CN115463519A - Method and system for efficiently producing nitroso-sulfuric acid - Google Patents
Method and system for efficiently producing nitroso-sulfuric acid Download PDFInfo
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Abstract
The invention relates to a method and a system for efficiently producing nitroso-sulfuric acid, belonging to the technical field of chemical production, wherein the method for producing the 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: the method comprises the following steps of 1, controlling the temperature in a reaction kettle to be 80-95 ℃ and the pressure to be 0.1-0.15MPa, observing that materials in the reaction kettle are cyan and transparent, namely, the reaction is finished, additionally arranging a tubular heat exchanger in a nitroso-sulfuric acid production system for cooling, wherein the tubular heat exchanger is high in heat exchange speed, and is beneficial to promoting the reaction efficiency and shortening the reaction time.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a method and a system for efficiently producing nitroso-sulfuric acid.
Background
The nitroso sulfuric acid is mainly used for replacing sodium nitrite in the diazo reaction of the disperse dye, thereby reducing the cost, improving the product quality and being widely applied to the fields of pesticides and medicines.
The invention patent CN106379875B discloses a production method and application of nitroso sulfuric acid, and the production method disclosed in the invention is as follows: 1. heating and dehydrating waste acid generated by diazotizing and deaminating 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. mixing waste gas generated by the chloronitro reaction of nitrobenzene compounds with air, introducing the mixture into a mixed acid spray tower for absorption, and directly pumping nitroso sulfuric acid prepared in the spray tower into a nitroso sulfuric acid storage tank after the nitroso sulfuric acid is detected to be qualified.
In response to increasing production demands, the most common process for the production of nitrososulfuric acid is: absorption method of concentrated nitric acid sulfur dioxide gas (SO for short) 2 Absorption method) in which concentrated sulfuric acid is used as a medium, sulfur dioxide gas and concentrated nitric acid are directly reacted to obtain nitroso-sulfuric acid, but the method has a complex process and low production efficiency, so that the production time is long, generally 12-24h is required, 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 present invention aims to provide a method and a system for producing nitroso-sulfuric acid with high efficiency.
The purpose of the invention can be realized by the following technical scheme:
a method for producing nitroso-sulfuric acid with high efficiency comprises the following steps:
a1, pumping 98% sulfuric acid (sold in the market) 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 the 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 addition 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 the sulfuric acid pump to finish the preparation work of the sulfuric acid;
pumping A2 and 98 percent nitric acid into a nitric acid metering tank through a nitric acid pump to finish the preparation work of the nitric acid;
a3, pumping liquid sulfur dioxide in the liquid sulfur dioxide storage tank into an air-temperature vaporizer through a liquid sulfur dioxide magnetic pump, converting the liquid sulfur dioxide into a gaseous state through heat exchange of the air-temperature vaporizer, and conveying the gaseous sulfur dioxide to a buffer tank to finish sulfur dioxide preparation work;
a4, adding 98% sulfuric acid into a reaction kettle, stirring and adding nitric acid, starting a circulating pump, circularly stirring for 30min, 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, directly reacting sulfur dioxide with nitric acid to prepare nitroso-sulfuric acid, releasing heat in the reaction, controlling the temperature in a reaction kettle to be 80-95 ℃, controlling the pressure in the reaction kettle to be 0.1-0.15MPa, if the pressure in the reaction kettle is too high, regulating and controlling by stopping or reducing the introduction of sulfur dioxide, observing that materials in the reaction kettle are cyan and transparent, namely the reaction is finished, and pumping finished products into a finished product tank to finish the high-efficiency production of the nitroso-sulfuric acid.
In the production process, the reaction principle is as follows:
SO 2 +HNO 3 ＝＝NOHSO 4
wherein, concentrated sulfuric acid provides a reaction system environment.
Further, in the step A4, the mass ratio of the 98% sulfuric acid to the nitric acid to the sulfur dioxide is 2.52:1.02:1.
further, the temperature in the reaction vessel in step A4 was 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 preparation kettle, a sulfuric acid intermediate tank, a 90% sulfuric acid metering tank, a reaction kettle, a tubular heat exchanger, a nitric acid storage tank, a nitric acid metering tank, a liquid sulfur dioxide storage tank, a magnetic pump, an air-temperature vaporizer, a buffer tank and a finished product tank;
the sulfuric acid storage tank is internally provided with 98% sulfuric acid sold in the market, a discharge port of the sulfuric acid storage tank is communicated with a feed port of the 98% sulfuric acid metering tank, a sulfuric acid pump is installed on a pipeline between the sulfuric acid storage tank and the 98% sulfuric acid metering tank, a discharge port of the 98% sulfuric acid metering tank is communicated with a feed port on one side of the acid preparation kettle, a feed port on the other side of the acid preparation kettle is communicated with a discharge port of the water metering tank, the acid preparation kettle is used for preparing the 98% sulfuric acid sold in the market into 90% sulfuric acid, the discharge port of the acid preparation kettle is communicated with a feed port of the sulfuric acid intermediate tank, the sulfuric acid intermediate tank is used for temporarily storing the 90% sulfuric acid, the discharge port of the sulfuric acid intermediate tank is communicated with the feed port of the 90% sulfuric acid metering tank, the sulfuric acid pump is installed on a pipeline between the sulfuric acid intermediate tank and the 90% sulfuric acid metering tank, meanwhile, an exhaust port is formed in the upper end of the 90% sulfuric acid metering tank and is communicated with the upper end of the sulfuric acid intermediate tank, the discharge port of the 90% sulfuric acid metering tank is communicated with the first feed port of the reaction kettle, and the sulfuric acid pipeline is installed, and the sulfuric acid is installed completely.
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 installation finishes.
The discharge gate of liquid sulfur dioxide storage tank and the feed inlet intercommunication of empty warm formula vaporizer, empty warm formula vaporizer is used for becoming the gaseous state with liquid sulfur dioxide heat transfer, install the magnetic drive pump on the pipeline between liquid sulfur dioxide storage tank and the empty warm formula vaporizer, the discharge gate of empty warm formula vaporizer and the feed inlet intercommunication of buffer tank, the buffer tank is used for keeping in sulfur dioxide gas, the discharge gate of buffer tank and one side feed inlet intercommunication of shell and tube heat exchanger, the opposite side feed inlet of shell and tube heat exchanger and one side discharge gate intercommunication of reation kettle, reation kettle's the opposite side discharge gate and the feed inlet intercommunication of finished product jar, the discharge gate of shell and tube heat exchanger and reation kettle's third feed inlet intercommunication, sulfur dioxide pipe erection finishes. The tube type heat exchanger is used for reducing the temperature of materials in the reaction kettle.
Furthermore, the sulfuric acid pump, the nitric acid pump and the magnetic pump are all provided with one standby for use, so that the continuous operation of the system is ensured.
Further, the outer sides of the kettle bodies of the acid preparation kettle and the reaction kettle are provided with clamping sleeves, circulating water is introduced into the clamping sleeves, and the circulating water is used for cooling the kettle bodies.
Further, waste gas ports are formed in the sulfuric acid storage tank, the 98% sulfuric acid metering tank, the water metering tank, the acid preparation 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, and the waste gas ports are communicated with the plant tail gas absorption device.
The invention has the beneficial effects that:
the method comprises the following steps of firstly, reacting sulfur dioxide with concentrated nitric acid to prepare nitroso-sulfuric acid, wherein a refrigerating device is usually additionally arranged in the traditional process, the method adopts an additionally arranged tubular heat exchanger as a reaction kettle cooling treatment device, the tubular heat exchanger has high heat exchange speed, can timely carry away reaction heat, greatly promotes reaction efficiency, shortens reaction time, and simultaneously can promote the circulating flow of materials, improve the contact efficiency of sulfur dioxide and nitric acid and achieve the purpose of improving the reaction efficiency.
Then, the invention improves the reaction temperature during production, the temperature is controlled below 70 ℃ during production of the traditional process, the most preferable scheme in the invention controls the temperature to be 85 ℃, and the reaction efficiency is improved, namely the reaction time is reduced.
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 used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a system for producing nitroso-sulfuric acid with high efficiency according to the present invention.
In the drawings, the components represented by the respective reference numerals are listed below:
1. a sulfuric acid storage tank; 2. a 98% sulfuric acid metering tank; 3. a water metering tank; 4. preparing an acid 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 vaporizer; 14. a buffer tank; 15. and (5) a finished product can.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for producing nitroso-sulfuric acid with high efficiency comprises the following steps:
a1, pumping 98% sulfuric acid (sold in the market) 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 the 98% sulfuric acid while stirring, diluting the 98% sulfuric acid into 90% sulfuric acid, controlling the temperature in the acid preparation kettle 4 to be 80 ℃, slowing down the addition 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 the sulfuric acid pump to finish the preparation work of the sulfuric acid;
pumping A2 and 98 percent 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 vaporizer 13 through a liquid sulfur dioxide magnetic pump 12, converting the liquid sulfur dioxide into a gaseous state through the heat exchange of the air-temperature vaporizer 13, and conveying the gaseous sulfur dioxide to a buffer tank 14 to finish the sulfur dioxide preparation work;
a4, adding 98% sulfuric acid into a reaction kettle 7, stirring and adding nitric acid, starting a circulating pump, circularly stirring for 30min, 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, directly reacting sulfur dioxide with nitric acid to prepare nitroso-sulfuric acid, releasing heat in the reaction, controlling the temperature in a reaction kettle 7 to be 80 ℃, controlling the pressure in the reaction kettle 7 to be 0.1MPa, if the pressure in the reaction kettle 7 is too high, regulating and controlling by stopping or reducing the introduction of sulfur dioxide, observing that materials in the reaction kettle 7 are cyan and transparent, namely the reaction is finished, pumping a finished product into a finished product tank 15, finishing the high-efficiency production of the nitroso-sulfuric acid, wherein the reaction time is 5.5 hours, and the content of the nitroso-sulfuric acid is 41%.
Example 2
A method for producing nitroso-sulfuric acid with high efficiency comprises the following steps:
a1, pumping 98% sulfuric acid (sold in the market) 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 the 98% sulfuric acid while stirring, diluting the 98% sulfuric acid into 90% sulfuric acid, controlling the temperature in the acid preparation kettle 4 to be 90 ℃, slowing down the addition 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 the sulfuric acid pump to finish the preparation work of the sulfuric acid;
pumping A2 and 98 percent 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 vaporizer 13 through a liquid sulfur dioxide magnetic pump 12, converting the liquid sulfur dioxide into a gaseous state through the heat exchange of the air-temperature vaporizer 13, and conveying the gaseous sulfur dioxide to a buffer tank 14 to finish the sulfur dioxide preparation work;
a4, adding 98% sulfuric acid into a reaction kettle 7, stirring and adding nitric acid, starting a circulating pump, circularly stirring for 30min, 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: in a concentrated sulfuric acid system, sulfur dioxide directly reacts with nitric acid to prepare nitroso-sulfuric 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 too high, the introduction of sulfur dioxide is stopped or reduced for regulation and control, the reaction is finished when materials in the reaction kettle 7 are observed to be cyan and transparent, finished products are pumped into a finished product tank 15, the high-efficiency production of the nitroso-sulfuric acid is finished, the reaction time is 5 hours, and the content of the nitroso-sulfuric acid is 42%.
Example 3
A method for producing nitroso-sulfuric acid with high efficiency comprises the following steps:
a1, pumping 98% sulfuric acid (sold in the market) 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 the 98% sulfuric acid while stirring, diluting the 98% sulfuric acid into 90% sulfuric acid, controlling the temperature in the acid preparation kettle 4 to be 100 ℃, slowing down the addition 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 the sulfuric acid pump to finish the preparation work of the sulfuric acid;
pumping A2 and 98 percent 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 vaporizer 13 through a liquid sulfur dioxide magnetic pump 12, converting the liquid sulfur dioxide into a gaseous state through the heat exchange of the air-temperature vaporizer 13, and conveying the gaseous sulfur dioxide to a buffer tank 14 to finish the sulfur dioxide preparation work;
a4, adding 98% sulfuric acid into a reaction kettle 7, stirring and adding nitric acid, starting a circulating pump, circularly stirring for 30min, 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, directly reacting sulfur dioxide with nitric acid to prepare nitroso-sulfuric acid, releasing heat in the reaction, controlling the temperature in a reaction kettle 7 to be 95 ℃, controlling the pressure in the reaction kettle 7 to be 0.15MPa, if the pressure in the reaction kettle 7 is too high, regulating and controlling by stopping or reducing the introduction of sulfur dioxide, observing that materials in the reaction kettle 7 are cyan and transparent, namely the reaction is finished, pumping a finished product into a finished product tank 15, finishing the high-efficiency production of the nitroso-sulfuric acid, wherein the reaction time is 5 hours, and the content of the nitroso-sulfuric acid is 42%.
Example 4
Referring to fig. 1, a system for producing nitroso-sulfuric acid with high efficiency includes a sulfuric acid storage tank 1, a 98% sulfuric acid metering tank 2, a water metering tank 3, an acid preparation kettle 4, a sulfuric acid intermediate tank 5, a 90% sulfuric acid metering tank 6, a reaction kettle 7, a tubular 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 vaporizer 13, a buffer tank 14 and a finished product tank 15;
the sulfuric acid storage tank 1 is internally provided with 98% of commercially available sulfuric acid, a discharge port of the sulfuric acid storage tank 1 is communicated with a feed port of the 98% sulfuric acid metering tank 2, a sulfuric acid pump is arranged on a pipeline between the sulfuric acid storage tank 1 and the 98% sulfuric acid metering tank 2 and is used for preparing one standby sulfuric acid, so that the continuous operation of the system is guaranteed, a discharge port of the 98% sulfuric acid metering tank 2 is communicated with a feed port on one side of the acid preparation kettle 4, a feed port on the other side of the acid preparation kettle 4 is communicated with a discharge port of the water metering tank, the acid preparation kettle 4 is used for preparing the 98% of commercially available sulfuric acid into 90% sulfuric acid, a discharge port of the acid preparation kettle 4 is communicated with a feed port of the sulfuric acid intermediate tank 5, the sulfuric acid intermediate tank 5 is used for temporarily storing the 90% sulfuric acid, a discharge port of the sulfuric acid intermediate tank 5 is communicated with a feed port of the 90% sulfuric acid metering tank 6, the sulfuric acid pump is arranged on a pipeline between the sulfuric acid intermediate tank 5 and the 90% sulfuric acid metering tank 6, the sulfuric acid pump is also provided with a standby one standby for use so as to guarantee the continuous operation of the system, meanwhile, an exhaust port is arranged at the upper end of the 90% sulfuric acid metering tank 6, the upper end of the sulfuric acid metering tank 5 is communicated with an upper end of the sulfuric acid metering tank, a discharge port, the sulfuric acid metering tank 6, a discharge port is communicated with a first reaction pipeline 7 of the sulfuric acid metering tank 6, and is arranged, and is communicated with a first reaction kettle, and is communicated with a discharge port of the sulfuric acid metering tank 6, and is arranged on the sulfuric acid metering tank 7 of the sulfuric acid metering tank 6, and is communicated with a reaction kettle, and is arranged, and is communicated with a reaction kettle.
The discharge gate of nitric acid storage tank 9 and the feed inlet of nitric acid metering tank 10 communicate, install the nitric acid pump on the pipeline between nitric acid storage tank 9 and the nitric acid metering tank 10, the nitric acid pump sets up one and is equipped with one and use, the discharge gate of nitric acid metering tank 10 and the second feed inlet of reation kettle 7 communicate, and the installation of nitric acid pipeline finishes.
The discharge gate of liquid sulfur dioxide storage tank 11 and the feed inlet of empty temperature formula vaporizer 13 communicate, empty temperature formula vaporizer 13 is used for becoming the gaseous state with liquid sulfur dioxide heat transfer, install magnetic drive pump 12 on the pipeline between liquid sulfur dioxide storage tank 11 and the empty temperature formula vaporizer 13, magnetic drive pump 12 sets up one and uses one, the discharge gate of empty temperature formula vaporizer 13 and the feed inlet of buffer tank 14 communicate, buffer tank 14 is used for keeping in sulfur dioxide gas, the discharge gate of buffer tank 14 and one side feed inlet of shell and tube heat exchanger 8 communicate, the opposite side feed inlet of shell and tube heat exchanger 8 and one side discharge gate of reation kettle 7 communicate, the opposite side discharge gate of reation kettle 7 and the feed inlet of finished product jar 15 communicate, the discharge gate of shell and tube heat exchanger 8 and the third feed inlet of reation kettle 7 communicate, sulfur dioxide pipeline installation finishes. The effect of shell and tube heat exchanger 8 is at first the temperature of material in reduction reation kettle 7, simultaneously, sets up shell and tube heat exchanger 8 and can promote the circulation flow of material, improves the contact efficiency of sulfur dioxide and nitric acid, realizes improving reaction efficiency's purpose.
Waste gas ports are formed in the sulfuric acid storage tank 1, the 98% sulfuric acid metering tank 2, the water metering tank 3, the acid preparation 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, and the waste gas ports are communicated with a plant tail gas absorption device.
The outer sides of the kettle bodies of the acid preparation kettle 4 and the reaction kettle 7 are provided with clamping sleeves, circulating water is introduced into the clamping sleeves, and the circulating water is used for cooling the kettle bodies.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to 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 invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. 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 exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (8)
1. A method for efficiently producing nitrososulfuric acid, which is characterized by comprising the following steps:
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 the industrial water into an acid preparation kettle (4), slowly adding the 98% sulfuric acid while stirring, diluting the 98% sulfuric acid into 90% sulfuric acid, controlling the temperature in the acid preparation kettle (4) to be 80-100 ℃, slowing down the addition 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 the sulfuric acid pump to finish preparation work of the sulfuric acid;
pumping A2 and 98 percent 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 vaporizer (13) through a liquid sulfur dioxide magnetic pump (12), converting the liquid sulfur dioxide into a gaseous state through the heat exchange of the air-temperature vaporizer (13), and conveying the gaseous sulfur dioxide to a buffer tank (14) to finish the sulfur preparation work of the dioxide;
a4, adding 98% sulfuric acid into a reaction kettle (7), stirring and adding nitric acid, starting a circulating pump, circularly stirring for 30min, 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: 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 too high, 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 finishing the reaction, and pumping finished products into a finished product tank (15) to finish the high-efficiency production of the nitroso-sulfuric acid.
2. A method for producing nitroso-sulfuric acid with high efficiency according to claim 1, wherein the mass ratio of the 98% 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 kettle (7) in step A4 is 85 ℃.
4. A method for producing nitroso-sulfuric acid with high efficiency according to claim 1, wherein the pressure in the reaction tank (7) in step A4 is 0.12MPa.
5. A system for producing nitroso-sulfuric acid with high efficiency is characterized by comprising a sulfuric acid storage tank (1), a 98% sulfuric acid metering tank (2), a water metering tank (3), an acid preparation 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 vaporizer (13), a buffer tank (14) and a finished product tank (15);
the sulfuric acid storage tank (1) is internally provided with 98% of commercially available sulfuric acid, a discharge port of the sulfuric acid storage tank (1) is communicated with a feed port of the 98% sulfuric acid metering tank (2), a sulfuric acid pump is installed on a pipeline between the sulfuric acid storage tank (1) and the 98% sulfuric acid metering tank (2), a discharge port of the 98% sulfuric acid metering tank (2) is communicated with a feed port on one side of the acid preparation kettle (4), a feed port on the other side of the acid preparation kettle (4) is communicated with a discharge port of the water metering tank, a discharge port of the acid preparation kettle (4) is communicated with a feed port of the sulfuric acid intermediate tank (5), a discharge port of the sulfuric acid intermediate tank (5) is communicated with a feed port of the 90% sulfuric acid metering tank (6), a sulfuric acid pump is installed on a pipeline between the sulfuric acid intermediate tank (5) and the 90% sulfuric acid metering tank (6), meanwhile, 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), a discharge port of the 90% sulfuric acid metering tank (6) is communicated with a feed port of the reaction kettle (7), and a sulfuric acid pipeline is installed completely.
The discharge gate of nitric acid storage tank (9) and the feed inlet of nitric acid metering tank (10) communicate, install the nitric acid pump on the pipeline between nitric acid storage tank (9) and nitric acid metering tank (10), the discharge gate of nitric acid metering tank (10) and the second feed inlet of reation kettle (7) communicate, and the nitric acid pipe-line installation finishes.
The discharge gate of liquid sulfur dioxide storage tank (11) and the feed inlet intercommunication of empty warm formula vaporizer (13), install magnetic drive pump (12) on the pipeline between liquid sulfur dioxide storage tank (11) and empty warm formula vaporizer (13), the discharge gate of empty warm formula vaporizer (13) and the feed inlet intercommunication of buffer tank (14), the discharge gate of buffer tank (14) and one side feed inlet intercommunication of shell and tube heat exchanger (8), the opposite side feed inlet of shell and tube heat exchanger (8) and one side discharge gate intercommunication of reation kettle (7), the opposite side discharge gate of reation kettle (7) and the feed inlet intercommunication of finished product jar (15), the discharge gate of shell and tube heat exchanger (8) and the third feed inlet intercommunication of reation kettle (7), sulfur dioxide pipe erection finishes.
6. A system for the efficient production of nitroso-sulfuric acid according to claim 5, wherein the sulfuric acid pump, nitric acid pump and magnetic pump (12) are provided for one use.
7. A system for producing nitroso-sulfuric acid with high efficiency according to claim 5, wherein the acid preparation kettle (4) and the reaction kettle (7) are provided with jackets at the outer sides of the kettle bodies, and circulating water is introduced into the jackets.
8. The system for producing nitroso-sulfuric acid with high efficiency according to claim 5, wherein the sulfuric acid storage tank (1), the 98% sulfuric acid metering tank (2), the water metering tank (3), the acid preparation 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 tail gas absorption device.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105536478A (en) * | 2016-01-16 | 2016-05-04 | 浙江奇彩环境科技股份有限公司 | Resourceful treatment method and system for H acid production tail gas |
| CN107963617A (en) * | 2017-12-28 | 2018-04-27 | 浙江迪邦化工有限公司 | The production method and system of a kind of nitrosyl sulfuric acid |
| CN111268657A (en) * | 2020-01-22 | 2020-06-12 | 浙江迪邦化工有限公司 | Method and system for continuously producing nitrosyl sulfuric acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105536478A (en) * | 2016-01-16 | 2016-05-04 | 浙江奇彩环境科技股份有限公司 | Resourceful treatment method and system for H acid production tail gas |
| CN107963617A (en) * | 2017-12-28 | 2018-04-27 | 浙江迪邦化工有限公司 | The production method and system of a kind of nitrosyl sulfuric acid |
| CN111268657A (en) * | 2020-01-22 | 2020-06-12 | 浙江迪邦化工有限公司 | Method and system for continuously producing nitrosyl sulfuric acid |
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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 |