gas delivery ring pipe 102. The gas delivery pipe 101 is fixedly connected to the inner wall of the generating vessel 1 and communicates with the inside of the venturi tube 5. The gas delivery ring pipe 102 is arranged around the inner wall of the synthesis vessel 3, and a discharge hole is opened around the outside of the gas delivery ring pipe 102. The gas delivery pipe 101 introduces the hydrogen chloride gas delivered by the venturi tube 5 into the gas delivery ring pipe 102 to ensure uniform gas distribution. The gas delivery ring pipe 102, through the discharge hole, allows the hydrogen chloride gas to be evenly dispersed into the reaction system through multiple small holes, further increasing the contact area between the gas and the liquid material and accelerating the reaction process. Multiple sets of one-way valves 27 are provided. The multiple sets of one-way valves 27 are respectively installed on the inner walls of the conveying pipe a22, the connecting pipe b6, and the conveying pipe b42. The one-way valves 27 on the conveying pipe a22 and the conveying pipe b42 are used to prevent gas backflow, and the one-way valve 27 on the connecting pipe b6 is used to prevent material backflow. The inner walls of both the generating vessel 1 and the synthesis vessel 3 are lined with enamel glass. The venturi tube 5, the conveying pipe a22, the connecting pipe b6, and the conveying pipe b42 are made of polytetrafluoroethylene.

[0024] Working principle: In operation, hydrogen chloride gas is first prepared in generating reactor 1. Hydrochloric acid storage tank 23 and sulfuric acid storage tank 24 are respectively fed into generating reactor 1 through delivery pipe a22 under the control of metering pump a25. The two react inside the reactor. The 98% concentrated sulfuric acid absorbs water from the hydrochloric acid and releases hydrogen chloride gas. The 90% sulfuric acid produced after the reaction can be recycled for use in the dye manufacturing process.

[0025] The generated hydrogen chloride gas is transported to the venturi tube 5 through connecting pipe a26. During this process, the one-way valve 27 in connecting pipe a26 prevents backflow of gas. At the same time, the synthesis reactor 3 receives raw materials through the dosing assembly b4: m-phenylenediamine from storage tank c43, glacial acetic acid from storage tank d44, and the previous batch of mother liquor recovered from mother liquor tank 45. These materials enter the synthesis reactor 3 through the delivery pipe b42 under the control of the metering pump b46. The one-way valve 27 in the delivery pipe b42 prevents reverse flow of materials.

[0026] When hydrogen chloride gas passes through the Venturi tube 5, it is forcibly mixed with the material pumped into the synthesis vessel 3 through the connecting pipe b6. Powered by the delivery pump 7, the gas then enters the gas delivery ring pipe 102 through the gas delivery pipe 101 of the auxiliary component 10, and is evenly dispersed into the synthesis vessel 3 through the discharge hole on the ring pipe. It reacts fully with m-phenylenediamine and glacial acetic acid at 85°C to generate m-acetaminoaniline hydrochloride.

[0027] After the reaction is complete, the material enters the filter 9 through the connecting pipe b6 to separate the product, meta-acetaminoaniline hydrochloride. The filtered mother liquor is recycled to the mother liquor tank 45 for use in the next batch reaction. The one-way valve 27 in the connecting pipe b6 ensures that the material is conveyed in the set direction to avoid backflow and contamination.

[0028] Finally, it should be noted that the above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Although the present utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. A device for producing m-acetaminoaniline hydrochloride, characterized in that: The apparatus includes a generating vessel (1), a synthesis vessel (3) connected to the upper right side of the generating vessel (1) via a dosing assembly a (2), a dosing assembly b (4) fixedly connected to the outer side of the synthesis vessel (3), a venturi tube (5) fixedly connected to the upper left side of the synthesis vessel (3), an auxiliary assembly (10) fixedly connected to the lower part of the venturi tube (5) near the interior of the synthesis vessel (3), a connecting pipe b (6) fixedly connected to the outer side of the venturi tube (5), the lower part of the connecting pipe b (6) fixedly connected to the lower part of the synthesis vessel (3), a delivery pump (7) connected to the inner wall of the connecting pipe b (6), a three-way valve (8) fixedly connected to the right side of the lower part of the connecting pipe b (6), and a filter (9) fixedly connected to the right side of the three-way valve (8).

2. The device for m-acetaminoaniline hydrochloride according to claim 1, characterized in that: The dosing assembly a (2) includes a support frame a (21), which is fixedly connected to the outside of the generating vessel (1). A hydrochloric acid storage tank (23) and a sulfuric acid storage tank (24) are fixedly connected to the upper part of the support frame a (21). The hydrochloric acid storage tank (23) and the sulfuric acid storage tank (24) are respectively connected to the inner wall of the generating vessel (1) through a delivery pipe a (22). A metering pump a (25) is fixedly connected to the outside of the delivery pipe a (22). A connecting pipe a (26) is fixedly connected to the upper right side of the generating vessel (1). The right end of the connecting pipe a (26) is fixedly connected to the upper part of the venturi tube (5). A one-way valve (27) is fixedly connected to the inner wall of the connecting pipe a (26).

3. The device for producing m-acetaminoaniline hydrochloride according to claim 1, characterized in that: The dosing assembly b (4) includes a support frame b (41). The upper part of the support frame b (41) is fixedly connected to a storage tank c (43), a storage tank d (44) and a mother liquor tank (45). The storage tank c (43), the storage tank d (44) and the mother liquor tank (45) are connected to the inside of the synthesis vessel (3) through multiple sets of conveying pipes b (42). A metering pump b (46) is provided on the outside of the conveying pipes b (42).

4. The apparatus for m-acetaminoaniline hydrochloride according to claim 1, characterized in that: The auxiliary component (10) includes a gas supply pipe (101) and a gas supply ring pipe (102). The gas supply pipe (101) is fixedly connected to the inner wall of the generating vessel (1) and communicates with the inside of the venturi tube (5). The gas supply ring pipe (102) is arranged around the inner wall of the synthesis vessel (3).

5. The apparatus for m-acetaminoaniline hydrochloride according to claim 4, characterized in that: The gas delivery ring pipe (102) has a discharge hole around its outer side.

6. The apparatus for m-acetaminoaniline hydrochloride according to claim 2, characterized in that: The one-way valve (27) is provided in multiple sets, and the multiple sets of one-way valves (27) are respectively installed on the inner wall of the conveying pipe a (22), the connecting pipe b (6) and the conveying pipe b (42).

7. The apparatus for m-acetaminoaniline hydrochloride according to claim 1, characterized in that: The inner walls of both the generating vessel (1) and the synthesis vessel (3) are lined with enamel glass.

8. The apparatus for m-acetaminoaniline hydrochloride according to claim 3, characterized in that: The Venturi tube (5), conveying pipe a (22), connecting pipe b (6) and conveying pipe b (42) are made of polytetrafluoroethylene.

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