An etherification salt slag treatment device

Abstract

The application provides an etherification salt slag treatment device, which comprises a reaction kettle, a first feeding port, a second feeding port and a third feeding port which are respectively connected with a spiral conveyor, an isopropyl alcohol dropping device and waste sulfuric acid dropping device arranged on the top of the reaction kettle, a sandwich layer arranged on the side wall of the reaction kettle, temperature raising devices and temperature lowering devices which are alternately arranged in the sandwich layer, a stirring device and a distillation module. The etherification salt slag treatment device takes the reaction kettle as the core, integrates the spiral conveyor, the isopropyl alcohol / waste sulfuric acid double-path precise dropping system and the sectional temperature control sandwich layer, realizes the accurate mixing of the etherification salt slag, the isopropyl alcohol and the waste sulfuric acid according to the set mass ratio, realizes the directional hydrolysis reaction in the low-temperature environment of 10-20 DEG C through the complex effect of the double-layer propelling stirring paddle and the frame type wall scraper, and finally realizes the recovery of isopropyl bromide through the condenser and the conical flow guide separation module, so that the problems of high cost and low resource utilization rate of the separate treatment of the etherification salt slag and the hydrolysis waste sulfuric acid in the prior art are solved.

Description

Technical Field

[0001] This utility model relates to the technical field of etherified salt residue recycling and treatment, and in particular to an etherified salt residue treatment device. Background Technology

[0002] 2,4-Dichloro-5-isopropoxynitrobenzene is an important intermediate in the synthesis of propyne oxadiazon technical grade. It is generally prepared by the etherification reaction of 2,4-dichloro-5-nitrophenol. The reaction equation is as follows: Nitrobenzene (C6H5NO2) + Isopropyl bromide ((CH3)2CHBr) + Potassium carbonate (K2CO3) → Nitroisopropylbenzene (C6H4(CH(CH3)2)NO2) + Potassium bicarbonate (KHCO3) + Potassium bromide (KBr). This process generates a large amount of etherified salt residue. This type of salt residue has a complex composition. Analysis shows that the main components and their mass content are approximately: potassium bromide 35%–65%, potassium bicarbonate 30%–50%, potassium carbonate 1%–10%, 2,4-dichloro-5-isopropoxynitrobenzene 0.1%–3%, water 0.5%–3%, and other components 0.5%–10%.

[0003] The etherified salt residue contains a variety of inorganic and organic components, making it costly and complex to process, and difficult to treat directly, posing a major challenge to environmental protection.

[0004] The subsequent production of propyzinoxadiazon requires a hydrolysis reaction. The reaction principle is that oxadiazon reacts with water under the catalysis of concentrated sulfuric acid to produce the intermediate phenol ketone (abbreviated) and isopropanol. The reaction equation is as follows: C 20 H 19 ClN2O3 + H2O → C 18 H 15 ClN2O2 + (CH3)2CHOH This process generates a large amount of hydrolyzed waste sulfuric acid. This type of acid has a complex composition. Analysis shows that the main components and their mass content are approximately: sulfuric acid 50%–90%, isopropanol 5%–30%, water 10%–30%, and other components 0.5%–3%.

[0005] This waste sulfuric acid contains a variety of components, has poor appearance, high processing costs, and complex methods, making it difficult to treat directly and posing a major challenge to environmental protection.

[0006] Both types of waste are difficult and costly to treat individually, resulting in a significant waste of resources. However, combining these two types of waste for comprehensive treatment, and making full use of their effective components to carry out chemical reactions, can produce significant environmental and economic benefits. It can not only effectively treat the two types of waste, but also produce valuable industrial products as byproducts, resulting in significant economic and environmental benefits.

[0007] The principles and chemical reaction equations for the comprehensive utilization of the two types of waste are as follows: KBr + H2SO4 + (CH3)2CHOH → (CH3)2CHBr + KHSO4 + H2O HBr + (CH3)2CHOH → (CH3)2CHBr + H2O KHCO3 + H2SO4 → KHSO4 + H2O + CO2 K2CO3 + 2H2SO4 → 2KHSO4 + H2O + CO2 Utility Model Content

[0008] The purpose of this invention is to solve the problem that, in the existing technology, it is very difficult and costly to treat etherified salt residue and hydrolyzed waste sulfuric acid separately, resulting in a large waste of resources.

[0009] To achieve the above objectives, this application proposes an etherified salt residue treatment apparatus, comprising: The reactor has a first feed port, a second feed port, and a third feed port at its top; the side wall of the reactor is provided with a jacket; and the side wall of the reactor is provided with a fourth feed port that slopes downwards. The screw conveyor connected to the first feed port An isopropanol dispensing device connected to the second feed port; Waste sulfuric acid dripping device connected to the fourth feed port; A stirring device that runs vertically through the top of the reactor and extends to the bottom. The temperature control device arranged in the interlayer includes: a heating device and a cooling device that alternately surround the interlayer; The distillation module is connected to the third feed port.

[0010] The etherified salt residue treatment device of this application takes a reactor as its core and integrates a screw conveyor, a dual-path precision dripping system for isopropanol / waste sulfuric acid, and a segmented temperature control jacket to achieve precise mixing of etherified salt residue, isopropanol, and waste sulfuric acid at a set mass ratio. Through the combined action of a double-layer propulsion agitator and a frame-type wall scraper, a directional hydrolysis reaction is completed in a low-temperature environment of 10-20℃. Finally, isopropyl bromide is recovered through a condenser and a conical guide liquid separation module, while improving the waste acid reuse rate. This solves the problems of high cost and low resource utilization rate of separate treatment of two types of hazardous waste, etherified salt residue and hydrolyzed waste sulfuric acid, in the existing technology.

[0011] Furthermore, to ensure the stirring effect, the stirring device includes: a top double-layer propulsion stirring paddle; and a bottom frame stirring paddle, the gap between its outer edge and the inner wall of the reactor being ≤10mm.

[0012] Furthermore, in order to effectively control the temperature during the reaction process, the heating device is a steam coil wound along the interlayer; the cooling device is a semiconductor refrigeration chip array embedded in the interlayer, with the spacing between adjacent refrigeration chips being the same as the spacing between the steam coils.

[0013] Furthermore, to control the amount of isopropanol and hydrolyzed waste sulfuric acid added, the isopropanol adding device includes: a storage tank with a graduated window; a precision peristaltic pump, the outlet of which is connected to a second feed port via a polytetrafluoroethylene hose. The waste sulfuric acid adding device includes: a corrosion-resistant metering tank lined with polypropylene; and a pneumatic diaphragm pump, the outlet of which is connected to a third feed port.

[0014] Furthermore, to increase condensation efficiency, the distillation module includes: a condenser with a serpentine coil structure; and a distributor connected to the inlet of the condenser.

[0015] Furthermore, in order to increase the wear resistance of the screw in the screw conveyor, the screw surface of the screw conveyor is coated with a tungsten carbide coating.

[0016] Furthermore, in order to achieve precise control of the reaction temperature, the jacket of the reactor is divided into three independent temperature control zones: upper, middle, and lower. Each zone contains at least one set of heating and cooling devices.

[0017] Furthermore, the openings of the first, second, and third feed inlets are all arranged at a 45° angle downwards, and the ends of the inlets are provided with umbrella-shaped dispersion covers.

[0018] The beneficial effects of this application are as follows: 1. The etherified salt residue treatment device of this application takes a reactor as its core and integrates a screw conveyor, a dual-path precision dripping system for isopropanol / waste sulfuric acid, and a segmented temperature control jacket to achieve precise mixing of etherified salt residue, isopropanol, and waste sulfuric acid at a set mass ratio. Through the combined action of a double-layer propulsion agitator and a frame-type wall scraper, a directional hydrolysis reaction is completed in a low-temperature environment of 10-20℃. Finally, isopropyl bromide is recovered through a condenser and a conical guide liquid separation module, while improving the waste acid reuse rate. This solves the problems of high cost and low resource utilization rate of separate treatment of two types of hazardous waste, etherified salt residue and hydrolyzed waste sulfuric acid, in the existing technology.

[0019] 2. This application provides a fourth downward-sloping feed port on the side wall of the reactor. The waste sulfuric acid dripping device feeds the hydrolyzed waste sulfuric acid into the reactor from the side wall, thereby accelerating the diffusion efficiency of the hydrolyzed waste sulfuric acid.

[0020] 3. The etherification salt residue treatment device of this application is easy to operate, has no special requirements for production equipment, and produces almost no secondary pollution during the treatment process, making it suitable for industrial production. Attached Figure Description

[0021] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0022] Figure 1 This is a schematic diagram of the structure of an etherified salt residue treatment device according to an embodiment of this application; Figure 2 This is a partial cross-sectional view of the reactor in an embodiment of this application; Figure 3 This is a partial distribution diagram of the temperature control device in the embodiments of this application; Figure 4 This is a schematic diagram of the distillation module in an embodiment of this application.

[0023] Explanation of reference numerals in the attached figures: 1. Reactor; 11. First feed inlet; 12. Second feed inlet; 13. Third feed inlet; 14. Jacket; 15. Fourth feed inlet; 100. Umbrella-shaped dispersion hood; 2. Screw conveyor; 3. Isopropanol dripping device; 31. Storage tank; 32. Precision peristaltic pump; 33. Polytetrafluoroethylene hose; 4. Waste sulfuric acid dripping device; 41. Corrosion-resistant metering tank; 42. Pneumatic diaphragm pump; 5. Agitator; 51. Double-layer propeller-type agitator; 52. Frame-type agitator; 6. Temperature control device; 61. Heating device; 62. Cooling device; 7. Distillation module; 71. Condenser; 72. Dispenser. Detailed Implementation

[0024] The following will be combined with the appendix Figures 1-4 The embodiments of the technical solutions of this application are described in detail below. The following embodiments are only used to more clearly illustrate the technical solutions of this application, and are therefore merely examples and should not be used to limit the scope of protection of this application. Furthermore, the technical features involved in the various embodiments of this application described below can be combined with each other as long as they do not conflict with each other.

[0025] Example 1 like Figures 1-2 This illustration depicts an etherified salt residue treatment device according to this application. To achieve precise mixing and low-temperature directional hydrolysis, the device is centered around a reactor 1 and integrates a screw conveyor 2, an isopropanol dripping device 3, and a waste sulfuric acid dripping device 4. The reactor 1 serves as the primary reaction site, used for stirring and mixing the materials. Simultaneously, the screw conveyor 2 precisely feeds the etherified salt residue into the reactor 1 through the first feed port 11. The isopropanol dripping device 3 and the waste sulfuric acid dripping device 4 precisely control the dripping amounts of isopropanol and waste sulfuric acid through the second feed port 12 and the third feed port 13, respectively, ensuring that the three materials are precisely mixed according to a set mass ratio.

[0026] Preferably, this application includes a precision peristaltic pump 32 and a pneumatic diaphragm pump 42 on the dripping device to control the amount of isopropanol and hydrolyzed waste sulfuric acid added.

[0027] The reactor 1 is equipped with a vertically penetrating stirring device 5, including a top double-layer propeller-type stirring paddle 51 and a bottom frame-type stirring paddle 52. The double-layer propeller-type stirring paddle 51 promotes thorough mixing of materials, while the gap between the outer edge of the bottom frame-type stirring paddle 52 and the inner wall of the reactor is ≤10mm, ensuring uniform stirring of materials at the bottom of the reactor and preventing material sedimentation. Under low-temperature conditions of 10-20℃, the directional hydrolysis reaction is completed through the combined action of the stirring device 5.

[0028] Please continue to refer to Figure 3 , Figure 3 The diagram illustrates two sets of alternating heating devices 61 and cooling devices 62. The heating device 61 is equipped with a coil, and the side wall of the reactor 1 has a jacket 14. The heating device 61 and cooling device 62 are alternately arranged within the jacket 14, enabling precise temperature control during the reaction process. The heating device 61 uses a steam coil wound along the jacket 14, while the cooling device 62 is an array of semiconductor cooling chips embedded in the jacket. The spacing between adjacent cooling chips is consistent with the spacing of the steam coil, ensuring the accuracy and stability of temperature control.

[0029] Please refer to Figures 1-2 To achieve high-purity isopropyl bromide recovery and improve waste acid reuse rate, this embodiment includes a fourth feed port at the top of reactor 1. After the reaction is complete, the product is discharged through the fourth feed port 15 and enters distillation module 7. Distillation module 7 includes a serpentine coil condenser 71 and a separator 72 connected to the inlet of condenser 71. The serpentine coil condenser 71 increases the condensation area and improves condensation efficiency, ensuring efficient recovery of isopropyl bromide.

[0030] As a preferred option, longitudinal fins can be provided on the surface of the coil, with the fin height being 0.2 to 0.3 times the coil diameter. Providing longitudinal fins on the condenser coil can increase the heat dissipation area and improve heat dissipation efficiency. At the same time, the micro-liquid film tearing phenomenon can be used to accelerate the droplet shedding, further improving condensation efficiency.

[0031] The condensing medium first enters the separator 72, then flows evenly to the coil on the condenser 71. The reacted liquid is sprayed out through the nozzle at the top of the distillation module 7, and condenses upon contact with the coil during its descent, before falling into the collection chamber at the bottom, thus separating isopropyl bromide from waste acid. The finished isopropyl bromide product has a purity of over 98% and can be directly used in the production of propyne oxadiazon, resulting in significant economic benefits. Simultaneously, the waste acid, after recycling, has a significantly increased reuse rate, reducing waste acid emissions, lowering treatment costs, and achieving resource recycling.

[0032] Example 3 like Figures 1-2 This illustration depicts an etherified salt slag treatment device according to this application. To achieve ease of operation and applicability to industrial production, this application optimizes the etherified salt slag treatment device. The screw surface of the screw conveyor 2 is coated with tungsten carbide, which improves the wear resistance of the screw conveyor and extends its service life. The inlets of the first feed port 11, the second feed port 12, and the third feed port 13 are all arranged at a 45° downward angle, and the ends of the inlets are equipped with umbrella-shaped dispersion covers 100 to ensure that the material can enter the reaction vessel 1 uniformly and stably, avoiding material splashing and blockage.

[0033] Please refer to Figure 3 The jacket 14 of the reactor 1 is divided into three independent temperature-controlled zones: upper, middle, and lower. Each zone includes at least one heating device 61 and a cooling device 62, enabling precise control of the reaction temperature. The entire process produces almost no secondary pollution, making it suitable for industrial production and capable of meeting the needs of large-scale treatment of etherified salt residue and hydrolyzed waste sulfuric acid.

[0034] The method for comprehensively utilizing the etherified salt residue and hydrolyzed waste sulfuric acid generated from the production of propyne oxadiazon, as described in this invention, comprises the following steps: Add the etherified salt residue, water, and supplementary isopropanol to the reaction flask, stir, and after thorough mixing, cool to below 10°C, control the temperature below 20°C, and add hydrolyzed waste sulfuric acid dropwise. The mass ratio of the etherified salt residue, isopropanol, and hydrolyzed waste sulfuric acid is 1:0.2-0.6:1.5-3.

[0035] After the addition is complete, the mixture is heated to reflux and kept at reflux for 2 to 4 hours. After the reaction is complete, the material is heated to about 100°C and distilled at atmospheric pressure to obtain isopropyl bromide. The resulting fraction contains isopropyl bromide, a small amount of acid water, isopropanol, etc. High-quality isopropyl bromide can be obtained by washing with water.

[0036] In the description of the embodiments of this application, the technical terms "upper", "lower", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the embodiments of this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the embodiments of this application.

[0037] In the description of the embodiments of this application, unless otherwise expressly specified and limited, technical terms such as "set," "equipped with," "connected," and "installed" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a direct connection or an indirect connection through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in the embodiments of this application according to the specific circumstances.

[0038] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. An etherified salt residue treatment device, characterized in that, include: The reactor (1) is provided with a first feed port (11), a second feed port (12) and a third feed port (13) at the top; the side wall of the reactor (1) is provided with a jacket (14); the side wall of the reactor (1) is provided with a fourth feed port (15) that is inclined downward. A screw conveyor (2) connected to the first feed port (11); Isopropanol dripping device (3) connected to the second feed port (12); Waste sulfuric acid dripping device (4) connected to the fourth feed port (15); A stirring device (5) that runs vertically through the top of the reactor (1) and extends to the bottom; The temperature control device (6) arranged in the interlayer (14) includes: a heating device (61) and a cooling device (62) that alternately surround the interlayer (14). The distillation module (7) is connected to the third feed port (13).

2. The etherified salt residue treatment device according to claim 1, characterized in that, The stirring device (5) includes: Top double-layer propulsion stirring paddle (51); The bottom frame stirring paddle (52) has a gap of ≤10mm between its outer edge and the inner wall of the reactor.

3. The etherified salt residue treatment device according to claim 1, characterized in that, The heating device (61) is a steam coil coiled along the interlayer (14); the cooling device (62) is a semiconductor cooling chip array embedded in the interlayer, with the spacing between adjacent cooling chips being the same as the spacing between the steam coils.

4. The etherified salt residue treatment device according to claim 1, characterized in that, The isopropanol dripping device (3) includes: A liquid storage tank with a graduated viewing window (31); A precision peristaltic pump (32) has its outlet connected to a second feed port (12) via a polytetrafluoroethylene hose (33).

5. The etherified salt residue treatment device according to claim 1, characterized in that, The waste sulfuric acid dripping device (4) includes: Corrosion-resistant metering tank (41), lined with polypropylene material; A pneumatic diaphragm pump (42) has its outlet connected to a third feed port (13).

6. The etherified salt residue treatment device according to claim 1, characterized in that, The distillation module (7) includes: a condenser (71) with a serpentine coil structure; and a distributor (72) connected to the inlet of the condenser (71).

7. The etherified salt residue treatment device according to claim 1, characterized in that, The screw surface of the screw conveyor (2) is coated with tungsten carbide.

8. The etherified salt residue treatment apparatus according to claim 1, characterized in that, The jacket (14) of the reactor (1) is divided into three independent temperature control zones: upper, middle and lower. Each zone contains at least one heating device (61) and a cooling device (62).

9. The etherified salt residue treatment device according to claim 1, characterized in that, The openings of the first feed port (11), the second feed port (12) and the third feed port (13) are all arranged at a 45° angle downwards, and the ends of the openings are provided with umbrella-shaped dispersion covers (100).

Images