Reaction device for preparing methyl hydrazinodithioformate

Abstract

The utility model provides a reaction device for preparing methyl hydrazinodithioformate, which is characterized in that a filter pressing mechanism and a stirring mechanism are arranged in a filter, the front end receives materials of a first reaction kettle for filter pressing and solid-liquid separation, and on the premise that solids are not transferred, solvent pulping and water pulping are sequentially performed in the filter, so that the materials in the first reaction kettle are subjected to solid-liquid separation; finally, the solid is directly conveyed into the second reaction kettle for cyclization reaction, and the whole process is carried out in a closed environment, so that the problem of odor is effectively solved, the working procedures are simplified, and meanwhile, the efficiency and the productivity are improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to the field of chemical reaction device, especially relates to a reaction device for preparing methyl hydrazine dithioformate. BACKGROUND

[0002] Methyl n-aminocardamodithioate, CAS: 5397-03-5, molecular formula: C2H6N2S2, molecular weight: 122.2124, physical property: white or greenish granules, density 314g / cm3, boiling point 207.3 degrees, flash point 79.2 degrees, easy to be oxidized, easy to discolor in air but not affect use, intermediate of new pesticide.

[0003] The existing production equipment for preparing methyl hydrazine dithioformate has the following problems:

[0004] 1. The existing technology uses centrifuge to centrifuge, and the odor is difficult to control, and the odor is easy to overflow from the high-speed centrifuge during operation.

[0005] 2. The solid is easy to run to the centrifugal liquid during centrifugation, reducing the product yield.

[0006] 3. The overall device is not continuous, and the solid material needs to be discharged from the centrifuge, and the solid material has an odor, which has a great impact on the environment.

[0007] 4. The process is complicated, and multiple devices are required to meet the process requirements, reaction, centrifugation, solid discharge, organic solvent beating, filtration, solid discharge, washing, centrifugation, solid discharge, etc. are completed in multiple processes, and the solid discharge is three times, which seriously affects the environment. INVENTION CONTENTS

[0008] Therefore, a reaction device for preparing methyl hydrazine dithioformate is needed to solve the problems in the background art.

[0009] To achieve the above purpose, the utility model provides a reaction device for preparing methyl hydrazine dithioformate, comprising:

[0010] The first reaction kettle is used for feeding related materials to prepare hydrazine sulfate by reaction, and the bottom of the first reaction kettle is provided with a first discharge port, and the first discharge port is provided with a first discharge valve;

[0011] The filter is provided with a filter press mechanism and a stirring mechanism in the inside, the top of the filter is provided with a filter feed port, the filter feed port is connected with the first discharge port, the bottom of the filter is provided with a filter discharge port, and the sidewall bottom of the filter is provided with a filter liquid outlet.

[0012] A second reaction kettle is used for carrying out a cyclization reaction, and a second feeding port is arranged at the top of the second reaction kettle and connected with the filter outlet through a second pipeline.

[0013] Further, a first receiving tank is arranged, and a first receiving port is arranged at the top of the first receiving tank and used for receiving the filtered solvent in the filter. A first liquid outlet is arranged at the bottom of the first receiving tank and connected with the liquid inlet of a first material transfer pump. The liquid outlet of the first material transfer pump is connected with a first treatment liquid inlet of a first treatment kettle.

[0014] Further, a second receiving tank is arranged, and a second receiving port is arranged at the top of the second receiving tank and used for receiving the filtered wastewater in the filter. A second liquid outlet is arranged at the bottom of the second receiving tank and connected with the liquid inlet of a second material transfer pump. The liquid outlet of the second material transfer pump is connected with a second treatment liquid inlet of a second treatment kettle.

[0015] Further, a stirrer is arranged in the first reaction kettle; and / or a pressure gauge is arranged on the first reaction kettle.

[0016] Further, a stirrer is arranged in the second reaction kettle; and / or a pressure gauge is arranged on the second reaction kettle.

[0017] Further, a stirrer is arranged in the first treatment kettle; and / or a pressure gauge is arranged on the first treatment kettle.

[0018] Further, a stirrer is arranged in the second treatment kettle; and / or a pressure gauge is arranged on the second treatment kettle.

[0019] Further, the first reaction kettle, the second reaction kettle, the second receiving tank and the first treatment kettle are respectively provided with a plurality of units.

[0020] Different from the prior art, the above technical scheme is characterized in that a filter press mechanism and a stirring mechanism are arranged in the filter. The filter press mechanism and the stirring mechanism are used for carrying out filter pressing and solid-liquid separation on the material received from the first reaction kettle. The filter press mechanism and the stirring mechanism are used for sequentially carrying out solvent beating and water beating in the filter without transferring the solid. Finally, the solid is directly delivered to the second reaction kettle for carrying out a cyclization reaction. The whole process is carried out in a closed environment, effectively solves the odor problem, reduces the process, and improves the efficiency and the production capacity. BRIEF DESCRIPTION OF DRAWINGS

[0021] Figure 1 A structural schematic diagram of a reaction device for preparing methyl hydrazine dithiocarbamate according to the embodiment;

[0022] Figure 2 A structural schematic diagram of a reaction device for preparing methyl hydrazine dithiocarbamate according to another embodiment, which is provided with a first receiving tank, a first material transfer pump and a first treatment kettle.

[0023] Figure 3 The reaction device for preparing methyl hydrazine dithiocarbamate of another embodiment is provided with a second receiving tank, a second material transfer pump and a second treatment kettle.

[0024] Figure 4 The reaction device for preparing methyl hydrazine dithiocarbamate of another embodiment is provided with two first reaction kettles and two second reaction kettles.

[0025] Figure 5 The reaction device for preparing methyl hydrazine dithiocarbamate of another embodiment is provided with two second receiving tanks and two second treatment kettles.

[0026] Explanation of reference signs:

[0027] 10, first reaction kettle; 11, filter; 111, filter pressing mechanism; 112, stirring mechanism; 12, second reaction kettle; 13, first receiving tank; 14, first material transfer pump; 15, first treatment kettle; 16, second receiving tank; 17, second material transfer pump; 18, second treatment kettle; 19, stirrer; 20, pressure gauge. DETAILED DESCRIPTION

[0028] In order to describe the technical content, structural features, purposes and effects of the technical scheme in detail, the following will be described in combination with specific embodiments and the accompanying drawings.

[0029] In this document, the term “embodiment” means that the specific features, structures or properties described in combination with the embodiment can be included in at least one embodiment of the present application. The term “embodiment” appearing in various places in the specification does not necessarily refer to the same embodiment, and does not particularly limit the independence or association between other embodiments. In principle, in this application, as long as there is no technical contradiction or conflict, each technical feature mentioned in each embodiment can be combined in any way to form a corresponding implementable technical scheme.

[0030] Unless otherwise defined, the meanings of the technical terms used in this document are the same as those commonly understood by those skilled in the art to which the present application belongs; the use of related terms in this document is only for the purpose of describing specific embodiments, and is not intended to limit the present application.

[0031] In the description of the present application, the phrase “and / or” is used to describe the logical relationship between the objects, which means that there can be three relationships, for example, A and / or B, which means that there are three cases: A exists, B exists, and A and B exist at the same time. In addition, the character “ / ” in this document generally represents the logical relationship of “or” between the associated objects before and after it.

[0032] In the present application, the terms such as "first" and "second" are merely used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual number, primary or secondary, or order relationship between the entities or operations.

[0033] In the present application, the "includes", "contains", "has", or other similar expressions used in the statements are intended to cover non-exclusive inclusion, and the expressions do not exclude the presence of additional elements in the process, method or product comprising the elements, so that the process, method or product comprising a series of elements can not only include those defined elements, but also include other elements not explicitly listed, or also include elements inherent to such process, method or product.

[0034] As the same understanding as in the "Guidelines for Examination", in the present application, the expressions such as "greater than", "less than", "exceed" are understood as not including the number; the expressions such as "above", "below", "within" are understood as including the number. In addition, in the description of the embodiments of the present application, the meaning of "multiple" is more than two (including two), and similar expressions related to "multiple" are also understood in this way, for example, "multiple groups", "multiple times", etc., unless otherwise explicitly specified.

[0035] In the description of the embodiments of the present application, the spatial-related expressions used, such as "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "perpendicular", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. The indicated orientation or position relationship is based on the orientation or position relationship shown in the specific embodiment or the drawing, and is only for the convenience of describing the specific embodiments of the present application or for the reader to understand, and does not indicate or imply that the indicated device or component must have a specific position, a specific orientation, or be constructed or operated in a specific orientation, and therefore cannot be understood as a limitation on the embodiments of the present application.

[0036] Unless otherwise explicitly specified or limited, in the description of the embodiments of the present application, the terms "mount", "connect", "connect", "fix", "set", etc. should be understood broadly. For example, the "connection" can be a fixed connection, or a detachable connection, or an integral setting; it can be a mechanical connection, or an electrical connection, or a communication connection; it can be directly connected, or indirectly connected through an intermediate medium; it can be the internal communication or interaction relationship of two elements. For those skilled in the art to which the present application belongs, the specific meaning of the above terms in the embodiments of the present application can be understood according to the specific circumstances.

[0037] Please refer to Figures 1 to 5 The embodiment provides a reaction device for preparing methyl hydrazine dithiocarbonate, comprising:

[0038] The first reaction kettle 10 is used for feeding relevant materials to prepare hydrazine sulfate by reaction, and is provided with a first discharge port at the bottom. A first discharge valve is arranged at the first discharge port. The first reaction kettle can also be referred to as a hydrazine reaction kettle. The material of the first reaction kettle needs to be able to resist chemical substances that can be contacted in the reaction process, such as CO2, H2S, SO2 and other acid gases. Therefore, the material of the first reaction kettle is preferably at least one of Monel (nickel alloy), chromium-nickel-iron alloy and acid-resistant nickel alloy, so as to prolong the service life and improve the production efficiency. In addition to the first discharge port and the first discharge valve mentioned in the embodiment, the structure of the first reaction kettle can refer to the prior art. Specifically, it can include a kettle body, a kettle cover, a kettle bottom, a kettle leg, a heater, a heating medium, a heat transfer pipeline, a cooling medium, a cooling pipeline, a motor, a bearing, a sealing system and a feeding and discharging system. Among them, the kettle body bears the pressure and temperature of the reaction material to ensure the safety of the reaction process; the kettle cover is used to seal the reaction kettle to prevent material leakage; the kettle bottom is responsible for collecting and discharging the reaction product; the kettle leg supports the whole reaction kettle; the heater and the cooling medium are used to control the reaction temperature respectively; the sealing system prevents material leakage and external impurities from entering. Preferably, the first reaction kettle has a plurality of reaction kettles to improve the reaction efficiency.

[0039] The filter 11 is provided with a filter pressing mechanism 111 and a stirring mechanism 112 in the inside, and is provided with a filter feeding port at the top. A filter feeding valve is arranged at the filter feeding port. The filter feeding port is connected with the first discharge port. The first discharge port is provided with a first discharge valve. The bottom of the filter 11 is provided with a filter discharge port. The filter discharge port is provided with a filter discharge valve. The sidewall bottom of the filter 11 is provided with a filter liquid outlet. The filter liquid outlet is provided with a filter liquid valve.

[0040] The filter press 111 can include filter plates and their supports, filter cloth, filtrate collection chamber, filter 11 non-enclosed frame and power device, etc. The filter plate and its support are the core part of the filter press, the filter plate adopts a symmetrical barrel-shaped structure, which is composed of filter cloth, filter plate and filter plate support (also known as filter plate frame). The filter plate support is used to support the filter plate, fix the filter cloth and the filter plate. The filter cloth is the main filter material, which is usually made of acid-resistant, alkali-resistant, wear-resistant and stretch-resistant synthetic fiber material. Its function is to support the suspension and the filtered solid, and at the same time, it plays a filtering role. The filtrate collection chamber is located outside the filter cloth and is used to receive the filtrate filtered through the filter cloth. Usually, a tank or a barrel is used to contain the filtrate. The filter 11 non-enclosed frame is used to fix the filter plate and the filter cloth support, to ensure the flatness and sealing of the filter cloth. The power device is the core component of the filter press, which usually uses a motor, a hydraulic station or a pneumatic element to drive the movement of the filter plate and the filter cloth, to complete the filter pressing process.

[0041] The stirring mechanism 112 can include a shaft seat, a speed reducer, a lifting oil cylinder, a main shaft and a paddle. The stirring shaft is driven to rotate by the main motor, thereby driving the stirring mechanism 112 to work. The stirring mechanism 112 can be controlled in forward and reverse rotation. When rotating counterclockwise, the blade is used to stir the material; when rotating clockwise, the filter cake can be slightly extruded. Through the operation of the power supply group and the hydraulic control valve, the stirring mechanism 112 can be raised or lowered under the action of two hydraulic cylinders. The operator can accurately operate through the sight glass observation port, and at the same time, the amplitude and speed of the stirring mechanism 112 blade working can be clearly observed.

[0042] The second reaction kettle 12 is used for carrying out a cyclization reaction, which is a reaction for forming a new carbon ring or heterocyclic ring in a molecule of an organic compound, and is also referred to as a ring-closing or ring-forming condensation. The top of the second reaction kettle 12 is provided with a second feeding port, which is connected with the filtering discharge port through a second pipeline, and a second feeding valve is arranged at the second feeding port. The second reaction kettle 12 can be made of carbon manganese steel, stainless steel, zirconium, nickel-based (Hastelloy, Monel) alloy and other composite materials. These materials can meet the process requirements in different working environments such as acid resistance, high temperature resistance, wear resistance and corrosion resistance. Specifically, the reaction kettle can be made of stainless steel materials such as SUS304 and SUS316L, which have good corrosion resistance and processing performance. The structural components of the second reaction kettle 12 can include a tank body, a jacket, a discharge pipe, a manhole, a shaft seal, a support and the like. The tank body serves as the main part of the reaction kettle and is used to contain the reaction materials. The jacket is used for heating or cooling, which can be electric heating, hot water heating, heat conduction oil circulation heating and the like. The discharge pipe is used to discharge the products or residual materials after the reaction from the reaction kettle. The manhole is used for the operator to enter the inside of the reaction kettle for cleaning or maintenance. The shaft seal ensures that the inside of the reaction kettle is isolated from the outside environment to prevent material leakage and outside air from entering. The support supports the structure of the entire reaction kettle to ensure its stable operation. Further, a damping mechanism can also be provided, including a damping buffer groove on the base, a U-shaped damping sleeve, a support leg and a pad, etc., to reduce vibration during work and reduce environmental noise. Preferably, the second reaction kettle 12 has multiple reaction kettles to improve the efficiency of the cyclization reaction.

[0043] The present application uses the filter press mechanism 111 in the filter 11 to perform filter pressing. After the reaction mother liquor is filter pressed, the solid is in the filter 11, and then solvent B, water and the like are added to the filter 11 in batches for beating and filter pressing, so that multiple process procedures can be carried out in one device, the process requirements can be effectively met, the solid material does not need to be output, the whole process is carried out in a closed device, the stench smell is effectively prevented, and the operability and safety are greatly improved under normal temperature reaction conditions. The filter press mechanism 111 in the filter 11 is used to replace the general filter 11, which has the problems of slow filtering and easy blocking. The filter press mechanism 111 directly uses a squeezing method to separate the liquid and the solid through a filter screen, so that the problem of slow filtering of the organic material, especially the oily material, which is easy to form an oil film on the filter cloth, is solved.

[0044] The working process of the novel type is as follows: in the clean first reaction kettle (5000L, enamel sulfhydryl), water, alkali, catalyst, a1 and other materials are sequentially added, the stirrer 19 in the first reaction kettle is started, and the temperature is controlled, then a2 is slowly added, after the dropwise addition is completed, the reaction is kept for a certain time, after the control sampling is qualified, the material is transferred to the filter 11, the solid-liquid separation is carried out through the filter pressing mechanism 111, after the solid-liquid separation, the liquid is transferred to the rear-end treatment, the solid is left in the filter 11, a certain amount of solvent b is continuously added to the filter 11, the stirring mechanism 112 in the filter 11 is started, and the beating is carried out, after the stirring for 30 min, the beating solvent is separated from the solid again, the beating solvent is transferred to the rear-end treatment, then a certain amount of water is added to the filter 11, the beating action is repeated, after the water washing is completed and the filter pressing is dry, the beating water is transferred to the rear-end treatment, the solid in the filter 11 is slowly scraped into powder material through the stirring mechanism 112, and finally the powder material is put into the second reaction kettle 12 for the next ring closing reaction.

[0045] The novel type is provided with the filter pressing mechanism 111 and the stirring mechanism 112 in the filter 11, the material of the first reaction kettle is received in the front end for filter pressing and solid-liquid separation, the solvent beating and water beating are sequentially carried out in the filter 11 without transferring the solid, finally the solid is directly transported to the second reaction kettle 12 for the ring closing reaction, the whole process is carried out in a closed environment, the odor problem is effectively solved, the process is reduced, and the efficiency and capacity are improved.

[0046] Further, the first receiving tank 13 is further provided, the first receiving tank 13 is a closed container, the top of the first receiving tank 13 is provided with a first receiving port, the first receiving port is provided with a first receiving valve, the bottom of the first receiving tank 13 is provided with a first liquid outlet, the first liquid outlet is provided with a first liquid outlet valve, the first liquid outlet is connected with the liquid inlet end of the first material transfer pump 14, and the liquid outlet end of the first material transfer pump 14 is connected with the first treatment liquid inlet of the first treatment kettle 15.

[0047] Further, a second receiving groove 16 is also included, the first receiving groove 13 is a closed container, the top of which is provided with a second receiving port, the second receiving port is provided with a second receiving valve, which is used to receive the filtered wastewater in the filter 11, the bottom of the second receiving groove 16 is provided with a second liquid outlet, the second liquid outlet is provided with a second liquid outlet valve, the second liquid outlet is connected with the liquid inlet end of the second material transfer pump 17, and the liquid outlet end of the second material transfer pump 17 is connected with the second treatment liquid inlet of the second treatment kettle 18. Because a large amount of wastewater is generated during beating, in order to avoid delayed treatment, the second receiving groove 16 has multiple. Correspondingly, in order to improve the water treatment efficiency, the second treatment kettle 18 has multiple.

[0048] Further, the inside of the first reaction kettle is provided with a stirrer 19; and the first reaction kettle is provided with a pressure gauge 20. The inside of the second reaction kettle 12 is provided with a stirrer 19; and / or the second reaction kettle 12 is provided with a pressure gauge 20. The inside of the first treatment kettle 15 is provided with a stirrer 19; and / or the first treatment kettle 15 is provided with a pressure gauge 20. The inside of the second treatment kettle 18 is provided with a stirrer 19; and / or the second treatment kettle 18 is provided with a pressure gauge 20.

[0049] The stirrer in the reaction kettle is the core component for realizing stirring operation, and its structure is precise and complex. The main components of the stirrer include an impeller, which transmits mechanical energy to the liquid with the movement of the rotating shaft to promote the movement of the liquid. The design and shape of the impeller are crucial to the stirring effect, and common shapes include paddle, spiral, anchor, etc., which are suitable for different stirring needs and material characteristics. The stirrer also includes a transmission device, which is usually composed of a motor and a speed reducer, which provides power and transmits power to the stirring shaft through a shaft coupling. The stirring shaft is a component that connects the impeller and the transmission device, which needs to have sufficient strength and corrosion resistance to ensure stable operation in various chemical environments. The shaft seal device is an important component of the stirrer, which prevents leakage of materials in the kettle, and common shaft seal types include mechanical seals and packing seals, which ensure that the stirrer does not leak under high temperature and high pressure conditions, ensuring the safety of the environment and operating personnel. The bearing, as an important component that supports the blades of the stirrer, is generally made of cast steel or cast iron to ensure stable operation of the stirrer. These components work together to enable the stirrer to effectively mix, heat and mass transfer materials, thereby improving the efficiency of chemical reactions and product quality.

[0050] The main function of the stirrer is to ensure that the materials can be fully mixed and uniformly distributed during the chemical reaction. The stirrer produces flow of liquid or gas medium in the reactor through its rotating motion, thereby promoting the contact and exchange between reactants, which is crucial for improving the reaction rate and efficiency. At the same time, the stirrer can also help to achieve uniform distribution of heat, especially in reactions that require heating or cooling, the stirrer can accelerate the transfer of heat, prevent local overheating or overcooling, and ensure uniform temperature throughout the reactor. In addition, the stirrer can also prevent the deposition or aggregation of solids that may occur during the reaction.

[0051] By setting the pressure gauge, the pressure situation in the reactor or processing tank can be monitored and indicated in real time, ensuring the safety and efficiency of the experimental process. The pressure gauge can help the operator understand the changing state of the material during production, control certain process parameters under specified conditions, and ensure that the product quality meets the specified requirements. By mastering the pressure parameters, the operator can provide reliable basis for monitoring and adjusting production, thereby protecting the safety of the production equipment.

[0052] It should be noted that although the above embodiments have been described in this paper, the patent protection scope of the utility model is not limited thereby. Therefore, based on the innovative idea of the utility model, the changes and modifications of the embodiments described in this paper, or the equivalent structure or equivalent process transformation made by using the contents of the utility model specification and drawings, directly or indirectly apply the above technical solutions to other related technical fields, are all included in the protection scope of the utility model patent.

Claims

1. A reaction apparatus for preparing methyl hydrazine dithiocarbamate, characterized in that, include: The first reaction vessel is used to feed relevant materials to react and prepare hydrazine sulfate. It has a first discharge port at the bottom and a first discharge valve at the first discharge port. The filter has a pressure filtration mechanism and a stirring mechanism inside. It has a filter inlet at the top, which is connected to the first outlet. It has a filter outlet at the bottom and a filter liquid outlet at the bottom of the side wall. The second reactor is used for cyclization reaction. It has a second feed inlet at the top, which is connected to the filter outlet through a second pipeline.

2. The reaction apparatus for preparing methyl hydrazine dithiocarbamate according to claim 1, characterized in that: It also includes a first receiving tank with a first receiving port at the top for receiving solvent filtered out of the filter. The bottom of the first receiving tank has a first liquid outlet, which is connected to the inlet of the first transfer pump. The outlet of the first transfer pump is connected to the first processing inlet of the first processing vessel.

3. The reaction apparatus for preparing methyl hydrazine dithiocarbamate according to claim 2, characterized in that: It also includes a second receiving tank with a second receiving port at the top for receiving wastewater filtered out of the filter. The bottom of the second receiving tank has a second liquid outlet, which is connected to the inlet of the second transfer pump. The outlet of the second transfer pump is connected to the second processing inlet of the second processing vessel.

4. The reaction apparatus for preparing methyl hydrazine dithiocarbamate according to claim 3, characterized in that: The first reactor is equipped with a stirrer inside; and / or a pressure gauge is installed on the first reactor.

5. The reaction apparatus for preparing methyl hydrazine dithiocarbamate according to claim 3, characterized in that: The second reactor is equipped with a stirrer inside; and / or a pressure gauge is installed on the second reactor.

6. The reaction apparatus for preparing methyl hydrazine dithiocarbamate according to claim 3, characterized in that: The first processing vessel is equipped with a stirrer inside; and / or a pressure gauge is installed on the first processing vessel.

7. The reaction apparatus for preparing methyl hydrazine dithiocarbamate according to claim 3, characterized in that: The second processing vessel is equipped with a stirrer inside; and / or a pressure gauge is installed on the second processing vessel.

8. The reaction apparatus for preparing methyl hydrazine dithiocarbamate according to claim 3, characterized in that: There are multiple first reaction vessels, second reaction vessels, second receiving tanks, and first processing vessels.

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