Production and purification device of 2, 3-dimethyl-2, 3-dinitrobutane

Abstract

The utility model discloses a production and purification device of 2, 3-dimethyl-2, 3-dinitrobutane, which is characterized in that a reaction kettle is connected with a reaction liquid discharging pump, the reaction liquid discharging pump is connected with a reaction liquid storage tank, the reaction liquid storage tank is connected with a solvent separation tower feeding pump, the solvent separation tower feeding pump is connected with a solvent separation tower, the top of the solvent separation tower is connected with a solvent storage tank, and the solvent storage tank is connected with the solvent separation tower. The bottom of the solvent separation tower is connected with a crude product feeding pump, the crude product feeding pump is connected with a three-in-one washing kettle, the three-in-one washing kettle is connected with a water feeding pump, the water feeding pump is connected with a water storage tank, the three-in-one washing kettle is connected with a sewage discharging pump, and the three-in-one washing kettle is connected with a product drying cone. The device is simple in structure, convenient to operate and low in investment. The purity of the 2, 3-dimethyl-2, 3-dinitrobutane product is greater than 99.5%; the number of 2, 3-dimethyl-2, 3-dinitrobutane manufacturers is small, and the market vacancy is made up; the utility model provides an effective production method for the 1, 2, 3-dimethyl-2, 3-dinitrobutane downstream market.

Description

TECHNICAL FIELD

[0001] The utility model relates to the field of chemical industry, concretely relates to 2, 3 -dimethyl -2, 3 -dinitrobutane's production and purification device. BACKGROUND

[0002] 2, 3 -dimethyl -2, 3 -dinitrobutane (abbreviated as DMNB) is an important organic intermediate, and it is widely used, such as can replace nitrotoluene and be used as explosive tracer. DMNB is also one of the key raw materials for synthesizing 2-substituted-1, 3-dioxane-4, 4, 5, 5-tetramethyl imidazoline substance, and the substance has specific capture performance to NO, has important application in medicine, and is also one of the important raw materials for synthesizing new material molecular magnet and various nitrogen oxygen free radicals.

[0003] At present, the market of 2, 3 -dimethyl -2, 3 -dinitrobutane as explosive tracer is mainly in foreign countries, compared with foreign countries, the research of DMNB in China starts late, and the domestic demand is small.

[0004] At present, the synthesis method of 2, 3 -dimethyl -2, 3 -dinitrobutane is few in domestic data, and most of foreign data are old, and the production and extraction method of novel 2, 3 -dimethyl -2, 3 -dinitrobutane is complex, and the yield is low, so it is necessary to develop a set of 2, 3 -dimethyl -2, 3 -dinitrobutane extraction device. Utility model content

[0005] In view of the above-mentioned defects or deficiencies in the prior art, it is expected to provide a 2, 3 -dimethyl -2, 3 -dinitrobutane production and purification device.

[0006] According to the technical scheme provided in the embodiment of the application, the production and purification device of 2,3-dimethyl-2,3-dinitrobutane comprises a reaction kettle, a feed inlet of a reaction liquid discharge pump at one end is connected with a discharge port of the reaction kettle through a pipeline, a feed inlet of a solvent separation tower at an upper end side of a reaction liquid storage tank is connected with a discharge port of the reaction liquid discharge pump through a pipeline, a feed inlet of a solvent separation tower feed pump is connected with a discharge port of the reaction liquid storage tank at the bottom through a pipeline, a feed inlet of a solvent storage tank at a side of the solvent separation tower at the top is connected with a discharge port a of the solvent separation tower at the top through a pipeline, a discharge port b of the solvent separation tower at the bottom is connected with a crude product feed pump through a pipeline, the crude product feed pump is connected with a feed inlet a of a three-in-one water washing kettle at a side through a pipeline, a feed inlet b of the three-in-one water washing kettle is connected with a discharge port of a water feed pump through a pipeline, a water inlet of the water feed pump is connected with a water outlet of a water storage tank through a pipeline, a discharge port of the three-in-one water washing kettle is connected with a sewage discharge pump through a pipeline, and the three-in-one water washing kettle at the bottom is fixedly connected with a product drying cone at the top.

[0007] In the utility model, the reaction kettle is equipped with a feeding device and a stirring device, and the reaction kettle is wrapped with a jacket.

[0008] In the utility model, the three-in-one water washing kettle is equipped with a scraping plate, a solid outlet at the bottom of the three-in-one water washing kettle and a centrifugal device in the three-in-one water washing kettle.

[0009] In the utility model, the two return inlets at the lower end of the solvent separation tower are connected with a reboiler through a return pipeline.

[0010] In conclusion, the device has the advantages of simple structure, convenient operation and low investment, the purity of 2,3-dimethyl-2,3-dinitrobutane is greater than 99.5%, the device makes up the market vacancy, and provides an effective production method for the downstream market of 2,3-dimethyl-2,3-dinitrobutane. BRIEF DESCRIPTION OF DRAWINGS

[0011] Other features, objects and advantages of the application will become more apparent from the following detailed description of non-restrictive embodiments made with reference to the accompanying drawings:

[0012] Figure 1 It is a structural schematic view of the production and purification device.

[0013] Reference numerals in the drawings:

[0014] 1-Reaction vessel; 2-Solvent separation tower; 3-Three-in-one water washing vessel; 4-Product drying cone; 5-Reaction liquid storage tank; 6-Water storage tank; 7-Solvent storage tank; 8-Distillation tower condenser; 9-Distillation tower reboiler; 10-Reflux pump; 11-Reaction liquid discharge pump; 12-Solvent separation tower feed pump; 13-Crude product feed pump; 14-Water feed pump; 15-Wastewater discharge pump. Detailed Implementation

[0015] The present application will now be described in further detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the relevant utility model and not intended to limit the scope of the utility model. Furthermore, it should be noted that, for ease of description, only the parts relevant to the utility model are shown in the accompanying drawings.

[0016] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. This application will now be described in detail with reference to the accompanying drawings and embodiments.

[0017] like Figure 1 As shown, the production and purification apparatus for 2,3-dimethyl-2,3-dinitrobutane of this application consists of a reaction vessel 1, a solvent separation tower 2, a three-in-one water washing vessel 3, a product drying cone 4, a reaction liquid storage tank 5, a water storage tank 6, a solvent storage tank 7, a distillation column condenser 8, a distillation column reboiler 9, a reflux pump 10, a reaction liquid discharge pump 11, a solvent separation tower feed pump 12, a crude product feed pump 13, a water feed pump 14, and a wastewater discharge pump 15.

[0018] like Figure 1 As shown, the outlet of reactor 1 is connected to reaction liquid discharge pump 11 via a pipe. Reaction liquid discharge pump 11 is connected to the inlet of reaction liquid storage tank 5 via a pipe. The outlet of reaction liquid storage tank 5 is connected to solvent separation tower feed pump 12 via a pipe. Solvent separation tower feed pump 12 is connected to the inlet of solvent separation tower 2 via a pipe. The outlet a at the top of solvent separation tower 2 is connected to the side of solvent storage tank 7 via a pipe. The outlet b of solvent separation tower 2 is connected to crude product feed pump 13 via a pipe. Crude product feed pump 13 is connected to inlet a of three-in-one water washing reactor 3 via a pipe. The inlet b of three-in-one water washing reactor 3 is connected to water feed pump 14 via a pipe. Water feed pump 14 is connected to water storage tank 6 via a pipe. The outlet of three-in-one water washing reactor 3 is connected to wastewater discharge pump 15 via a pipe. The bottom of three-in-one water washing reactor 3 is fixedly connected to the top of product drying cone 4.

[0019] like Figure 1 As shown, reactor 1 is equipped with a feeding device for feeding raw materials; reactor 1 is equipped with a stirring device for mixing materials; reactor 1 is equipped with a jacket for heating the reactor.

[0020] likeFigure 1 As shown, the three-in-one washing kettle 3 is provided with a filtering device, which can filter liquid. The filtering device is distributed around the three-in-one washing kettle 3. During the filtering process, solids are adsorbed around the three-in-one washing kettle 3. Liquid flows out of the interlayer of the three-in-one washing kettle 3. The three-in-one washing kettle 3 is provided with a scraper, which can scrape the solids around the three-in-one washing kettle 3 into the solid outlet. The three-in-one washing kettle 3 is provided with a solid outlet at the bottom, through which solid products can be discharged. The three-in-one washing kettle 3 is provided with a centrifugal device, which can be used for solid-liquid separation of materials. The solvent separation tower 2 is provided with a reboiler 9 at the bottom, which can be used for heating materials.

[0021] Specific production process: 2,3-dimethyl-2,3-dinitrobutane is generated in the reaction kettle 1. The reaction kettle 1 is provided with a feeding device, a stirring device, a heating device and a filtering device. Then, the solid-liquid mixture containing 2,3-dimethyl-2,3-dinitrobutane enters the bottom of the solvent separation tower 2. The solvent separation tower 2 is provided with a reboiler 9 for heating. The heating temperature is set to 90°C. The obtained solvent is reused. The tower kettle liquid enters the three-in-one washing kettle 3 through the crude product feeding pump 13. The liquid is washed to obtain the product, which enters the product drying cone 4. The washing liquid enters the sewage treatment workshop through the sewage discharge pump 15.

[0022] The above description is only the preferred embodiment of the present application and the description of the technical principles and schemes used. Meanwhile, the utility model range involved in the present application is not limited to the technical solutions formed by the specific combination of the above technical features. Meanwhile, it should also cover other technical solutions formed by the combination of the above technical features or equivalent features without departing from the utility model concept. For example, the above features and the technical features disclosed in the present application (but not limited to) with similar functions are replaced with each other to form technical solutions.

Claims

A production and purification apparatus for 1,2,3-dimethyl-2,3-dinitrobutane, comprising a reaction vessel (1), characterized in that: The bottom outlet of the reactor (1) is connected to the inlet of one end of the reaction liquid discharge pump (11) via a pipe. The outlet of the reaction liquid discharge pump (11) is connected to the inlet on the upper side of the reaction liquid storage tank (5) via a pipe. The bottom outlet of the reaction liquid storage tank (5) is connected to the inlet of the solvent separation tower feed pump (12) via a pipe. The outlet of the solvent separation tower feed pump (12) is connected to the bottom inlet of the solvent separation tower (2) via a pipe. The top outlet a of the solvent separation tower (2) is connected to the inlet on the side of the solvent storage tank (7) via a pipe. The outlet b at the bottom of the solvent separation tower (2) is connected to the crude product feed pump (13) through a pipe. The crude product feed pump (13) is connected to the inlet a on the side of the three-in-one water washing tank (3) through a pipe. The inlet b of the three-in-one water washing tank (3) is connected to the outlet of the water feed pump (14) through a pipe. The inlet of the water feed pump (14) is connected to the outlet of the water storage tank (6) through a pipe. The outlet of the three-in-one water washing tank (3) is connected to the sewage discharge pump (15) through a pipe. The bottom of the three-in-one water washing tank (3) is fixedly connected to the top of the product drying cone (4).

2. The apparatus for producing and purifying 2,3-dimethyl-2,3-dinitrobutane according to claim 1, characterized in that: The reactor (1) is equipped with a feeding device and a stirring device, and the reactor (1) is covered with a jacket.

3. The apparatus for producing and purifying 2,3-dimethyl-2,3-dinitrobutane according to claim 1, characterized in that: The three-in-one washing kettle (3) is equipped with a filter device around its perimeter. During the filtration process, solids are adsorbed onto the inner perimeter of the filter device, and liquid flows out from the jacket of the three-in-one washing kettle (3). The three-in-one washing kettle (3) is equipped with a scraper, and the bottom of the three-in-one washing kettle (3) is equipped with a solid outlet. The three-in-one washing kettle (3) is equipped with a centrifugal device inside its interior.

4. The apparatus for producing and purifying 2,3-dimethyl-2,3-dinitrobutane according to claim 1, characterized in that: The two return ports at the lower end of the solvent separation tower (2) are connected to the reboiler (9) through a loop pipe.

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