CN112479245B - Preparation method of indium nitrate solution - Google Patents
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- CN112479245B CN112479245B CN202011472447.0A CN202011472447A CN112479245B CN 112479245 B CN112479245 B CN 112479245B CN 202011472447 A CN202011472447 A CN 202011472447A CN 112479245 B CN112479245 B CN 112479245B
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Abstract
The invention discloses a preparation method of an indium nitrate solution, which comprises the following steps: putting pure water into a reaction kettle; adding indium ingots into the pure water, and then replacing air in the kettle with oxygen to keep the pressure in the kettle between 0.1MPa and 0.15 MPa; heating to 80-98 ℃, adjusting the temperature of the reaction kettle to be constant, and continuously adding concentrated nitric acid into the reaction kettle to perform reaction for the first time; and after the first time, continuously introducing oxygen into the kettle to keep the pressure in the kettle between 0.16MPa and 0.25MPa, and carrying out reaction for a second time to obtain the indium nitrate solution. The method for preparing the indium nitrate solution has the advantages of less nitrogen oxides generated in the process of preparing the indium nitrate solution, simple preparation process and low acid consumption, and simultaneously, a small amount of generated nitrogen oxides can be directly discharged into the air after being absorbed by water, so that the tail gas treatment cost is reduced, the method is environment-friendly, and in addition, the dilute nitric acid solution generated after the nitrogen oxides are absorbed by the water can be recycled in a certain treatment mode.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a preparation method of an indium nitrate solution.
Background
Nitrate is an important chemical material, and is generally obtained by reacting metal with nitric acid, for example, indium nitrate can be obtained by dissolving indium metal with nitric acid, but a large amount of nitrogen oxide gas is generated in the process of dissolving indium metal with nitric acid, so that not only a large amount of nitric acid is wasted, but also the cost is increased by the treatment of nitrogen oxide in the later period, and certain influence is brought to the environment.
There are three main methods currently used to treat nitrogen oxide emissions during nitrate production: the first method is to absorb and treat nitrogen oxides generated by preparing indium nitrate by sodium thiosulfate and sodium hydroxide solution, but the method has high cost for treating the nitrogen oxides and can bring waste treatment cost; the second method is to reduce the generation of nitrogen oxides in the reaction process in the process of preparing nitrates, and the Chinese patent application CN97107236.1 with the application date of 1997, 12, 16 discloses that zeolite molecular sieves modified by sodium hydroxide and nitric acid are added in the process of preparing nitrates by dissolving nitric acid, oxygen-enriched air or oxygen is introduced, the pressure of a reaction kettle is controlled to be-0.04 MPa-0.11 MPa, the reaction is carried out for 4 hours at the temperature of 60 ℃, tail gas is absorbed by a water-sealed tank and an absorption tower, so that the discharge amount of nitrogen oxides is greatly reduced, but the method needs to add zeolite molecular sieve catalysts, so that the process is complex and the cost is high; the third method is to quench indium into indium flower, add into nitrate mother liquor, add concentrated nitric acid for reaction, introduce air to dilute the produced nitrogen oxide at the same time, introduce the end gas into water to absorb, this method has high requirements for indium flower specific surface area, and need to introduce a large amount of air to dilute the nitrogen oxide, only suitable for few batch productions, can't realize industrialization.
In view of the defects of the prior art, the invention provides a preparation method of an indium nitrate solution.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of an indium nitrate solution.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides a preparation method of an indium nitrate solution, which comprises the following steps: putting pure water into a reaction kettle; adding indium ingots into the pure water, and replacing air in the kettle with oxygen to keep the pressure in the kettle between 0.1MPa and 0.15 MPa; heating to 80-98 ℃, adjusting the temperature of the reaction kettle to be constant, and continuously adding concentrated nitric acid into the reaction kettle to perform reaction for the first time; and after the first time, continuously introducing oxygen into the kettle to keep the pressure in the kettle between 0.16MPa and 0.25MPa, and carrying out reaction for a second time to obtain the indium nitrate solution.
As a further improvement of the invention, the molar ratio of the concentrated nitric acid to the indium ingot is 2.
As a further improvement of the invention, the first time is 6-6.5 h.
As a further improvement of the invention, the second time is 6h to 6.2h.
As a further improvement of the invention, oxygen is continuously introduced into the kettle to keep the pressure in the kettle between 0.24MPa and 0.25 MPa.
In a further improvement of the present invention, the mass fraction of the concentrated nitric acid is 65% or more.
As a further improvement of the invention, the adding speed of the concentrated nitric acid is 140 mL/h-160 mL/h.
As a further improvement of the invention, the purity of the oxygen is more than or equal to 99.9 percent.
As a further improvement of the invention, when the concentrated nitric acid is added into the reaction kettle, the temperature of the reaction kettle is controlled between 80 ℃ and 98 ℃.
As a further improvement of the invention, the temperature of the reaction kettle is controlled between 96 ℃ and 98 ℃.
The invention provides a preparation method of an indium nitrate solution, which is characterized in that nitrogen oxides generated in the process of preparing the indium nitrate solution are less, the preparation process is simple, the acid consumption is less, a small amount of generated nitrogen oxides can be directly discharged into the air after being absorbed by water, the tail gas treatment cost is reduced, the environment is friendly, and in addition, a dilute nitric acid solution generated after the nitrogen oxides are absorbed by the water can be recycled in a certain treatment mode.
Detailed Description
The technical solutions will be clearly and completely described below with reference to 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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides a preparation method of an indium nitrate solution, which has the following reaction principle:
In+6HNO 3 →In（NO 3 ） 3 +3NO 2 ↑+3H 2 O；
3NO 2 +H 2 O→2HNO 3 +NO；
4NO+3O 2 +2H 2 O→4HNO 3 。
the method for preparing the indium nitrate solution comprises the following steps:
s1, taking pure water and placing the pure water in a reaction kettle.
S2, adding indium ingots into pure water, and replacing air in the kettle with oxygen to keep the pressure in the kettle between 0.1MPa and 0.15 MPa.
And S3, heating to 80-98 ℃, adjusting the temperature of the reaction kettle to be constant, adding concentrated nitric acid with the mass fraction of more than or equal to 65% into the reaction kettle at the speed of 140-160 mL/h, and carrying out the reaction for 6-6.5 h.
And S4, after the first time, continuously introducing oxygen with the purity of more than or equal to 99.9% into the kettle, keeping the pressure in the kettle between 0.16MPa and 0.25MPa, and carrying out reaction for 6-6.2 h to obtain the indium nitrate solution.
In the process of preparing the indium nitrate solution, the molar ratio of the added concentrated nitric acid to the indium ingot is 2.
In the process of preparing the indium nitrate solution, oxygen is continuously introduced into the kettle in the reaction process, so that the pressure in the kettle is preferably kept between 0.24MPa and 0.25 MPa.
In the process of preparing the indium nitrate solution, the temperature of the reaction kettle is controlled between 80 ℃ and 98 ℃, preferably between 96 ℃ and 98 ℃ in the process of adding the concentrated nitric acid into the reaction kettle for reaction.
For further understanding of the present invention, the method and effects of the present invention will be described in further detail with reference to specific examples. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
Example 1.
(1) Configuration 1.6m 3 Adding pure water into the reaction kettle;
(2) Adding 500kg indium ingots into pure water, and filling oxygen into a reaction kettle to replace air in the kettle, so that the pressure in the kettle is kept between 0.1MPa and 0.15 MPa;
(3) Heating the reaction kettle to 96 ℃, adding 65% concentrated nitric acid by mass into the reaction kettle at the rate of 150L/h for reaction, controlling the reaction temperature to be 96 ℃ in the process of adding the concentrated nitric acid, adding 930L of concentrated nitric acid, stopping adding acid, and carrying out reaction for 6.2h;
(4) Continuously introducing oxygen with the purity of more than or equal to 99.9 percent into the reaction kettle, keeping the pressure in the kettle between 0.24MPa and 0.25MPa, and carrying out the reaction for 6 hours to obtain the indium nitrate solution.
After the reaction is finished, 2.5m high yield indium nitrate was obtained, and it was confirmed by inspection that the indium nitrate concentration was 1.74mol/L, the free acid concentration was 10g/L, the weight of unreacted indium was 0.023kg, and the average emission of nitrogen oxides during the reaction was 0m 3 The calculated result shows that the reaction is participated in the process of producing the indium nitrateThe molar ratio of indium to nitric acid of (1): 3, the nitric acid generated in the process of preparing the indium nitrate can be directly used as a raw material, so that the consumption of the nitric acid raw material is reduced.
Example 2.
(1) Configuration 1.6m 3 Adding pure water into the reaction kettle;
(2) Adding 500kg indium ingots into pure water, and filling oxygen into a reaction kettle to replace air in the kettle, so that the pressure in the kettle is kept between 0.1MPa and 0.15 MPa;
(3) Heating the reaction kettle to 98 ℃, adding 65% by mass of concentrated nitric acid into the reaction kettle at a rate of 150L/h for reaction, controlling the reaction temperature to be 98 ℃ in the process of adding the concentrated nitric acid, adding 930L of concentrated nitric acid, stopping adding acid, and carrying out reaction for 6.2h;
(4) Continuously introducing oxygen with the purity of more than or equal to 99.9 percent into the reaction kettle, keeping the pressure in the kettle between 0.22 and 0.23MPa, and carrying out the reaction for 6 hours to obtain the indium nitrate solution.
Detection shows that the indium nitrate concentration is 1.73mol/L, the free acid concentration is 11g/L, the weight of the unreacted indium is 1.4kg, and the average discharge amount of nitrogen oxides in the reaction process is 0m 3 The molar ratio of indium to nitric acid participating in the reaction in the process of producing the indium nitrate is 1:3, the nitric acid generated in the process of preparing the indium nitrate can be directly used as a raw material, so that the consumption of the nitric acid raw material is reduced.
Example 3.
(1) Configuration 1.6m 3 Adding pure water into the reaction kettle;
(2) Adding 500kg of indium ingot into pure water, and filling oxygen into a reaction kettle to replace air in the kettle, so that the pressure in the kettle is kept between 0.1MPa and 0.15 MPa;
(3) Heating the reaction kettle to 80 ℃, adding 65 mass percent concentrated nitric acid into the reaction kettle at the speed of 150L/h for reaction, controlling the reaction temperature to be 80 ℃ in the process of adding the concentrated nitric acid, adding 930L of concentrated nitric acid, stopping adding the acid, and performing reaction for 6.2h;
(4) Continuously introducing oxygen with the purity of more than or equal to 99.9 percent into the reaction kettle, keeping the pressure in the kettle between 0.20MPa and 0.21MPa, and carrying out the reaction for 6 hours to obtain the indium nitrate solution.
After the reaction is finished, 2.5m high yield indium nitrate was obtained, and it was confirmed by inspection that the indium nitrate concentration was 1.72mol/L, the free acid concentration was 13g/L, the weight of the unreacted indium was 4.2kg, and the average emission of nitrogen oxides during the reaction was 0m 3 And/h, calculating that the molar ratio of indium to nitric acid participating in the reaction in the process of producing the indium nitrate is 1:3, the nitric acid generated in the process of preparing the indium nitrate can be directly used as a raw material, so that the consumption of the nitric acid raw material is reduced.
Example 4.
(1) Configuration 1.6m 3 Adding pure water into the reaction kettle;
(2) Adding 500kg of indium ingot into pure water, and filling oxygen into a reaction kettle to replace air in the kettle, so that the pressure in the kettle is kept between 0.1MPa and 0.15 MPa;
(3) Heating the reaction kettle to 96 ℃, adding 65 mass percent concentrated nitric acid into the reaction kettle at the speed of 150L/h for reaction, controlling the reaction temperature to be 96 ℃ in the process of adding the concentrated nitric acid, adding 930L of concentrated nitric acid, stopping adding the acid, and carrying out the reaction for 6.2h;
(4) Continuously introducing oxygen with the purity of more than or equal to 99.9 percent into the reaction kettle, keeping the pressure in the kettle between 0.18MPa and 0.19MPa, and carrying out the reaction for 6 hours to obtain the indium nitrate solution.
Detection shows that the indium nitrate concentration is 1.66mol/L, the free acid concentration is 14g/L, the weight of unreacted indium is 21.5kg, and the average discharge amount of nitrogen oxides in the reaction process is 0.77m 3 And/h, calculating that the molar ratio of indium to nitric acid participating in the reaction in the process of producing the indium nitrate is 1:3.1, it can be seen that the nitric acid generated in the process of preparing indium nitrate can be directly used as a raw material, and the consumption of the nitric acid raw material is reduced.
Example 5.
(1) Configuration 1.6m 3 Adding pure water into the reaction kettle;
(2) Adding 500kg of indium ingot into pure water, and filling oxygen into a reaction kettle to replace air in the kettle, so that the pressure in the kettle is kept between 0.1MPa and 0.15 MPa;
(3) Heating the reaction kettle to 85 ℃, adding 65 mass percent concentrated nitric acid into the reaction kettle at the speed of 150L/h for reaction, controlling the reaction temperature to be 85 ℃ in the process of adding the concentrated nitric acid, adding 930L of concentrated nitric acid, stopping adding the acid, and carrying out the reaction for 6.2h;
(4) Continuously introducing oxygen with the purity of more than or equal to 99.9 percent into the reaction kettle, keeping the pressure in the kettle between 0.16MPa and 0.17MPa, and carrying out the reaction for 6 hours to obtain the indium nitrate solution.
After the reaction is finished, 2.5m high yield indium nitrate was obtained, and it was confirmed by inspection that the indium nitrate concentration was 1.61mol/L, the free acid concentration was 14g/L, the weight of unreacted indium was 36.5kg, and the average emission of nitrogen oxides during the reaction was 1.48m 3 And/h, calculating that the molar ratio of indium to nitric acid participating in the reaction in the process of producing the indium nitrate is 1:3.2, it can be seen that the nitric acid generated in the process of preparing indium nitrate can be directly used as a raw material, and the consumption of the nitric acid raw material is reduced.
Comparative example 1.
(1) Configuration 1.6m 3 Adding pure water into the reaction kettle;
(2) Adding 500kg of indium ingot into pure water, and filling oxygen into a reaction kettle to replace air in the kettle, so that the pressure in the kettle is kept between 0.1MPa and 0.15 MPa;
(3) Heating the reaction kettle to 96 ℃, adding 65 mass percent concentrated nitric acid into the reaction kettle at the speed of 150L/h for reaction, controlling the reaction temperature to be 96 ℃ in the process of adding the concentrated nitric acid, adding 930L of concentrated nitric acid, stopping adding the acid, and carrying out the reaction for 6.2h;
(4) And continuously introducing oxygen with the purity of more than or equal to 99.9 percent into the reaction kettle, keeping the pressure in the kettle between 0MPa, and carrying out the reaction for 6 hours to obtain the indium nitrate solution.
After the reaction is finished, 2.5m high-speed dry-harvest method is obtained, and detection shows that the concentration of indium nitrate is 0.8mol/L and the concentration of free acid is highThe degree is 24g/L, the weight of unreacted indium is 270kg, and the average emission of nitrogen oxides in the reaction process is 11.9m 3 And/h, calculating that the molar ratio of indium to nitric acid participating in the reaction in the process of producing the indium nitrate is 1: from this, it is apparent that nitric acid generated in the process of producing indium nitrate can be used as a raw material as it is, and the consumption of the nitric acid raw material is reduced.
Comparative example 2.
(1) Configuration 1.6m 3 Adding pure water into the reaction kettle;
(2) Adding 500kg of indium ingot into pure water, and filling oxygen into a reaction kettle to replace air in the kettle, so that the pressure in the kettle is kept between 0.1MPa and 0.15 MPa;
(3) Heating the reaction kettle to 96 ℃, adding 65% by mass of concentrated nitric acid into the reaction kettle at the rate of 150L/h for reaction, controlling the reaction temperature to be 96 ℃ in the process of adding the concentrated nitric acid, adding 1860L of the concentrated nitric acid, stopping adding acid, and carrying out the reaction for 12.4 h;
(4) And continuously introducing oxygen with the purity of more than or equal to 99.9 percent into the reaction kettle, keeping the pressure in the kettle between 0MPa, and carrying out the reaction for 6 hours to obtain the indium nitrate solution.
After the reaction is finished, 3.4m high yield indium nitrate was obtained, and it was confirmed by inspection that the indium nitrate concentration was 1.27mol/L, the free acid concentration was 26g/L, the weight of the unreacted indium was 0.95kg, and the average emission of nitrogen oxides during the reaction was 16m 3 And/h, calculating that the molar ratio of indium to nitric acid participating in the reaction in the process of producing the indium nitrate is 1:6.
as can be seen from comparative example 1, the invention can produce less nitrogen oxides, and is more environment-friendly; as can be seen from comparative example 2, the nitric acid generated in the preparation of the indium nitrate solution can be directly used as a raw material, so that a large amount of nitric acid is saved, and the production cost is saved.
The invention provides a preparation method of an indium nitrate solution, which has the advantages of less nitrogen oxides generated in the process of preparing the indium nitrate solution, simple preparation process and less acid consumption, and meanwhile, a small amount of generated nitrogen oxides can be directly discharged into the air after being absorbed by water, so that the tail gas treatment cost is reduced, and the environment is friendly.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (4)
1. The preparation method of the indium nitrate solution is characterized by comprising the following steps of:
s1, placing pure water in a reaction kettle;
s2, adding indium ingots into the pure water, and replacing air in the kettle with oxygen to keep the pressure in the kettle between 0.1MPa and 0.15 MPa;
s3, heating to 80-98 ℃, adjusting the temperature of the reaction kettle to be constant, and continuously adding concentrated nitric acid into the reaction kettle to perform reaction for the first time;
s4, after the first time, continuously introducing oxygen into the kettle to keep the pressure in the kettle between 0.16MPa and 0.25MPa, and carrying out reaction for a second time to obtain an indium nitrate solution;
the molar ratio of the concentrated nitric acid to the indium ingot is 2;
the first time is 6-6.5 h;
the second time is 6-6.2 h;
the mass fraction of the concentrated nitric acid is more than or equal to 65 percent;
the adding speed of the concentrated nitric acid is 140 mL/h-160 mL/h;
when the concentrated nitric acid is added into the reaction kettle, the temperature of the reaction kettle is controlled between 80 ℃ and 98 ℃.
2. The method according to claim 1, wherein in S4, oxygen is continuously introduced into the reactor to maintain the pressure in the reactor at 0.24MPa to 0.25 MPa.
3. The method for preparing an indium nitrate solution according to claim 1, wherein the purity of the oxygen gas is not less than 99.9%.
4. The method for preparing an indium nitrate solution according to claim 1, wherein the temperature of the reaction vessel is controlled to be 96 ℃ to 98 ℃.
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