CN220425092U - Sulfuric acid diluting device and NO synthesis system using same - Google Patents

Sulfuric acid diluting device and NO synthesis system using same Download PDF

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Publication number
CN220425092U
CN220425092U CN202321811641.6U CN202321811641U CN220425092U CN 220425092 U CN220425092 U CN 220425092U CN 202321811641 U CN202321811641 U CN 202321811641U CN 220425092 U CN220425092 U CN 220425092U
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pipeline
sulfuric acid
valve
tank
reaction kettle
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赵东君
张福旺
杜志勇
马春菊
闫赵新
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Linggas Tianjin Co ltd
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Linggas Tianjin Co ltd
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Abstract

The utility model provides a sulfuric acid diluting device and an NO synthesis system using the same, comprising a sulfuric acid mixing device, a concentrated sulfuric acid storage tank, a concentrated sulfuric acid source tank and a vacuum pump; the sulfuric acid mixing device is connected with the concentrated sulfuric acid storage tank through a first pipeline, the concentrated sulfuric acid storage tank is connected with the concentrated sulfuric acid source tank through a second pipeline, and the vacuum pump is connected with the concentrated sulfuric acid storage tank through a third pipeline; the sulfuric acid mixing device comprises a cooling assembly, a first stirring assembly and a sulfuric acid diluting tank, wherein the cooling assembly is arranged outside the sulfuric acid diluting tank, and the first stirring assembly is arranged in the sulfuric acid diluting tank. The device reduces the labor intensity of staff by means of vacuumizing and feeding, automatic dropwise adding of concentrated sulfuric acid, motor stirring and the like, and reduces and eliminates the safety risk to the greatest extent.

Description

Sulfuric acid diluting device and NO synthesis system using same
Technical Field
The utility model belongs to the field of chemical synthesis, and particularly relates to a sulfuric acid diluting device and an NO synthesis system using the same.
Background
In the NO synthesis process, dilute sulfuric acid is an important raw material. The process is mainly characterized in that the process is mainly carried out by outsourcing concentrated sulfuric acid with the concentration of 98%, then pure water is used for diluting the concentrated sulfuric acid to the concentration required by the process after the concentrated sulfuric acid reaches the factory, the preparation process is carried out by pure hands, water is received in advance, then the concentrated sulfuric acid is slowly poured into the water by hands, manual continuous stirring is needed in the process, and finally the obtained process diluted sulfuric acid is filled into a diluted sulfuric acid storage tank of an NO system by hands. The acid preparation efficiency is low, and a plurality of safety risks exist in the operation process.
Disclosure of Invention
In view of the above, the present utility model is directed to a sulfuric acid diluting device and a NO synthesis system using the same, so as to solve the problems of low acid preparing efficiency and various safety risks in the operation process.
In order to achieve the above purpose, the technical scheme of the utility model is realized as follows:
a sulfuric acid diluting device comprises a sulfuric acid mixing device, a concentrated sulfuric acid storage tank, a concentrated sulfuric acid source tank and a vacuum pump;
the sulfuric acid mixing device is connected with the concentrated sulfuric acid storage tank through a first pipeline, the concentrated sulfuric acid storage tank is connected with the concentrated sulfuric acid source tank through a second pipeline, and the vacuum pump is connected with the concentrated sulfuric acid storage tank through a third pipeline;
the sulfuric acid mixing device comprises a cooling assembly, a first stirring assembly and a sulfuric acid diluting tank, wherein the cooling assembly is arranged outside the sulfuric acid diluting tank, and the first stirring assembly is arranged in the sulfuric acid diluting tank.
Further, the sulfuric acid diluting tank is connected with the bottom of the concentrated sulfuric acid storage tank through a first pipeline, and a first valve is arranged on the first pipeline;
the top of the concentrated sulfuric acid storage tank is connected with a concentrated sulfuric acid source tank through a second pipeline, and a second valve is arranged on the second pipeline;
the vacuum pump is connected with the top of the concentrated sulfuric acid source tank through a third pipeline; and a third valve is arranged on the third pipeline.
Further, a fourth pipeline is arranged on the sulfuric acid diluting tank, a fourth valve is arranged on the water adding pipeline, the sulfuric acid diluting tank is connected with the dilute sulfuric acid storage tank through a fifth pipeline, and a fifth valve is arranged on the fifth pipeline; the dilute sulfuric acid storage tank is connected with the vacuum pump through a sixth pipeline, and a sixth valve is arranged on the sixth pipeline.
The first stirring assembly comprises a first stirring motor, a first stirring shaft and a first stirring rod, wherein the output end of the first stirring motor is fixedly connected with the first stirring shaft, and the first stirring rod is arranged at the bottom of the first stirring shaft.
Preferably, the first stirring rod is of a U-shaped structure, and the middle part of the first stirring rod is connected with the first stirring shaft.
The stiff end of first agitator motor passes through the motor support and sets up the top at the sulphuric acid dilution tank.
Further, the cooling assembly comprises a water jacket clamp, and the inner layer of the water jacket clamp corresponds to the size of the sulfuric acid dilution tank.
And a cofferdam is also arranged on the outer side of the sulfuric acid mixing device, and is prepared from an acrylic plate.
Prevent that the staving from breaking and causing the sulphuric acid to leak and overflow everywhere to set up ya keli board protective wall in the outermost, prevent that the pipeline from breaking and splash.
The sulfuric acid mixing device is internally provided with a first temperature device, the concentrated sulfuric acid storage tank is internally provided with a second temperature device, and the dilute sulfuric acid storage tank is internally provided with a third temperature device.
The interval between the inner layer and the outer layer of the water jacket is not less than 200mm, and the first stirring motor is provided with a speed reducing machine. A first stirring motor (about 60 r/min) with a speed reducer is used for being matched with a glass stirring spear to replace manual stirring, and a water jacket is additionally arranged on the outer layer of the acid storage barrel for cooling.
In the process of acid preparation, a water jet acid and alkali resistant vacuum pump is used for vacuumizing a concentrated sulfuric acid storage tank, and after the storage tank is pumped to-100 KPa, concentrated sulfuric acid is added into a high-level barrel through a negative pressure environment.
The concentrated sulfuric acid storage tank of the design utilizes a 50L glass storage tank, and according to capacity calculation, the sulfuric acid pumping action is needed to be carried out twice when the dilute sulfuric acid needed by two kettles is prepared at one time.
And finally, dropwise adding concentrated sulfuric acid into the stirring dilution barrel at the speed of (2-3) L/min by adjusting the opening of the valve, and preparing dilute sulfuric acid.
The NO synthesis system using the sulfuric acid dilution device comprises a sulfuric acid dilution device, a reaction kettle device, a first-stage buffer tank, an alkaline washing device, a second-stage buffer tank, a gas-liquid separator, an adsorption column assembly, a finished product buffer tank and a finished product device;
the sulfuric acid diluting device is connected with the reaction kettle device through a pipeline, the reaction kettle device is connected with the primary buffer tank through a pipeline, the primary buffer tank is connected with the alkaline washing device through a pipeline, the alkaline washing device is connected with the secondary buffer tank through a pipeline, the secondary buffer tank is connected with the gas-liquid separator through a pipeline, the gas-liquid separator assembly is connected with the adsorption column assembly through a pipeline, the adsorption column assembly is connected with the finished product buffer tank assembly through a pipeline, and the finished product buffer tube is connected with the finished product device through a pipeline.
Further, the reaction kettle device, the alkaline washing device, the adsorption column component and the finished product device are connected with a vacuum pump of the sulfuric acid diluting device through a seventh pipeline, and a seventh valve is arranged on the seventh pipeline.
Further, the top of the reaction kettle device is connected with the bottom of a dilute sulfuric acid storage tank of the sulfuric acid diluting device through an eighth pipeline, and an eighth valve is arranged on the eighth pipeline; a metering pump is arranged on the eighth pipeline;
the reaction kettle device comprises a reaction kettle, a second stirring assembly and a feeding pipeline, wherein the second stirring assembly is arranged in the reaction kettle, the feeding pipeline is connected with the reaction kettle, and a metering valve is arranged on the feeding pipeline;
the top of reation kettle is equipped with first adjusting pipeline, is equipped with first gas valve and first manometer on the first adjusting pipeline in proper order.
The reaction kettle is provided with a ninth pipeline, a ninth valve is arranged on the ninth pipeline, and the ninth pipeline is a nitrous acid liquid feeding pipeline.
Preferably, the second stirring assembly comprises a second stirring motor, a second stirring shaft and a second stirring rod, the output end of the second stirring motor is fixedly connected with the second stirring shaft, and a plurality of second stirring rods are uniformly arranged at the bottom of the second stirring shaft.
Further, the top of the reaction kettle is connected with the lower part of the first-stage buffer tank through a tenth pipeline, and a tenth valve is arranged on the tenth pipeline;
the top of the first-stage buffer tank is connected with the alkaline washing component through an eleventh pipeline, an eleventh valve is arranged on the eleventh pipeline, the top of the alkaline washing component is connected with the bottom of the second-stage buffer tank through a twelfth pipeline, a twelfth valve is arranged on the twelfth pipeline,
the alkaline washing component comprises a plurality of alkaline washing tanks which are connected through thirteenth pipelines, and thirteenth valves are arranged on the thirteenth pipelines; the alkaline washing tanks are connected with a vacuum pump through pipelines.
The alkaline washing tank is provided with a feeding pipeline, and the feeding pipeline is provided with a feeding valve.
The top of the second-stage buffer tank is connected with the bottom of the gas-liquid separator through a fourteenth pipeline, and a fourteenth valve is arranged on the fourteenth pipeline.
Further, the adsorption column assembly comprises a plurality of adsorption columns, the adsorption columns are sequentially connected through pipelines, a second adjusting pipeline is arranged on the pipelines, and a second gas valve and a second pressure gauge are sequentially arranged on the second adjusting pipeline.
The top of the gas-liquid separator is connected with the bottom of the adsorption column component through a fifteenth pipeline, a fifteenth valve is arranged on the fifteenth pipeline, a first nitrogen purging pipe is arranged on the fifteenth pipeline, and a first nitrogen purging valve is arranged on the first nitrogen purging pipe.
The adsorption column assembly is connected with a finished product buffer tank through a sixteenth pipeline, the sixteenth pipeline is provided with a sixteenth valve, the finished product buffer tank is connected with a finished product device through a seventeenth pipeline, the seventeenth pipeline is provided with a seventeenth valve and a third adjusting pipeline, and the third adjusting pipeline is sequentially provided with a third gas valve and a third pressure gauge.
Further, the finished product device comprises a filling compressor and a vacuum tank assembly, the finished product buffer tank is connected with the filling compressor through a pipeline, the filling compressor is connected with the vacuum tank assembly through an eighteenth pipeline, an eighteenth valve and a fourth pressure gauge are arranged on the eighteenth pipeline, the vacuum tank assembly comprises two vacuum tank groups, the two vacuum tank groups are connected with the eighteenth pipeline in parallel through a nineteenth pipeline, and the nineteenth pipeline is provided with the nineteenth valve and the fifth pressure gauge.
The nineteenth valve and the second pressure gauge are respectively arranged at two sides of the vacuum tanks.
The second nitrogen purging pipeline is connected with the vacuum tank group through a twentieth pipeline respectively, and a twentieth valve is arranged on the twentieth pipeline.
The vacuum tank group comprises a plurality of vacuum tanks, the vacuum tanks are connected with a nineteenth pipeline through a twenty-first pipeline, and a twenty-first valve is arranged on the twenty-first pipeline.
Compared with the prior art, the sulfuric acid diluting device and the NO synthesis system using the same have the following advantages:
1. the device reduces the labor intensity of staff by means of vacuumizing and feeding, automatic dropwise adding of concentrated sulfuric acid, motor stirring and the like, and reduces and eliminates the safety risk to the greatest extent.
2. The sulfuric acid diluting device is added in the NO synthesis process system, concentrated sulfuric acid is filled into the concentrated sulfuric acid storage tank above through vacuumizing, a bottom valve is opened during acid preparation, the concentrated sulfuric acid is added into the acid preparation storage tank at a constant speed through adjusting the opening of the valve, and meanwhile, the stirring motor of the acid preparation storage tank is started, so that the aim of safe acid preparation is fulfilled. The prepared dilute sulfuric acid is stored in a tank, is connected with a dilute sulfuric acid storage tank in the process through a pipeline, and is filled into the process dilute sulfuric acid storage tank at any time according to production requirements.
Drawings
The accompanying drawings, which are included to provide a further understanding of the utility model and are incorporated in and constitute a part of this specification, illustrate embodiments of the utility model and together with the description serve to explain the utility model. In the drawings:
FIG. 1 is a schematic view of a sulfuric acid dilution apparatus according to an embodiment of the present utility model;
fig. 2 is a schematic diagram of an NO synthesis system using the device according to an embodiment of the present utility model.
Reference numerals illustrate:
1. a concentrated sulfuric acid storage tank; 2. a concentrated sulfuric acid source tank; 3. a vacuum pump; 4. a sulfuric acid dilution tank; 5. a first valve; 6. a second valve; 7. a third valve; 8. a fourth valve; 9. a first water pump; 10. a first stirring motor; 11. a first stirring shaft; 12. a first stirring rod; 13. a water jacket clamp; 14. a cofferdam; 15. a first-stage buffer tank; 16. a second-stage buffer tank; 17. a gas-liquid separator; 18. a finished product buffer tank; 19. a seventh valve; 20. an eighth valve; 21. a reaction kettle; 22. a metering valve; 23. a first gas valve; 24. a first pressure gauge; 25. a ninth valve; 26. a second stirring assembly; 27. a tenth valve; 28. an eleventh valve; 29. a twelfth valve; 30. an alkaline washing tank; 31. a thirteenth valve; 32. a fourteenth valve; 33. an adsorption column; 34. a second gas valve; 35. a second pressure gauge; 36. a fifteenth valve; 37. a first purge nitrogen valve; 38. a sixteenth valve; 39. seventeenth valve; 40. a third gas valve; 41. a third pressure gauge; 42. filling the compressor; 43. a vacuum tank group; 44. an eighteenth valve; 45. a fourth pressure gauge; 46. a nineteenth valve; 47. a fifth pressure gauge; 48. a twentieth valve; 49. a twenty-first valve; 50. a dilute sulfuric acid storage tank; 51. metering pump.
Detailed Description
It should be noted that, without conflict, the embodiments of the present utility model and features of the embodiments may be combined with each other.
In the description of the present utility model, it should be understood that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present utility model and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present utility model. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first", "a second", etc. may explicitly or implicitly include one or more such feature. In the description of the present utility model, unless otherwise indicated, the meaning of "a plurality" is two or more.
In the description of the present utility model, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present utility model can be understood by those of ordinary skill in the art in a specific case.
The utility model will be described in detail below with reference to the drawings in connection with embodiments.
As shown in fig. 1 to 2, a sulfuric acid diluting device comprises a sulfuric acid mixing device, a concentrated sulfuric acid storage tank 1, a concentrated sulfuric acid source tank 2 and a vacuum pump 3; the sulfuric acid mixing device is connected with a concentrated sulfuric acid storage tank 1 through a first pipeline, the concentrated sulfuric acid storage tank 1 is connected with a concentrated sulfuric acid source tank 2 through a second pipeline, and a vacuum pump 3 is connected with the concentrated sulfuric acid storage tank 1 through a third pipeline; the sulfuric acid mixing device comprises a cooling component, a first stirring component and a sulfuric acid diluting tank 4, wherein the cooling component is arranged outside the sulfuric acid diluting tank 4, and the first stirring component is arranged in the sulfuric acid diluting tank 4. The sulfuric acid dilution tank 4 is connected with the bottom of the concentrated sulfuric acid storage tank 1 through a first pipeline, and a first valve 5 is arranged on the first pipeline; the top of the concentrated sulfuric acid storage tank 1 is connected with the concentrated sulfuric acid source tank 2 through a second pipeline, and a second valve 6 is arranged on the second pipeline; the vacuum pump 3 is connected with the top of the concentrated sulfuric acid source tank 2 through a third pipeline; the third pipeline is provided with a third valve 7.
The sulfuric acid diluting tank 4 is provided with a fourth pipeline, the water adding pipeline is provided with a fourth valve 8, the sulfuric acid diluting tank 4 is connected with the dilute sulfuric acid storage tank 50 through a fifth pipeline, and the fifth pipeline is provided with a fifth valve; the dilute sulfuric acid tank 50 is connected with the vacuum pump 3 through a sixth pipeline, and a sixth valve is arranged on the sixth pipeline. The first stirring assembly comprises a first stirring motor 10, a first stirring shaft 11 and a first stirring rod 12, wherein the output end of the first stirring motor 10 is fixedly connected with the first stirring shaft 11, and the first stirring rod 12 is arranged at the bottom of the first stirring shaft 11.
In a specific embodiment, the first stirring rod 12 has a U-shaped structure, and the middle part of the first stirring rod 12 is connected with the first stirring shaft 11. The fixed end of the first stirring motor 10 is disposed above the sulfuric acid dilution tank 4 by a motor bracket (not shown in fig. 1).
The cooling assembly comprises a water jacket clamp 13, and the inner layer of the water jacket clamp 13 corresponds to the size of the sulfuric acid dilution tank 4. The outer side of the sulfuric acid mixing device is also provided with a cofferdam 14, and the cofferdam 14 is prepared from an acrylic plate. Prevent that the staving from breaking and causing the sulphuric acid to leak and overflow everywhere to set up ya keli board protective wall in the outermost, prevent that the pipeline from breaking and splash. The sulfuric acid mixing device is internally provided with a first temperature device, the concentrated sulfuric acid storage tank 1 is internally provided with a second temperature device, and the dilute sulfuric acid storage tank 50 is internally provided with a third temperature device. The space between the inner layer and the outer layer of the water jacket is not less than 200mm, and the first stirring motor 10 is provided with a speed reducing machine. The first stirring motor 10 (about 60 r/min) with a speed reducer is used in combination with a glass stirring spear to replace manual stirring, and a water jacket is additionally arranged on the outer layer of the acid storage barrel for cooling. In the process of acid preparation, a water jet acid-alkali resistant vacuum pump 3 is used for vacuumizing the concentrated sulfuric acid storage tank 1, and after the storage tank is pumped to-100 KPa, the concentrated sulfuric acid is added into a high-level barrel through a negative pressure environment. The concentrated sulfuric acid storage tank 1 of the design utilizes a 50L glass storage tank, and according to capacity calculation, the sulfuric acid pumping action is needed to be carried out twice when the dilute sulfuric acid needed by two kettles is prepared at one time. And finally, dropwise adding concentrated sulfuric acid into the stirring dilution barrel at the speed of (2-3) L/min by adjusting the opening of the valve, and preparing dilute sulfuric acid.
The NO synthesis system using the sulfuric acid dilution device comprises a sulfuric acid dilution device, a reaction kettle device, a first-stage buffer tank 15, an alkaline washing device, a second-stage buffer tank 16, a gas-liquid separator 17, an adsorption column assembly, a finished product buffer tank 18 and a finished product device; the sulfuric acid diluting device is connected with the reaction kettle device through a pipeline, the reaction kettle device is connected with the primary buffer tank 15 through a pipeline, the primary buffer tank is connected with the alkaline washing device through a pipeline, the alkaline washing device is connected with the secondary buffer tank 16 through a pipeline, the secondary buffer tank 16 is connected with the gas-liquid separator 17 through a pipeline, the gas-liquid separator assembly is connected with the adsorption column assembly through a pipeline, the adsorption column assembly is connected with the finished product buffer tank assembly through a pipeline, and the finished product buffer tube is connected with the finished product device through a pipeline. The reaction kettle device, the alkaline washing device, the adsorption column component and the finished product device are connected with the vacuum pump 3 of the sulfuric acid diluting device through a seventh pipeline, and a seventh valve 19 is arranged on the seventh pipeline.
The top of the reaction kettle device is connected with the bottom of a dilute sulfuric acid storage tank 50 of the sulfuric acid diluting device through an eighth pipeline, and an eighth valve 20 is arranged on the eighth pipeline; the reaction kettle device comprises a reaction kettle 21, a second stirring assembly 26 and a feeding pipeline, wherein the second stirring assembly 26 is arranged in the reaction kettle 21, the feeding pipeline is connected with the reaction kettle 21, and a metering valve 22 is arranged on the feeding pipeline; the top of the reaction kettle 21 is provided with a first adjusting pipeline, and a first gas valve 23 and a first pressure gauge 24 are sequentially arranged on the first adjusting pipeline. The reaction kettle 21 is provided with a ninth pipeline, the ninth pipeline is provided with a ninth valve 25, and the ninth pipeline can discharge gas in the reaction kettle 21.
In a specific embodiment, the second stirring assembly 26 includes a second stirring motor, a second stirring shaft, and a second stirring rod, where an output end of the second stirring motor is fixedly connected to the second stirring shaft, and a plurality of second stirring rods are uniformly disposed at the bottom of the second stirring shaft.
The top of the reaction kettle 21 is connected with the lower part of the primary buffer tank 15 through a tenth pipeline, and a tenth valve 27 is arranged on the tenth pipeline; the top of the primary buffer tank 15 is connected with an alkaline cleaning component through an eleventh pipeline, an eleventh valve 28 is arranged on the eleventh pipeline, the top of the alkaline cleaning component is connected with the bottom of the secondary buffer tank 16 through a twelfth pipeline, a twelfth valve 29 is arranged on the twelfth pipeline, the alkaline cleaning component comprises a plurality of alkaline cleaning tanks 30, the plurality of alkaline cleaning tanks 30 are connected through thirteenth pipelines, and a thirteenth valve 31 is arranged on the thirteenth pipeline; the alkaline washing tank 30 is connected with the vacuum pump 3 through pipelines. The alkaline washing tank 30 is provided with a feeding pipeline, and the feeding pipeline is provided with a feeding valve. The top of the secondary buffer tank 16 is connected with the bottom of the gas-liquid separator 17 through a fourteenth pipeline, and a fourteenth valve 32 is arranged on the fourteenth pipeline.
The adsorption column assembly comprises a plurality of adsorption columns 33, the adsorption columns 33 are sequentially connected through pipelines, and a second adjusting pipeline is arranged on the pipeline and is sequentially provided with a second gas valve 34 and a second pressure gauge 35. The top of the gas-liquid separator 17 is connected with the bottom of the adsorption column assembly through a fifteenth pipeline, a fifteenth valve 36 is arranged on the fifteenth pipeline, a first purging nitrogen pipe is arranged on the fifteenth pipeline, and a first purging nitrogen valve 37 is arranged on the first purging nitrogen pipe. The adsorption column assembly is connected with the finished product buffer tank 18 through a sixteenth pipeline, the sixteenth pipeline is provided with a sixteenth valve 38, the finished product buffer tank 18 is connected with a finished product device through a seventeenth pipeline, the seventeenth pipeline is provided with a seventeenth valve 39 and a third adjusting pipeline, and the third adjusting pipeline is sequentially provided with a third gas valve 40 and a third pressure gauge 41. The finished product device comprises a filling compressor 42 and a vacuum tank assembly, the finished product buffer tank 18 is connected with the filling compressor 42 through a pipeline, the filling compressor 42 is connected with the vacuum tank assembly through an eighteenth pipeline, an eighteenth valve 44 and a fourth pressure gauge 45 are arranged on the eighteenth pipeline, the vacuum tank assembly comprises two vacuum tank groups 43, the two vacuum tank groups 43 are connected with the eighteenth pipeline in parallel through a nineteenth pipeline, and a nineteenth valve 46 and a fifth pressure gauge 47 are arranged on the nineteenth pipeline. Nineteenth valve 46, second manometer 35 are provided on both sides of the several vacuum tanks, respectively.
The process adopts sodium nitrite solution and dilute sulfuric acid to react intermittently at normal temperature to produce nitric oxide, and the nitric oxide is then alkali washed, adsorbed and dried and compressed in a compressor into steel cylinder to obtain low purity product. The aqueous solution of sodium nitrite reacts with dilute sulfuric acid in the reaction kettle 21, the generated nitric oxide gas is discharged out of the reaction kettle 21, and the rest products comprise sodium sulfate (Na 2 SO 4 ) Sodium nitrate (NaNO) 3 ) Water remains in the reaction vessel 21. Before production, a sulfuric acid diluting device is required to be used in advance to prepare dilute sulfuric acid with a certain concentration, the dilute sulfuric acid is connected with a sulfuric acid storage tank in a process line through a bottom inserting pipe of the device, before each reaction, a vacuum pump 3 is used for vacuumizing the sulfuric acid storage tank of the process line, a sulfuric acid feeding valve can be opened when the sulfuric acid is pumped to below-80 KPa, the dilute sulfuric acid is filled into the sulfuric acid storage tank through negative pressure (the dosage of one kettle is filled each time), and after the filling is finished, the dilute sulfuric acid for one kettle is prepared by the diluting device for later use.
The synthesis process principle is as follows:
the process adopts sodium nitrite solution and 52% dilute sulfuric acid to react to generate nitric oxide, and then the nitric oxide is subjected to alkaline washing, adsorption drying and compression into a steel cylinder by a compressor, so that a low-purity product is obtained. The reaction can be carried out at normal temperature without heating. The aqueous solution of sodium nitrite reacts with dilute sulfuric acid in the reaction kettle 21, the generated nitric oxide gas is discharged out of the reaction kettle 21, and the rest products comprise sodium sulfate (Na 2 SO 4 ) Sodium nitrate (NaNO) 3 ) Water remains in the reaction vessel 21. The reaction is a batch reaction, and the residual liquid in the reaction vessel 21 is discharged after each reaction.
The reaction equation is: naNO 2 +H 2 SO 4 →NO+Na 2 SO 4 +NaNO 3 +H 2 O
The synthetic operation flow is as follows:
before production, a sulfuric acid diluting device is required to be used in advance to prepare dilute sulfuric acid with a certain concentration, the dilute sulfuric acid is connected with a sulfuric acid storage tank in a process line through a bottom inserting pipe of the device, before each reaction, a vacuum pump 3 is used for vacuumizing the sulfuric acid storage tank of the process line, a sulfuric acid feeding valve can be opened when the sulfuric acid is pumped to below-80 KPa, the dilute sulfuric acid is filled into the sulfuric acid storage tank through negative pressure (the dosage of one kettle is filled each time), and after the filling is finished, the dilute sulfuric acid for one kettle is prepared by the diluting device for later use.
And vacuumizing the reaction kettle 21 and the dilute sulfuric acid storage tank 50, and closing a valve on a vacuum pipe when the vacuum degree is less than-0.08 Mpa. The dilute sulfuric acid tank bottom valve and the sulfuric acid feed valve of the reaction kettle 21 are opened, and then the stirrer of the reaction kettle 21 is started. The metering valve 22 is started, the knob of the metering valve 22 is turned, the flow knob of the metering valve 22 is adjusted to 20%, the reaction starts and products are produced, when the pressure of the reaction kettle 21 is increased to 0bar, the knob of the metering valve 22 is adjusted to 15%, and the stable reaction starts. When the pressure of the reaction kettle 21 reaches 0.05Mpa, an outlet valve of the reaction kettle 21 is opened, and then a valve between the primary buffer and the primary alkaline wash is opened. And opening all valves on a main pipeline of the production system, starting a compressor to press when the pressure of the nitric oxide storage tank reaches 0.2Mpa, replacing the production system by using the pressed product, and discharging the replaced product to a washing tower through a filling pipe converging emptying valve to be washed and then emptying. The processed empty bottles are correctly connected to the filling system, and the valves on the pipelines at the connection positions are opened. And in the process of the replacement system, sampling and analyzing by using a steel cylinder, stopping replacement after the index of 2.8N of the product is reached, and starting filling the steel cylinder.
When the liquid level of the dilute sulfuric acid storage tank 50 reaches a warning line or the pressure of the reaction kettle 21 is gradually reduced, the power supply of the metering valve 22 is closed, the addition of sulfuric acid is stopped, and the bottom valve of the dilute sulfuric acid storage tank 50 and the sulfuric acid dropping valve on the reaction kettle 21 are closed. When the pressure of the reaction kettle 21 is less than 0.05Mpa, stopping the stirrer and the compressor, closing the steel cylinder valve, and closing the discharge valve of the reaction kettle 21. Starting a tail gas washing tower and an exhaust fan, placing a residual liquid collector under a liquid outlet of the reaction kettle 21, slowly opening a residual liquid discharge valve on the reaction kettle 21, starting to discharge residual liquid, and closing the residual liquid discharge valve on the reaction kettle 21 after the residual liquid is discharged. Repeating the operation steps to carry out the production of the next kettle.
The foregoing description of the preferred embodiments of the utility model is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the utility model.

Claims (10)

1. A sulfuric acid dilution device, characterized in that: comprises a sulfuric acid mixing device, a concentrated sulfuric acid storage tank (1), a concentrated sulfuric acid source tank (2) and a vacuum pump (3);
the sulfuric acid mixing device is connected with the concentrated sulfuric acid storage tank (1) through a first pipeline, the concentrated sulfuric acid storage tank (1) is connected with the concentrated sulfuric acid source tank (2) through a second pipeline, and the vacuum pump (3) is connected with the concentrated sulfuric acid storage tank (1) through a third pipeline;
the sulfuric acid mixing device comprises a cooling component, a first stirring component and a sulfuric acid diluting tank (4), wherein the cooling component is arranged outside the sulfuric acid diluting tank (4), and the first stirring component is arranged in the sulfuric acid diluting tank (4).
2. A sulfuric acid dilution apparatus according to claim 1, wherein: the sulfuric acid diluting tank (4) is connected with the bottom of the concentrated sulfuric acid storage tank (1) through a first pipeline, and a first valve (5) is arranged on the first pipeline;
the top of the concentrated sulfuric acid storage tank (1) is connected with the concentrated sulfuric acid source tank (2) through a second pipeline, and a second valve (6) is arranged on the second pipeline;
the vacuum pump (3) is connected with the top of the concentrated sulfuric acid source tank (2) through a third pipeline; the third pipeline is provided with a third valve (7).
3. A sulfuric acid dilution apparatus according to claim 1, wherein: the sulfuric acid diluting tank (4) is provided with a fourth pipeline, the water adding pipeline is provided with a fourth valve (8), the sulfuric acid diluting tank (4) is connected with the dilute sulfuric acid storage tank (50) through a fifth pipeline, and the fifth pipeline is provided with a fifth valve; the dilute sulfuric acid storage tank (50) is connected with the vacuum pump (3) through a sixth pipeline, and a sixth valve is arranged on the sixth pipeline;
the first stirring assembly comprises a first stirring motor (10), a first stirring shaft (11) and a first stirring rod (12), wherein the output end of the first stirring motor (10) is fixedly connected with the first stirring shaft (11), and the first stirring rod (12) is arranged at the bottom of the first stirring shaft (11).
4. A sulfuric acid dilution apparatus according to claim 1, wherein: the cooling assembly comprises a water jacket clamp (13), and the inner layer of the water jacket clamp (13) corresponds to the sulfuric acid dilution tank (4) in size;
a cofferdam (14) is arranged on the outer side of the sulfuric acid mixing device;
the sulfuric acid mixing device is internally provided with a first temperature device, the concentrated sulfuric acid storage tank (1) is internally provided with a second temperature device, and the dilute sulfuric acid storage tank (50) is internally provided with a third temperature device.
5. A NO synthesis system using the sulfuric acid dilution unit according to any one of claims 1-4, characterized in that: comprises a sulfuric acid diluting device, a reaction kettle device, a primary buffer tank (15), an alkaline washing device, a secondary buffer tank (16), a gas-liquid separator (17), an adsorption column assembly, a finished product buffer tank (18) and a finished product device;
the sulfuric acid diluting device is connected with the reaction kettle device through a pipeline, the reaction kettle device is connected with the primary buffer tank (15) through a pipeline, the primary buffer device is connected with the alkaline washing device through a pipeline, the alkaline washing device is connected with the secondary buffer tank (16) through a pipeline, the secondary buffer tank (16) is connected with the gas-liquid separator (17) through a pipeline, the gas-liquid separator component is connected with the adsorption column component through a pipeline, the adsorption column component is connected with the finished product buffer tank component through a pipeline, and the finished product buffer tube is connected with the finished product device through a pipeline.
6. The NO synthesis system according to claim 5, wherein: the reaction kettle device, the alkaline washing device, the adsorption column component and the finished product device are connected with a vacuum pump (3) of the sulfuric acid diluting device through a seventh pipeline, and a seventh valve (19) is arranged on the seventh pipeline.
7. A sulfuric acid diluting device and NO synthesis system using the same according to claim 5, wherein: the top of the reaction kettle device is connected with the bottom of a dilute sulfuric acid storage tank (50) of the sulfuric acid diluting device through an eighth pipeline, and an eighth valve (20) is arranged on the eighth pipeline;
a metering pump (51) is arranged on the eighth pipeline;
the reaction kettle device comprises a reaction kettle (21), a second stirring assembly (26) and a feeding pipeline, wherein the second stirring assembly (26) is arranged in the reaction kettle (21), the feeding pipeline is connected with the reaction kettle (21), and a metering valve (22) is arranged on the feeding pipeline;
the top of the reaction kettle (21) is provided with a first adjusting pipeline, and a first gas valve (23) and a first pressure gauge (24) are sequentially arranged on the first adjusting pipeline;
the reaction kettle (21) is provided with a ninth pipeline, and the ninth pipeline is provided with a ninth valve (25).
8. A sulfuric acid diluting device and NO synthesis system using the same according to claim 7, wherein: the top of the reaction kettle (21) is connected with the lower part of the first-stage buffer tank (15) through a tenth pipeline, and a tenth valve (27) is arranged on the tenth pipeline;
the top of the primary buffer tank (15) is connected with an alkaline washing assembly through an eleventh pipeline, an eleventh valve (28) is arranged on the eleventh pipeline, the top of the alkaline washing assembly is connected with the bottom of the secondary buffer tank (16) through a twelfth pipeline, and a twelfth valve (29) is arranged on the twelfth pipeline;
the alkaline washing assembly comprises a plurality of alkaline washing tanks (30), the plurality of alkaline washing tanks (30) are connected through thirteenth pipelines, and thirteenth valves (31) are arranged on the thirteenth pipelines; the alkaline washing tanks (30) are connected with a vacuum pump (3) through pipelines;
a feeding pipeline is arranged on the alkaline washing tank (30), and a feeding valve is arranged on the feeding pipeline;
the top of the second-stage buffer tank (16) is connected with the bottom of the gas-liquid separator (17) through a fourteenth pipeline, and a fourteenth valve (32) is arranged on the fourteenth pipeline.
9. A sulfuric acid diluting device and NO synthesis system using the same according to claim 8, wherein: the adsorption column assembly comprises a plurality of adsorption columns (33), the adsorption columns (33) are sequentially connected through pipelines, a second adjusting pipeline is arranged on the pipelines, and a second gas valve (34) and a second pressure gauge (35) are sequentially arranged on the second adjusting pipeline;
the top of the gas-liquid separator (17) is connected with the bottom of the adsorption column assembly through a fifteenth pipeline, a fifteenth valve (36) is arranged on the fifteenth pipeline, a first nitrogen purging pipe is arranged on the fifteenth pipeline, and a first nitrogen purging valve (37) is arranged on the first nitrogen purging pipe;
the adsorption column assembly is connected with a finished product buffer tank (18) through a sixteenth pipeline, a sixteenth valve (38) is arranged on the sixteenth pipeline, the finished product buffer tank (18) is connected with a finished product device through a seventeenth pipeline, a seventeenth valve (39) and a third adjusting pipeline are arranged on the seventeenth pipeline, and a third gas valve (40) and a third pressure gauge (41) are sequentially arranged on the third adjusting pipeline.
10. A sulfuric acid diluting device and NO synthesis system using the same according to claim 9, wherein: the finished product device comprises a filling compressor (42) and a vacuum tank assembly, wherein the finished product buffer tank (18) is connected with the filling compressor (42) through a pipeline, the filling compressor (42) is connected with the vacuum tank assembly through an eighteenth pipeline, an eighteenth valve (44) and a fourth pressure gauge (45) are arranged on the eighteenth pipeline, the vacuum tank assembly comprises two vacuum tank groups (43), the two vacuum tank groups (43) are connected with the eighteenth pipeline in parallel through nineteenth pipelines, and the nineteenth pipeline is provided with a nineteenth valve (46) and a fifth pressure gauge (47);
the nineteenth valve (46) and the second pressure gauge (35) are respectively arranged at two sides of the vacuum tanks;
the second nitrogen purging pipeline is connected with the vacuum tank group (43) through a twentieth pipeline respectively, and a twentieth valve (48) is arranged on the twentieth pipeline;
the vacuum tank group (43) comprises a plurality of vacuum tanks, the vacuum tanks are connected with a nineteenth pipeline through a twenty-first pipeline, and a twenty-first valve (49) is arranged on the twenty-first pipeline.
CN202321811641.6U 2023-07-11 2023-07-11 Sulfuric acid diluting device and NO synthesis system using same Active CN220425092U (en)

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