Continuous post-treatment system for nitrate-containing synthetic liquid

Abstract

The utility model belongs to the technical field of chemical synthesis equipment, and particularly relates to a continuous post-treatment system for nitrate-containing synthetic liquid, which is characterized in that the continuous post-treatment system is of a vertical structure, a three-layer frame structure is arranged in a vertical shell, and a first water washing module, an alkali washing module and a second water washing module are sequentially arranged from top to bottom; a first PH meter is arranged on a pipeline where a heavy phase outlet is located, and the first PH meter, a feeding pump and a first washing water pump are in interlocking control. In the alkali washing module, a pipeline where a heavy phase outlet is located is provided with a PH meter II, a pipeline where a heavy phase inlet is located is provided with a regulating valve I, and the PH meter II is in interlocking control with an alkali washing pump and the regulating valve I; in the second washing module, a third PH meter is arranged on a pipeline where a heavy phase outlet is located, a second adjusting valve is arranged on a pipeline where a heavy phase inlet is located, and the third PH meter, the second washing pump and the second adjusting valve are in interlocking control. The utility model has the advantages that: the vertical structure is adopted, and liquid flows among the units flow by gravity, so that the energy consumption is reduced, and the process is ensured to be orderly and smooth.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical synthesis equipment, and particularly relates to a continuous post-treatment system for a synthetic solution containing nitrate ester. Background Art

[0002] Nitrate ester plasticizers are the most commonly used energetic plasticizers in solid propellant and gun propellant formulations. As a classic nitrate ester plasticizer, nitroglycerin (NG) has a mature production process, extremely low cost, and excellent performance. It has characteristics such as high energy, high density, and high oxygen balance, and has been widely used in various explosives, propellants, and gun propellants for nearly a century. However, nitroglycerin has disadvantages such as high sensitivity, strong volatility, high melting point, and easy migration. To solve this problem, a variety of nitrate ester energetic plasticizers have been developed and applied successively, such as EGDN, TEGDN, BTTN, TMETN, DEGDN, etc. It can be foreseen that nitrate ester energetic plasticizers will still be one of the most widely used energetic plasticizers in the future for a long time due to their excellent performance, mature process, and low cost.

[0003] After the nitration reaction is quenched by water, the material contains not only the nitrate ester-containing product generated by the reaction, but also some unreacted raw material components. It is necessary to wash off the excess acid and the salt generated by alkali neutralization through water washing - alkali washing - water washing. According to the conventional kettle washing method, a large amount of water (or alkali solution) needs to be added repeatedly for washing and stirring, and then liquid separation. The amount of waste liquid is large; moreover, the density of nitrate ester compounds is generally greater than that of water, and each time washing and liquid separation are required, the nitrate ester product needs to be poured into another kettle, resulting in low production efficiency and high labor intensity.

[0004] The Chinese utility model patent with the application number 201010540280.7 discloses a continuous and rapid post-treatment method for n-butyl-2-nitroethyl nitramine, in which a cylindrical centrifugal extractor is used for water washing and alkali washing of n-butyl-2-nitroethyl nitramine to achieve the extraction of n-butyl-2-nitroethyl nitramine; the treatment process of this scheme is: first, the optimal rotation speed of the drum is determined by combining the physical properties of n-butyl-2-nitroethyl nitramine with ice water experiments and the hydraulic characteristics of the cylindrical centrifugal extractor; then, single-stage normal temperature water washing and single-stage normal temperature alkali washing experiments of the cylindrical centrifugal extractor are carried out respectively to determine the optimal conditions (the proportion of each feed amount) of water washing and alkali washing. Finally, the number of stages of water washing and alkali washing is determined through the water washing and alkali washing effects (purity comparison value) of the n-butyl-2-nitroethyl nitramine system, and the purpose of continuous post-treatment is finally achieved. The disadvantage of this scheme is poor process flexibility. The number of treatment stages is greatly affected by the composition of the initial material. When production fluctuates, the process parameters cannot be changed in time, which will inevitably affect the quality of the final product. Summary of the Utility Model

[0005] The purpose of the present utility model is to provide a continuous post-treatment system for a nitrate ester synthesis solution, overcoming the deficiencies of the prior art. Using the pH index as the control index for the post-treatment process of the nitrate ester synthesis solution, and cooperating with multiple annular centrifugal extractors to form a multi-stage series system to complete the continuous water washing - alkali washing - water washing process. An on-line pH meter is used for interlocking control with the feed pump and valves to monitor the washing - separation effect in real time, and to achieve rapid, efficient, automatic and continuous extraction of the reaction product.

[0006] To achieve the above purpose, the present utility model is realized through the following technical solutions:

[0007] A continuous post-treatment system for a nitrate ester synthesis solution, characterized in that it has a vertical structure. There is a three-layer frame structure inside the vertical shell. The first water washing module, the alkali washing module, and the second water washing module are arranged layer by layer from top to bottom. The vertical shell is provided with a first washing water pipeline, a first waste water pipeline, an alkali washing pipeline, a waste alkali pipeline, a second washing water pipeline, a second waste water pipeline, and a synthesis solution pipeline. The light phase inlet in the first water washing module is connected to the first washing water pipeline, the light phase outlet is connected to the first waste water pipeline, the heavy phase inlet is connected to the synthesis solution pipeline, and the heavy phase outlet is connected to the heavy phase inlet in the alkali washing module. The light phase inlet in the alkali washing module is connected to the alkali washing pipeline, the light phase outlet is connected to the waste alkali pipeline, the heavy phase inlet is connected to the heavy phase outlet in the first water washing module, and the heavy phase outlet is connected to the heavy phase inlet in the second water washing module. The light phase inlet in the second water washing module is connected to the second washing water pipeline, the light phase outlet is connected to the second waste water pipeline, the heavy phase inlet is connected to the heavy phase outlet in the alkali washing module, and the heavy phase outlet is connected to the product tank through a finished product pipeline. A feed pump is provided on the synthesis solution pipeline, a first washing water pump is provided on the first washing water pipeline, an alkali washing pump is provided on the alkali washing pipeline, and a second washing water pump is provided on the second washing water pipeline. In the first water washing module, a pH meter 1 is provided on the pipeline where the heavy phase outlet is located, and the pH meter 1 is interlocked with the feed pump and the first washing water pump for control. In the alkali washing module, a pH meter 2 is provided on the pipeline where the heavy phase outlet is located, and a first regulating valve is provided on the pipeline where the heavy phase inlet is located. The pH meter 2 is interlocked with the alkali washing pump and the first regulating valve for control. In the second water washing module, a pH meter 3 is provided on the pipeline where the heavy phase outlet is located, and a second regulating valve is provided on the pipeline where the heavy phase inlet is located. The pH meter 3 is interlocked with the second washing water pump and the second regulating valve for control.

[0008] Further, the main machines in the first water washing module, the alkali washing module, and the second water washing module are all annular centrifugal extractors with the same specifications.

[0009] Further, a flow meter and a differential pressure transmitter are provided on the feed side pipeline of any one of the feed pump, the first washing water pump, the alkali washing pump, and the second washing water pump.

[0010] Further, a check valve and a blowdown valve are provided on the discharge side pipeline of any one of the feed pump, the first washing water pump, the alkali washing pump, and the second washing water pump.

[0011] Further, a maintenance hole is provided on the side wall of the vertical shell; a lifting lug plate is provided at the top of the vertical shell.

[0012] Further, the pH meter one, pH meter two, and pH meter three are all industrial analysis integrated pH meters with a 4-20 mA signal remote transmission interface.

[0013] Further, the feed pump is any one of a diaphragm pump, a peristaltic pump, a viscose solution delivery pump, and a twin-screw pump.

[0014] Compared with the prior art, the beneficial effects of the present utility model are as follows:

[0015] 1) The vertical drop structure enables the liquid flow between units to rely on gravity, which helps reduce energy consumption, ensures the orderly progress of the process, uses a remote transmission pH meter as the benchmark for process adjustment, realizes the automatic adjustment of the flow rates of the primary water, caustic solution, and secondary water for washing, has strong continuity in the treatment process, low labor intensity, and realizes the rapid, efficient, and automatic extraction of the product after the reaction;

[0016] 2) It can real-time monitor parameters such as the pH value, conductivity, and moisture content at the outlets of each module according to the flow rate of the reaction liquid. It can not only reduce the usage of water and caustic solution, reduce the production of waste liquid, but also reduce the moisture content in the material after water washing, reduce the load of the subsequent drying system, improve production efficiency, and has a high degree of automation. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 is a schematic diagram of the external structure of an embodiment of the present utility model;

[0018] Figure 2 is a schematic diagram of the internal structure of an embodiment of the present utility model.

[0019] In the figure: 1 - first water washing module, 2 - caustic washing module, 3 - second water washing module, 4 - first waste water pipeline, 5 - first water washing pipeline, 6 - caustic washing pipeline, 7 - synthesis liquid pipeline, 8 - waste caustic pipeline, 9 - second water washing pipeline, 10 - second waste water pipeline, 11 - product tank, 12 - feed pump, 13 - first water washing pump, 14 - caustic washing pump, 15 - second water washing pump, 16 - pH meter one, 17 - pH meter two, 18 - first regulating valve, 19 - pH meter three, 20 - second regulating valve, 21 - finished product pipeline, 22 - lifting lug plate, 23 - vertical shell, 24 - maintenance hole. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0020] The technical solutions of the present utility model will be clearly and completely described below in conjunction with specific embodiments. Obviously, the described embodiments are some, but not all, of the embodiments of the present utility model.

[0021] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the specific examples required for the description of the specific embodiments or the prior art. Obviously, the specific examples described below are some embodiments of the present invention. For those of ordinary skill in the art, without creative work, other specific examples can be obtained based on these specific examples.

[0022] Generally, the components of the embodiments of the present invention described and shown in the specific examples here can be arranged and designed in countless different configurations. Therefore, the following detailed description of the embodiments of the present invention provided in the specific examples is not intended to limit the scope of the present invention claimed, but merely represents the selected embodiments of the present invention.

[0023] See Figure 1-2 , which is a schematic structural diagram of an embodiment of a continuous post-treatment system for a nitric ester synthesis solution of the present invention. It is a vertical structure. There are three-layer frame structures in the vertical shell. The first water washing module 1, the alkali washing module 2, and the second water washing module 3 are arranged layer by layer from top to bottom. There are a first washing water pipeline 5, a first waste water pipeline 4, an alkali washing pipeline 6, a waste alkali pipeline 8, a second washing water pipeline 9, a second waste water pipeline 10, and a synthesis solution pipeline 7 on the vertical shell; the light phase inlet in the first water washing module 1 is connected to the first washing water pipeline 5, the light phase outlet is connected to the first waste water pipeline 4, the heavy phase inlet is connected to the synthesis solution pipeline 7, and the heavy phase outlet is connected to the heavy phase inlet in the alkali washing module 2; the light phase inlet in the alkali washing module 2 is connected to the alkali washing pipeline 6, the light phase outlet is connected to the waste alkali pipeline 8, the heavy phase inlet is connected to the heavy phase outlet in the first water washing module 1, and the heavy phase outlet is connected to the heavy phase inlet in the second water washing module 3; the light phase inlet in the second water washing module 3 is connected to the second washing water pipeline 9, the light phase outlet is connected to the second waste water pipeline 10, the heavy phase inlet is connected to the heavy phase outlet in the alkali washing module 2, and the heavy phase outlet is connected to the product tank 11 through the finished product pipeline 21; there is a feed pump on the synthesis solution pipeline 7, a first washing water pump 13 on the first washing water pipeline 5, an alkali washing pump 14 on the alkali washing pipeline 6, and a second washing water pump 15 on the second washing water pipeline 9.

[0024] The main machines in the first water washing module 1, the alkali washing module 2, and the second water washing module 3 are all annular-gap centrifugal extractors of the same specification. A flow meter and a differential pressure transmitter are provided on the feed side pipeline of any one of the feed pump 12, the first washing water pump 13, the alkali washing pump 14, and the second washing water pump 15. The controller adjusts the flow rate and pressure in each pipeline according to the data of each pH meter to make the feed of each module meet the proportional requirements. A check valve and a blowdown valve are provided on the discharge side pipeline of any one of the feed pump 12, the first washing water pump 13, the alkali washing pump 14, and the second washing water pump 15 to drain the remaining material in the pipeline during shutdown.

[0025] In the first water washing module 1, a pH meter 16 is provided on the pipeline where the heavy phase outlet is located, and the pH meter 16 is interlocked with the feed pump 12 and the first water washing pump 13; in the caustic washing module 2, a pH meter 17 is provided on the pipeline where the heavy phase outlet is located, and a first regulating valve 18 is provided on the pipeline where the heavy phase inlet is located. The pH meter 17 is interlocked with the caustic washing pump 14 and the first regulating valve 18; in the second water washing module 3, a pH meter 19 is provided on the pipeline where the heavy phase outlet is located, and a second regulating valve 20 is provided on the pipeline where the heavy phase inlet is located. The pH meter 19 is interlocked with the second water washing pump 15 and the second regulating valve 20.

[0026] An inspection hole 24 is provided on the side wall of the vertical shell 23 for convenient inspection and maintenance; a lifting ear plate 22 is provided at the top of the vertical shell, and when needed, the whole system can be removed, which is convenient to use.

[0027] In the embodiment, the pH meter 16, the pH meter 17, and the pH meter 19 are all industrial analysis integrated pH meters with a 4-20 mA signal remote transmission interface, which can be remotely monitored in the central control room to improve the automation level.

[0028] Since the viscosity of the synthetic liquid containing nitrate ester is relatively large, the feed pump 12 is selected from any one of a diaphragm pump, a peristaltic pump, a viscose liquid transfer pump, and a twin-screw pump to meet the process requirements.

[0029] Although the embodiments of the present invention have been shown and described, those of ordinary skill in the art can understand that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principle and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A continuous post-treatment system for a nitrate ester synthetic liquid, characterized in that: It is a vertical structure, and a three-layer frame structure is arranged in the vertical shell. The water washing module 1, the alkali washing module and the water washing module 2 are arranged in layers from top to bottom. The vertical shell is provided with a washing water pipeline 1, a waste water pipeline 1, an alkali washing pipeline, a waste alkali pipeline, a washing water pipeline 2, a waste water pipeline 2 and a synthetic liquid pipeline; The light phase inlet of the water washing module 1 is connected to the washing water pipeline 1, the light phase outlet is connected to the waste water pipeline 1, the heavy phase inlet is connected to the synthetic liquid pipeline, and the heavy phase outlet is connected to the heavy phase inlet of the alkali washing module; The light phase inlet of the alkali washing module is connected to the alkali washing pipeline, the light phase outlet is connected to the waste alkali pipeline, the heavy phase inlet is connected to the heavy phase outlet of the water washing module 1, and the heavy phase outlet is connected to the heavy phase inlet of the water washing module 2; The light phase inlet in the second water washing module is connected to the second washing water pipeline, the light phase outlet is connected to the second waste water pipeline, the heavy phase inlet is connected to the heavy phase outlet in the alkali washing module, and the heavy phase outlet is connected to the product tank through the finished product pipeline; The synthetic liquid pipeline is provided with a feed pump, the first wash water pipeline is provided with a wash water pump 1, the alkali wash pipeline is provided with an alkali wash pump, and the second wash water pipeline is provided with a wash water pump 2; In the water washing module 1, a pH meter 1 is provided on the pipeline where the heavy phase outlet is located, and the pH meter 1 is interlocked with the feed pump and the washing water pump 1; In the alkali washing module, a second pH meter is provided on the pipeline where the heavy phase outlet is located, and a regulating valve is provided on the pipeline where the heavy phase inlet is located. The second pH meter is interlocked with the alkali washing pump and the regulating valve. In the water washing module 2, a pH meter 3 is provided on the pipeline where the heavy phase outlet is located, and a regulating valve 2 is provided on the pipeline where the heavy phase inlet is located. The pH meter 3 is interlocked with the washing water pump 2 and the regulating valve 2 for control.

2. A continuous post-processing system for a nitrate ester-containing synthetic liquid according to claim 1, characterized in that: The main machines in the water washing module 1, the alkali washing module and the water washing module 2 are all annular gap centrifugal extractors with the same specifications.

3. A continuous post-processing system for nitrate ester-containing synthetic liquid according to claim 1, characterized in that: A flow meter and a differential pressure transmitter are arranged on the feed side pipeline of any one of the feed pump, the first wash water pump, the alkali wash pump and the second wash water pump.

4. The continuous post-processing system for nitrate ester-containing synthetic liquid according to claim 1, characterized in that: A check valve and a drain valve are arranged on the discharge side pipeline of any one of the feed pump, the first wash water pump, the alkali wash pump and the second wash water pump.

5. The continuous post-processing system for nitrate ester-containing synthetic liquid according to claim 1, characterized in that: An inspection hole is provided on the side wall of the vertical shell; and a lifting ear plate is provided on the top of the vertical shell.

6. The continuous post-processing system for nitrate ester-containing synthetic liquid according to claim 1, characterized in that: The pH meter 1, pH meter 2 and pH meter 3 are all industrial analysis integrated pH meters with a 4-20mA signal remote transmission interface.

7. The continuous post-processing system for nitrate ester-containing synthetic liquid according to claim 1, characterized in that: The feed pump is any one of a diaphragm pump, a peristaltic pump, a viscose liquid delivery pump, and a twin-screw pump.

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