2, 3-dimethyl-2, 3-dinitrobutane recovery and extraction device

Abstract

The utility model discloses a 2, 3-dimethyl-2, 3-dinitrobutane recovery and extraction device which comprises a raw material tank, a filter, a post-treatment tower, a rectifying tower, a centrifugal machine, a crystallization kettle, a double-cone drying machine, a condenser, an extraction agent storage tank and the like, after raw materials are filtered, most of the 2, 3-dimethyl-2, 3-dinitrobutane is filtered, then the 2, 3-dimethyl-2, 3-dinitrobutane is extracted with ethyl acetate, the filtered raw materials enter a post-treatment tower, the ethyl acetate and the 2, 3-dimethyl-2, 3-dinitrobutane enter a rectifying tower to be separated, tower bottoms enter a crystallization kettle, and the 2, 3-dimethyl-2, 3-dinitrobutane enters the crystallization kettle to be crystallized. 3, 3-dinitrobutane is separated out from liquid after being condensed, solid and liquid are separated through a centrifugal machine, a solid product enters a double-cone drying machine, an extracting agent enters a rectifying tower for secondary rectification again, and a finished product is obtained after drying. The device is simple in structure, convenient to operate and low in investment, the filtering device can be prevented from being blocked, and meanwhile, 2, 3-dimethyl-2, 3-dinitrobutane can be recycled.

Description

Technical Field

[0001] The utility model relates to the field of 2,3-dimethyl-2,3-dinitrobutane recovery and extraction, and in particular to a 2,3-dimethyl-2,3-dinitrobutane recovery and extraction device. Background Art

[0002] 2,3-Dimethyl-2,3-dinitrobutane (DMNB) is an important organic intermediate with a wide range of applications. For example, it can be used as a tracer for explosives, replacing nitrotoluene. DMNB is also a key raw material in the synthesis of 2-substituted-1,3-dioxo-4,4,5,5-tetramethylimidazolines. This substance has specific NO capture properties and holds important medical applications. It is also a key raw material for various nitroxide free radicals, the main building blocks of novel molecular magnets. However, because DMNB is virtually insoluble in solvents such as water, methanol, and ethanol, it accumulates on the inner walls of filters and pipes in industrial production equipment. Prolonged operation increases resistance and poses a significant safety hazard. Currently, the standard treatment involves installing a filter in the reaction solution outlet pipe. However, this often clogs the filter over time, necessitating frequent disassembly and cleaning. Therefore, a non-disassembly cleaning device is needed. Utility Model Content

[0003] In view of the above-mentioned defects or deficiencies in the prior art, it is desired to provide a 2,3-dimethyl-2,3-dinitrobutane recovery and extraction device.

[0004] According to the technical solution provided in the embodiments of this application,

[0005] A 2,3-dimethyl-2,3-dinitrobutane recovery and extraction device, wherein a raw material tank is connected to a raw material discharge pump by a pipeline, the raw material tank is connected to a filter through the raw material discharge pump and a raw material feed valve, the right end of the filter is connected to a post-processing tower through the raw material discharge valve UI, the lower end of the filter is connected to a buffer tank through an extractant and 2,3-dimethyl-2,3-dinitrobutane mixture discharge valve and a 2,3-dimethyl-2,3-dinitrobutane discharge pump, and a nitrogen pipe network is connected to the filter through a nitrogen valve, an extractant valve, and a nitrogen and extractant main valve. The buffer tank is connected to the distillation tower through a 2,3-dimethyl-2,3-dinitrobutane feed pump, the condenser and the reboiler are respectively arranged at the upper and lower parts of the distillation tower, the crystallization kettle is connected to the bottom of the distillation tower through a 2,3-dimethyl-2,3-dinitrobutane mixture discharge pump, an agitator is arranged at the upper part of the crystallization kettle, a centrifuge is arranged below the crystallization kettle, the centrifuge is connected to the distillation tower through a centrifugal extractant pump, the condenser is connected to the extractant storage tank through an extractant recovery pump, and the extractant storage tank is connected to the filter through the extractant discharge pump.

[0006] Furthermore, the extractant storage tank is filled with ethyl acetate, and the 2,3-dimethyl-2,3-dinitrobutane attached to the filter is extracted by utilizing the principle that ethyl acetate is miscible with 2,3-dimethyl-2,3-dinitrobutane but not miscible with water.

[0007] Furthermore, a condenser is installed on the distillation tower, which can condense the extractant for easy collection and secondary utilization. The extractant after centrifugation is returned to the distillation tower through a centrifugal extractant pump.

[0008] Furthermore, the double-cone dryer is installed below the centrifuge so that the 2,3-dimethyl-2,3-dinitrobutane can directly enter the double-cone dryer.

[0009] Furthermore, the centrifuge is connected to the distillation tower via a centrifugal extractant pump.

[0010] Furthermore, the top of the distillation tower is connected to the extractant storage tank via a condenser and an extractant recovery pump.

[0011] In summary, the beneficial effects of this application are:

[0012] (1) After the raw materials are filtered, most of the 2,3-dimethyl-2,3-dinitrobutane is filtered out, and then ethyl acetate is used to extract 2,3-dimethyl-2,3-dinitrobutane. The filtered raw materials enter the post-treatment tower, and ethyl acetate and 2,3-dimethyl-2,3-dinitrobutane enter the distillation tower for separation. The bottom liquid enters the crystallization kettle, and 2,3-dimethyl-2,3-dinitrobutane is precipitated from the liquid after condensation. The solid and liquid are separated by a centrifuge, and the solid product enters a double-cone dryer. The extractant enters the distillation tower for secondary distillation. The device has a simple structure, is easy to operate, and requires little investment. It can prevent the filter device from being blocked and recover 2,3-dimethyl-2,3-dinitrobutane at the same time. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Other features, objects and advantages of the present application will become more apparent upon reading the detailed description of non-limiting embodiments made with reference to the following drawings:

[0014] Figure 1 This is a schematic diagram of the structure of the utility model.

[0015] Numbers in the figure: raw material tank-1, raw material discharge pump-2, raw material feed valve-3, filter-4, raw material discharge valve-5, nitrogen and extractant main valve-6, extractant and 2,3-dimethyl-2,3-dinitrobutane mixture discharge valve-7, post-treatment tower-8, 2,3-dimethyl-2,3-dinitrobutane discharge pump-9, buffer tank-10, 2,3-dimethyl-2,3-dinitrobutane feed pump-11, Distillation tower 12, centrifugal extractant pump 13, centrifuge 14, extractant and 2,3-dimethyl-2,3-dinitrobutane mixture discharge pump 15, crystallization kettle 16, double-cone dryer 17, agitator 18, reboiler 19, condenser 20, extractant recovery pump 21, extractant storage tank 22, extractant discharge pump 23, extractant valve 24, nitrogen valve 25, nitrogen pipeline network 26. DETAILED DESCRIPTION

[0016] The present application will be further described in detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely for the purpose of explaining the relevant utility model and are not intended to limit the utility model. It should also be noted that, for ease of description, only the portions relevant to the utility model are shown in the accompanying drawings.

[0017] It should be noted that, in the absence of conflict, the embodiments and features of the embodiments in this application can be combined with each other. The present application will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0018] Example:

[0019] like Figure 1As shown, the raw material is poured from the raw material tank 1 into the filter 4 through the raw material discharge pump 2. At this time, the raw material feed valve 3 and the raw material discharge valve 5 are opened, and the rest are closed. After being processed by the filter 4, the raw material discharge valve 5 is opened, and the raw material enters the post-processing tower 8. 2,3-dimethyl-2,3-dinitrobutane is attached to the filter 4. The nitrogen valve 25, the raw material feed valve 3, the raw material discharge valve 5 and the extractant and 2,3-dimethyl-2,3-dinitrobutane mixture discharge valve 7 are closed. The extractant valve 24 and the nitrogen valve 26 are opened. The extractant enters filter 4, where ethyl acetate is mixed with 2,3-dimethyl-2,3-dinitrobutane. Nitrogen valve 25, nitrogen, extractant main valve 6, and extractant / 2,3-dinitrobutane mixture discharge valve 7 are opened, while all other valves are closed. The mixture enters distillation tower 12 via 2,3-dimethyl-2,3-dinitrobutane feed pump 11, where nitrogen cleans the remaining mixture. After separation in distillation tower 12, ethyl acetate is evaporated from the top of the tower. It is recovered via condenser 20 and returned to extractant storage tank 22. The bottom liquid enters crystallizer 16, where it is cooled and treated by agitator 18, resulting in solid precipitation. The solid and liquid enter centrifuge 14, where they are centrifuged. The ethyl acetate liquid then re-enters distillation tower 12 via centrifugal extractant pump 13, while the 2,3-dimethyl-2,3-dinitrobutane solid enters double-cone dryer 17 for drying to yield the finished product.

[0020] The above description is merely an illustration of the preferred embodiments of this application and the technical principles employed. Furthermore, the scope of the utility model disclosed in this application is not limited to technical solutions formed by specific combinations of the aforementioned technical features. It also encompasses other technical solutions formed by any combination of the aforementioned technical features or their equivalents, without departing from the concept of the utility model. For example, a technical solution formed by replacing the aforementioned features with (but not limited to) technical features with similar functions disclosed in this application.

Claims

1. A 2,3-dimethyl-2,3-dinitrobutane recovery and extraction device, comprising a raw material tank (1), a raw material discharge pump (2), a raw material feed valve (3), a filter (4), a raw material discharge valve (5), a nitrogen and extractant main valve (6), a discharge valve for a mixture of extractant and 2,3-dimethyl-2,3-dinitrobutane (7), a post-treatment tower (8), a 2,3-dimethyl-2,3-dinitrobutane discharge pump (9), a buffer tank (10), a 2,3-dimethyl-2,3-dinitrobutane A feed pump (11), a distillation tower (12), a centrifugal extractant pump (13), a centrifuge (14), a discharge pump (15) for a mixture of extractant and 2,3-dimethyl-2,3-dinitrobutane, a crystallization kettle (16), a double-cone dryer (17), an agitator (18), a reboiler (19), a condenser (20), an extractant recovery pump (21), an extractant storage tank (22), an extractant discharge pump (23), an extractant valve (24), a nitrogen valve (25) and a nitrogen pipe network (26), characterized by: The raw material tank (1) is connected to the raw material discharge pump (2) by a pipeline. The raw material tank (1) is connected to the filter (4) through the raw material discharge pump (2) and the raw material feed valve (3). The right end of the filter (4) is connected to the UI post-treatment tower (8) through the raw material discharge valve (5). The lower end of the filter (4) is connected to the buffer tank (10) through the extractant and 2,3-dimethyl-2,3-dinitrobutane mixture discharge valve (7) and the 2,3-dimethyl-2,3-dinitrobutane discharge pump (9). The nitrogen pipe network (26) is connected to the filter (4) through the nitrogen valve (25), the extractant valve (24) and the nitrogen and extractant main valve (6). The buffer tank (10) is connected to the extractant and 2,3-dimethyl-2,3-dinitrobutane mixture discharge valve (7) and the 2,3-dimethyl-2,3-dinitrobutane mixture discharge pump (9). A butane feed pump (11) is connected to a distillation tower (12); the condenser (20) and the reboiler (19) are respectively arranged at the upper and lower parts of the distillation tower (12); the crystallization kettle (16) is connected to the bottom of the distillation tower (12) via a 2,3-dimethyl-2,3-dinitrobutane mixture discharge pump (15); an agitator (18) is arranged at the upper part of the crystallization kettle (16); the centrifuge (14) is arranged below the crystallization kettle (16); the centrifuge (14) is connected to the distillation tower (12) via a centrifugal extractant pump (13); the condenser (20) is connected to an extractant storage tank (22) via an extractant recovery pump (21); and the extractant storage tank (22) is connected to a filter (4) via an extractant discharge pump (23).

2. A 2,3-dimethyl-2,3-dinitrobutane recovery and extraction device according to claim 1, characterized in that: The condenser (20) is installed above the distillation tower (12).

3. A 2,3-dimethyl-2,3-dinitrobutane recovery and extraction device according to claim 1, characterized in that: The double-cone dryer (17) is installed below the centrifuge (14).

4. A 2,3-dimethyl-2,3-dinitrobutane recovery and extraction device according to claim 1, characterized in that: The centrifuge (14) is connected to the distillation tower (12) via a centrifugal extractant pump (13).

5. A 2,3-dimethyl-2,3-dinitrobutane recovery and extraction device according to claim 1, characterized in that: The top of the distillation tower (12) is connected to the extractant storage tank (22) via a condenser (20) and an extractant recovery pump (21).

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