CN115463519B - Method and system for producing nitrososulfuric acid with high efficiency - Google Patents
Method and system for producing nitrososulfuric acid with high efficiency Download PDFInfo
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- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
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- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/093—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more sulfur atoms
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Abstract
The invention relates to a method and a system for producing nitroso sulfuric acid with high efficiency, which belongs to the technical field of chemical production, and the production method of nitroso sulfuric acid comprises the following steps: adding 98% sulfuric acid into a reaction kettle, stirring, adding nitric acid, introducing sulfur dioxide, and controlling the mass ratio of the 98% sulfuric acid to the nitric acid to the sulfur dioxide to be 2.5-2.52:1-1.02:1, controlling the temperature in the reaction kettle to be 80-95 ℃ and the pressure to be 0.1-0.15MPa, observing that the materials in the reaction kettle are cyan and transparent, namely, the reaction is completed, adding a tube type heat exchanger in a nitrososulfuric acid production system for cooling, wherein the tube type heat exchanger has high heat exchange speed, is beneficial to promoting the reaction efficiency and shortening the reaction time, then controlling the temperature to be 85 ℃ by the most preferred scheme in the invention, improving the reaction efficiency, and finally controlling the pressure of the reaction kettle to be 0.12MPa by the most preferred scheme in the invention, carrying out low-pressure reaction, and improving the safety of the production process.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a method and a system for producing nitroso sulfuric acid with high efficiency.
Background
The nitrososulfuric acid is mainly used for substituting sodium nitrite in the diazo reaction of disperse dye, thereby reducing the cost and improving the product quality, and is also widely applied to the fields of pesticides and medicines.
The invention patent CN106379875B discloses a production method and application of nitrososulfuric acid, and the production method disclosed in the invention is as follows: 1. heating and dehydrating waste acid generated by diazotization deamination to obtain concentrated waste acid, wherein the total acid concentration of the concentrated waste acid is more than 70%, and adding concentrated sulfuric acid to prepare mixed acid; 2. waste gas generated by the chloronitro reaction of nitrobenzene compounds is mixed with air and then is led into a mixed acid spray tower for absorption, and after the nitrososulfuric acid prepared in the spray tower is detected to be qualified, the nitrososulfuric acid is directly pumped into a nitrososulfuric acid storage tank, and the process utilizes recovered waste acid to prepare nitrososulfuric acid.
In response to increasing yield demands, the most common production processes for nitrososulfuric acid are: concentrated nitric acid sulfur dioxide gas absorption method (SO for short) 2 Absorption method) which takes concentrated sulfuric acid as a medium and adopts direct reaction of sulfur dioxide gas and concentrated nitric acid to obtain nitrososulfuric acid, but the method has complex process and lower production efficiency, which leads to longer production time, generally requires 12-24h, and the production process needs to be improved in order to realize efficient production.
Disclosure of Invention
In order to solve the technical problems mentioned in the background art, the invention aims to provide a method and a system for producing nitrososulfuric acid with high efficiency.
The aim of the invention can be achieved by the following technical scheme:
a method for producing nitrososulfuric acid with high efficiency, comprising the steps of:
a1, pumping 98% sulfuric acid (commercially available) in a sulfuric acid storage tank into a 98% sulfuric acid metering tank through a sulfuric acid pump, adding industrial water into the water metering tank, adding the industrial water into an acid preparation kettle, slowly adding 98% sulfuric acid while stirring, diluting the 98% sulfuric acid into 90% sulfuric acid, controlling the temperature in the acid preparation kettle to be 80-100 ℃, slowing down the adding rate of the 98% sulfuric acid when the temperature is too high, introducing the prepared 90% sulfuric acid into a sulfuric acid intermediate tank, and pumping the prepared 90% sulfuric acid into the 90% sulfuric acid metering tank through a sulfuric acid pump to finish the preparation work of sulfuric acid;
pumping 98% nitric acid into a nitric acid metering tank through a nitric acid pump to finish the preparation work of the nitric acid;
a3, pumping the liquid sulfur dioxide in the liquid sulfur dioxide storage tank into an air temperature type vaporizer through a liquid sulfur dioxide magnetic pump, converting the liquid sulfur dioxide into a gas state through heat exchange of the air temperature type vaporizer, and conveying the gas state sulfur dioxide to a buffer tank to finish sulfur dioxide preparation work;
a4, adding 98% sulfuric acid into the reaction kettle, stirring, adding nitric acid, starting a circulating pump, stirring for 30min in a circulating way, introducing sulfur dioxide, and controlling the mass ratio of the 98% sulfuric acid to the nitric acid to the sulfur dioxide to be 2.5-2.52:1-1.02:1, in a concentrated sulfuric acid system, sulfur dioxide directly reacts with nitric acid to prepare nitrososulfuric acid, the reaction releases heat, the temperature in a reaction kettle is controlled to be 80-95 ℃, the pressure in the reaction kettle is controlled to be 0.1-0.15MPa, if the pressure in the reaction kettle is overlarge, the reaction kettle is controlled by stopping or reducing the introduction of sulfur dioxide, the reaction is completed after observing that materials in the reaction kettle are cyan and transparent, and a finished product is pumped into a finished product tank to complete the high-efficiency production of nitrososulfuric acid.
In the production process, the reaction principle is as follows:
SO 2 +HNO 3 ＝＝NOHSO 4
wherein, the concentrated sulfuric acid provides the reaction system environment.
Further, the mass ratio of 98% sulfuric acid, nitric acid and sulfur dioxide in the step A4 is 2.52:1.02:1.
further, the temperature in the reaction kettle in the step A4 is 85 ℃.
Further, the pressure in the reaction kettle in the step A4 is 0.12MPa.
Further, a system for producing nitroso sulfuric acid with high efficiency comprises a sulfuric acid storage tank, a 98% sulfuric acid metering tank, a water metering tank, an acid preparing kettle, a sulfuric acid intermediate tank, a 90% sulfuric acid metering tank, a reaction kettle, a tube type heat exchanger, a nitric acid storage tank, a nitric acid metering tank, a liquid sulfur dioxide storage tank, a magnetic pump, an air temperature type vaporizer, a buffer tank and a finished product tank;
the utility model discloses a sulphuric acid device, including sulphuric acid storage tank, 98% sulphuric acid metering tank, 90% sulphuric acid pump, 90% sulphuric acid metering tank, 90% sulphuric acid pipeline, the sulphuric acid storage tank is in commercial 98% sulphuric acid in the sulphuric acid storage tank, the discharge gate of sulphuric acid storage tank communicates with 98% sulphuric acid metering tank's feed inlet, install the sulphuric acid pump on the pipeline between sulphuric acid storage tank and the 98% sulphuric acid metering tank, 98% sulphuric acid metering tank's discharge gate communicates with one side feed inlet of joining in marriage the sour cauldron, joining in marriage sour cauldron and be used for configuring commercial 98% sulphuric acid into 90% sulphuric acid, joining in marriage sour cauldron's discharge gate and sulphuric acid intermediate tank's feed inlet, the sulphuric acid intermediate tank is in the temporary storage 90% sulphuric acid, sulphuric acid pump is installed on the pipeline between sulphuric acid intermediate tank and the 90% sulphuric acid metering tank, simultaneously, the gas vent has been seted up to 90% sulphuric acid metering tank's upper end, gas vent and sulphuric acid intermediate tank's upper end communicates with the first feed inlet of reation kettle, sulphuric acid pipeline installation is accomplished.
The discharge gate of nitric acid storage tank and the feed inlet intercommunication of nitric acid metering tank install the nitric acid pump on the pipeline between nitric acid storage tank and the nitric acid metering tank, the discharge gate of nitric acid metering tank and reation kettle's second feed inlet intercommunication, and the nitric acid pipeline is installed and is accomplished.
The utility model discloses a sulfur dioxide device, including shell and tube heat exchanger, shell and tube heat exchanger's feed inlet intercommunication with the feed inlet intercommunication of empty temperature formula vaporizer, empty temperature formula vaporizer is used for changing liquid sulfur dioxide into the gaseous state, installs the magnetic drive pump on the pipeline between liquid sulfur dioxide storage tank and the empty temperature formula vaporizer, the feed inlet intercommunication of empty temperature formula vaporizer and buffer tank, the buffer tank is used for keeping in sulfur dioxide gas, the feed inlet intercommunication of buffer tank and shell and tube heat exchanger's one side feed inlet, shell and tube heat exchanger's opposite side feed inlet and reation kettle's one side feed inlet intercommunication, reation kettle's opposite side feed inlet and finished product jar's feed inlet intercommunication, shell and tube heat exchanger's discharge gate and reation kettle's third feed inlet, sulfur dioxide pipeline installation is accomplished. The shell and tube heat exchanger is used for reducing the temperature of materials in the reaction kettle.
Further, the sulfuric acid pump, the nitric acid pump and the magnetic pump are all provided with a standby application, so that the continuous operation of the system is ensured.
Further, jackets are arranged on the outer sides of the acid preparation kettle and the reaction kettle, circulating water is introduced into the jackets, and the circulating water is used for cooling the kettle body.
Further, the sulfuric acid storage tank, the 98% sulfuric acid metering tank, the water metering tank, the acid distribution kettle, the sulfuric acid intermediate tank, the 90% sulfuric acid metering tank, the reaction kettle, the tubular heat exchanger, the nitric acid storage tank, the nitric acid metering tank, the liquid sulfur dioxide storage tank, the magnetic pump, the buffer tank and the finished product tank are all provided with waste gas ports, and the waste gas ports are communicated with the plant tail gas absorbing device.
The invention has the beneficial effects that:
firstly, the reaction of preparing nitrososulfuric acid by reacting sulfur dioxide with concentrated nitric acid is exothermic, a refrigerating device is usually additionally arranged in the traditional process, and the invention adopts the additional arrangement of a tube type heat exchanger as cooling treatment equipment of a reaction kettle.
Then, the invention improves the reaction temperature in production, the temperature in the production of the traditional process is controlled below 70 ℃, the most preferable scheme in the invention controls the temperature at 85 ℃, and the reaction efficiency is improved, namely the reduction of the reaction time is realized.
Finally, in the production process of the invention, the pressure of the reaction kettle is controlled to be 0.1-0.15MPa, and the reaction is carried out at low pressure, so that the safety of the production process is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a system for producing nitrososulfuric acid with high efficiency according to the present invention.
In the drawings, the list of components represented by the various numbers is as follows:
1. a sulfuric acid storage tank; 2. a 98% sulfuric acid metering tank; 3. a water metering tank; 4. an acid preparing kettle; 5. a sulfuric acid intermediate tank; 6. a 90% sulfuric acid metering tank; 7. a reaction kettle; 8. a shell and tube heat exchanger; 9. a nitric acid storage tank; 10. a nitric acid metering tank; 11. a liquid sulfur dioxide storage tank; 12. a magnetic pump; 13. an air temperature type vaporizer; 14. a buffer tank; 15. and (5) a finished product tank.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A method for producing nitrososulfuric acid with high efficiency, comprising the steps of:
a1, pumping 98% sulfuric acid (commercially available) in a sulfuric acid storage tank 1 into a 98% sulfuric acid metering tank 2 through a sulfuric acid pump, adding industrial water into a water metering tank 3, adding the industrial water into an acid preparation kettle 4, slowly adding 98% sulfuric acid while stirring, diluting the 98% sulfuric acid into 90% sulfuric acid, controlling the temperature in the acid preparation kettle 4 at 80 ℃, slowing down the adding rate of the 98% sulfuric acid when the temperature is too high, introducing the prepared 90% sulfuric acid into a sulfuric acid intermediate tank 5, and pumping the prepared 90% sulfuric acid into a 90% sulfuric acid metering tank 6 through a sulfuric acid pump, so as to finish the preparation work of sulfuric acid;
pumping 98% nitric acid into the nitric acid metering tank 10 through a nitric acid pump to finish the preparation work of the nitric acid;
a3, pumping the liquid sulfur dioxide in the liquid sulfur dioxide storage tank 11 into the air temperature type vaporizer 13 through the liquid sulfur dioxide magnetic pump 12, converting the liquid sulfur dioxide into a gas state through heat exchange of the air temperature type vaporizer 13, and conveying the gas state sulfur dioxide to the buffer tank 14 to finish the sulfur dioxide preparation work;
a4, adding 98% sulfuric acid into the reaction kettle 7, stirring, adding nitric acid, starting a circulating pump, stirring for 30min in a circulating way, introducing sulfur dioxide, and controlling the mass ratio of the 98% sulfuric acid to the nitric acid to the sulfur dioxide to be 2.5:1:1, in a concentrated sulfuric acid system, sulfur dioxide directly reacts with nitric acid to prepare nitrososulfuric acid, the reaction releases heat, the temperature in a reaction kettle 7 is controlled to be 80 ℃, the pressure in the reaction kettle 7 is controlled to be 0.1MPa, if the pressure in the reaction kettle 7 is overlarge, the reaction kettle 7 is observed to be cyan and transparent by stopping or reducing the introduction of sulfur dioxide to perform regulation and control, a finished product is pumped into a finished product tank 15 to complete the high-efficiency production of nitrososulfuric acid, the reaction time is 5.5h, and the nitrososulfuric acid content is 41%.
Example 2
A method for producing nitrososulfuric acid with high efficiency, comprising the steps of:
a1, pumping 98% sulfuric acid (commercially available) in a sulfuric acid storage tank 1 into a 98% sulfuric acid metering tank 2 through a sulfuric acid pump, adding industrial water into a water metering tank 3, adding the industrial water into an acid preparation kettle 4, slowly adding 98% sulfuric acid while stirring, diluting the 98% sulfuric acid into 90% sulfuric acid, controlling the temperature in the acid preparation kettle 4 at 90 ℃, slowing down the adding rate of the 98% sulfuric acid when the temperature is too high, introducing the prepared 90% sulfuric acid into a sulfuric acid intermediate tank 5, and pumping the prepared 90% sulfuric acid into a 90% sulfuric acid metering tank 6 through a sulfuric acid pump, so as to finish the preparation work of sulfuric acid;
pumping 98% nitric acid into the nitric acid metering tank 10 through a nitric acid pump to finish the preparation work of the nitric acid;
a3, pumping the liquid sulfur dioxide in the liquid sulfur dioxide storage tank 11 into the air temperature type vaporizer 13 through the liquid sulfur dioxide magnetic pump 12, converting the liquid sulfur dioxide into a gas state through heat exchange of the air temperature type vaporizer 13, and conveying the gas state sulfur dioxide to the buffer tank 14 to finish the sulfur dioxide preparation work;
a4, adding 98% sulfuric acid into the reaction kettle 7, stirring, adding nitric acid, starting a circulating pump, stirring for 30min in a circulating way, introducing sulfur dioxide, and controlling the mass ratio of the 98% sulfuric acid to the nitric acid to the sulfur dioxide to be 2.52:1.02:1, in a concentrated sulfuric acid system, sulfur dioxide directly reacts with nitric acid to prepare nitrososulfuric acid, the reaction releases heat, the temperature in a reaction kettle 7 is controlled to be 85 ℃, the pressure in the reaction kettle 7 is controlled to be 0.12MPa, if the pressure in the reaction kettle 7 is overlarge, the reaction kettle 7 is observed to be cyan and transparent by stopping or reducing the introduction of sulfur dioxide to perform regulation and control, a finished product is pumped into a finished product tank 15 to complete the high-efficiency production of nitrososulfuric acid, the reaction time is 5 hours, and the nitrososulfuric acid content is 42%.
Example 3
A method for producing nitrososulfuric acid with high efficiency, comprising the steps of:
a1, pumping 98% sulfuric acid (commercially available) in a sulfuric acid storage tank 1 into a 98% sulfuric acid metering tank 2 through a sulfuric acid pump, adding industrial water into a water metering tank 3, adding the industrial water into an acid preparation kettle 4, slowly adding 98% sulfuric acid while stirring, diluting the 98% sulfuric acid into 90% sulfuric acid, controlling the temperature in the acid preparation kettle 4 at 100 ℃, slowing down the adding rate of the 98% sulfuric acid when the temperature is too high, introducing the prepared 90% sulfuric acid into a sulfuric acid intermediate tank 5, and pumping the prepared 90% sulfuric acid into a 90% sulfuric acid metering tank 6 through a sulfuric acid pump, so as to finish the preparation work of sulfuric acid;
pumping 98% nitric acid into the nitric acid metering tank 10 through a nitric acid pump to finish the preparation work of the nitric acid;
a3, pumping the liquid sulfur dioxide in the liquid sulfur dioxide storage tank 11 into the air temperature type vaporizer 13 through the liquid sulfur dioxide magnetic pump 12, converting the liquid sulfur dioxide into a gas state through heat exchange of the air temperature type vaporizer 13, and conveying the gas state sulfur dioxide to the buffer tank 14 to finish the sulfur dioxide preparation work;
a4, adding 98% sulfuric acid into the reaction kettle 7, stirring, adding nitric acid, starting a circulating pump, stirring for 30min in a circulating way, introducing sulfur dioxide, and controlling the mass ratio of the 98% sulfuric acid to the nitric acid to the sulfur dioxide to be 2.52:1.02:1, in a concentrated sulfuric acid system, sulfur dioxide directly reacts with nitric acid to prepare nitrososulfuric acid, the reaction releases heat, the temperature in a reaction kettle 7 is controlled to be 95 ℃, the pressure in the reaction kettle 7 is controlled to be 0.15MPa, if the pressure in the reaction kettle 7 is overlarge, the reaction kettle 7 is observed to be cyan and transparent by stopping or reducing the introduction of sulfur dioxide to perform regulation and control, a finished product is pumped into a finished product tank 15 to complete the high-efficiency production of nitrososulfuric acid, the reaction time is 5 hours, and the nitrososulfuric acid content is 42%.
Example 4
Referring to fig. 1, a system for producing nitroso sulfuric acid with high efficiency comprises a sulfuric acid storage tank 1, a 98% sulfuric acid metering tank 2, a water metering tank 3, an acid preparing kettle 4, a sulfuric acid intermediate tank 5, a 90% sulfuric acid metering tank 6, a reaction kettle 7, a tube type heat exchanger 8, a nitric acid storage tank 9, a nitric acid metering tank 10, a liquid sulfur dioxide storage tank 11, a magnetic pump 12, an air temperature type vaporizer 13, a buffer tank 14 and a finished product tank 15;
the sulfuric acid tank 1 is internally provided with commercial 98% sulfuric acid, a discharge port of the sulfuric acid tank 1 is communicated with a feed port of a 98% sulfuric acid metering tank 2, a sulfuric acid pump is arranged on a pipeline between the sulfuric acid tank 1 and the 98% sulfuric acid metering tank 2, the sulfuric acid pump is provided with one standby, continuous operation of the system is guaranteed, the discharge port of the 98% sulfuric acid metering tank 2 is communicated with a feed port on one side of an acid preparation kettle 4, the feed port on the other side of the acid preparation kettle 4 is communicated with a discharge port of a water metering tank, the acid preparation kettle 4 is used for preparing commercial 98% sulfuric acid into 90% sulfuric acid, the discharge port of the acid preparation kettle 4 is communicated with a feed port of a sulfuric acid intermediate tank 5, the sulfuric acid intermediate tank 5 is used for temporarily storing 90% sulfuric acid, the discharge port of the sulfuric acid intermediate tank 5 is communicated with the feed port of the 90% sulfuric acid metering tank 6, the pipeline between the sulfuric acid intermediate tank 5 and the 90% sulfuric acid metering tank 6 is provided with one standby, the sulfuric acid pump is also arranged on the pipeline between the sulfuric acid metering tank 6, the continuous operation of the system is guaranteed, meanwhile, the upper end of the 90% sulfuric acid tank 6 is provided with an exhaust port, the exhaust port is communicated with the feed port of the sulfuric acid metering tank 6 on the intermediate tank 5, and the feed port of the sulfuric acid metering tank 6 is completely communicated with the feed port of the sulfuric acid tank 6.
The discharge gate of nitric acid storage tank 9 communicates with the feed inlet of nitric acid metering tank 10, installs the nitric acid pump on the pipeline between nitric acid storage tank 9 and the nitric acid metering tank 10, and the nitric acid pump sets up one and prepares one, and the discharge gate of nitric acid metering tank 10 communicates with the second feed inlet of reation kettle 7, and the nitric acid pipeline installation is accomplished.
The discharge port of the liquid sulfur dioxide storage tank 11 is communicated with the feed port of the air temperature type vaporizer 13, the air temperature type vaporizer 13 is used for exchanging heat of the liquid sulfur dioxide into gas, a magnetic pump 12 is arranged on a pipeline between the liquid sulfur dioxide storage tank 11 and the air temperature type vaporizer 13, the magnetic pump 12 is provided with a standby device, the discharge port of the air temperature type vaporizer 13 is communicated with the feed port of the buffer tank 14, the buffer tank 14 is used for temporarily storing sulfur dioxide gas, the discharge port of the buffer tank 14 is communicated with one side feed port of the shell and tube heat exchanger 8, the other side feed port of the shell and tube heat exchanger 8 is communicated with one side feed port of the reaction kettle 7, the other side feed port of the reaction kettle 7 is communicated with the feed port of the finished product tank 15, and the discharge port of the shell and tube heat exchanger 8 is communicated with the third feed port of the reaction kettle 7. The shell and tube heat exchanger 8 firstly reduces the temperature of the materials in the reaction kettle 7, and meanwhile, the shell and tube heat exchanger 8 can promote the circulation flow of the materials, improve the contact efficiency of sulfur dioxide and nitric acid, and achieve the purpose of improving the reaction efficiency.
The sulfuric acid storage tank 1, the 98% sulfuric acid metering tank 2, the water metering tank 3, the acid preparing kettle 4, the sulfuric acid intermediate tank 5, the 90% sulfuric acid metering tank 6, the reaction kettle 7, the tubular heat exchanger 8, the nitric acid storage tank 9, the nitric acid metering tank 10, the liquid sulfur dioxide storage tank 11, the magnetic pump 12, the buffer tank 14 and the finished product tank 15 are all provided with waste gas ports, and the waste gas ports are communicated with a plant area tail gas absorbing device.
The outer sides of the acid preparation kettle 4 and the reaction kettle 7 are provided with jackets, circulating water is introduced into the jackets, and the circulating water is used for cooling the kettle body.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (8)
1. A method for producing nitrososulfuric acid with high efficiency, comprising the steps of:
a1, pumping 98% sulfuric acid in a sulfuric acid storage tank (1) into a 98% sulfuric acid metering tank (2) through a sulfuric acid pump, adding industrial water into a water metering tank (3), adding industrial water into an acid preparation kettle (4), slowly adding 98% sulfuric acid while stirring, diluting 98% sulfuric acid into 90% sulfuric acid, controlling the temperature in the acid preparation kettle (4) to be 80-100 ℃, slowing down the adding rate of 98% sulfuric acid when the temperature is too high, pumping the prepared 90% sulfuric acid into a sulfuric acid intermediate tank (5), and pumping the prepared 90% sulfuric acid into a 90% sulfuric acid metering tank (6) through a sulfuric acid pump, so as to finish the preparation work of sulfuric acid;
pumping 98% nitric acid into a nitric acid metering tank (10) through a nitric acid pump to finish the preparation work of the nitric acid;
a3, pumping the liquid sulfur dioxide in the liquid sulfur dioxide storage tank (11) into an air temperature type vaporizer (13) through a liquid sulfur dioxide magnetic pump (12), converting the liquid sulfur dioxide into a gas state through heat exchange of the air temperature type vaporizer (13), and conveying the gas state sulfur dioxide to a buffer tank (14) to finish sulfur dioxide preparation work;
a4, adding 90% sulfuric acid into the reaction kettle (7), stirring, adding nitric acid, starting a circulating pump, stirring for 30min in a circulating way, introducing sulfur dioxide, and controlling the mass ratio of the 90% sulfuric acid to the nitric acid to the sulfur dioxide to be 2.5-2.52:1-1.02:1, controlling the temperature in the reaction kettle (7) to be 80-95 ℃, controlling the pressure in the reaction kettle (7) to be 0.1-0.15MPa, if the pressure in the reaction kettle (7) is overlarge, regulating and controlling by stopping or reducing the introduction of sulfur dioxide, observing that the materials in the reaction kettle (7) are cyan and transparent, namely, the reaction is completed, pumping a finished product into a finished product tank (15), and completing the high-efficiency production of nitroso sulfuric acid.
2. A method for producing nitrososulfuric acid with high efficiency according to claim 1, wherein the mass ratio of 90% sulfuric acid, nitric acid and sulfur dioxide in step A4 is 2.52:1.02:1.
3. a method for producing nitrososulfuric acid with high efficiency according to claim 1, wherein the temperature in the reaction vessel (7) in step A4 is 85 ℃.
4. The method for producing nitrososulfuric acid according to claim 1, wherein the pressure in the reaction vessel (7) in the step A4 is 0.12MPa.
5. A system for implementing a method for producing nitrososulfuric acid with high efficiency according to claim 1, characterized by comprising a sulfuric acid tank (1), a 98% sulfuric acid metering tank (2), a water metering tank (3), an acid preparing tank (4), a sulfuric acid intermediate tank (5), a 90% sulfuric acid metering tank (6), a reaction tank (7), a shell and tube heat exchanger (8), a nitric acid tank (9), a nitric acid metering tank (10), a liquid sulfur dioxide tank (11), a magnetic pump (12), an air temperature vaporizer (13), a buffer tank (14) and a finished product tank (15);
the sulfuric acid tank is characterized in that commercial 98% sulfuric acid is arranged in the sulfuric acid tank (1), a discharge port of the sulfuric acid tank (1) is communicated with a feed port of a 98% sulfuric acid metering tank (2), a sulfuric acid pump is arranged on a pipeline between the sulfuric acid tank (1) and the 98% sulfuric acid metering tank (2), the discharge port of the 98% sulfuric acid metering tank (2) is communicated with a feed port on one side of an acid distribution kettle (4), the feed port on the other side of the acid distribution kettle (4) is communicated with a feed port of a water metering tank, the feed port of the acid distribution kettle (4) is communicated with a feed port of a sulfuric acid intermediate tank (5), the feed port of the sulfuric acid intermediate tank (5) is communicated with a feed port of a 90% sulfuric acid metering tank (6), a sulfuric acid pump is arranged on a pipeline between the sulfuric acid intermediate tank (5) and the 90% sulfuric acid metering tank (6), an exhaust port is formed in the upper end of the 90% sulfuric acid metering tank (6), the exhaust port is communicated with the upper end of the sulfuric acid intermediate tank (5), and the discharge port of the 90% sulfuric acid metering tank (6) is communicated with a first pipeline of the reaction kettle (7);
the discharge port of the nitric acid storage tank (9) is communicated with the feed port of the nitric acid metering tank (10), a nitric acid pump is arranged on a pipeline between the nitric acid storage tank (9) and the nitric acid metering tank (10), the discharge port of the nitric acid metering tank (10) is communicated with the second feed port of the reaction kettle (7), and the nitric acid pipeline is completely arranged;
the discharge port of the liquid sulfur dioxide storage tank (11) is communicated with the feed port of the air temperature type vaporizer (13), a magnetic pump (12) is arranged on a pipeline between the liquid sulfur dioxide storage tank (11) and the air temperature type vaporizer (13), the discharge port of the air temperature type vaporizer (13) is communicated with the feed port of the buffer tank (14), the discharge port of the buffer tank (14) is communicated with one side feed port of the shell and tube heat exchanger (8), the other side feed inlet of shell and tube heat exchanger (8) communicates with one side discharge gate of reation kettle (7), the opposite side discharge gate of reation kettle (7) communicates with the feed inlet of finished product jar (15), the discharge gate of shell and tube heat exchanger (8) communicates with the third feed inlet of reation kettle (7), the sulfur dioxide pipeline installation is accomplished.
6. The system according to claim 5, characterized in that the sulfuric acid pump, the nitric acid pump and the magnetic pump (12) are each provided with a backup.
7. The system according to claim 5, wherein the outside of the acid preparing kettle (4) and the outside of the kettle body of the reaction kettle (7) are provided with jackets, and circulating water is introduced into the jackets.
8. The system of claim 5, wherein the sulfuric acid storage tank (1), the 98% sulfuric acid metering tank (2), the water metering tank (3), the acid preparing kettle (4), the sulfuric acid intermediate tank (5), the 90% sulfuric acid metering tank (6), the reaction kettle (7), the shell and tube heat exchanger (8), the nitric acid storage tank (9), the nitric acid metering tank (10), the liquid sulfur dioxide storage tank (11), the magnetic pump (12), the buffer tank (14) and the finished product tank (15) are all provided with waste gas ports, and the waste gas ports are communicated with the plant tail gas absorbing device.
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Denomination of invention: A Method and System for Efficient Production of Nitrososulfuric Acid Effective date of registration: 20230918 Granted publication date: 20230620 Pledgee: Lai An county Jinan financing Company limited by guarantee Pledgor: Anhui Haihui Chemical Co.,Ltd. Registration number: Y2023980057185 |
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