CN116216767A - Silver nitrate preparation method and device - Google Patents
Silver nitrate preparation method and device Download PDFInfo
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- CN116216767A CN116216767A CN202310319684.0A CN202310319684A CN116216767A CN 116216767 A CN116216767 A CN 116216767A CN 202310319684 A CN202310319684 A CN 202310319684A CN 116216767 A CN116216767 A CN 116216767A
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 title claims abstract description 194
- 229910001961 silver nitrate Inorganic materials 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 52
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 42
- 239000007788 liquid Substances 0.000 claims abstract description 37
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000001301 oxygen Substances 0.000 claims abstract description 21
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 21
- 229910052709 silver Inorganic materials 0.000 claims abstract description 21
- 239000004332 silver Substances 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 20
- 238000003860 storage Methods 0.000 claims description 15
- 239000012452 mother liquor Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 238000002425 crystallisation Methods 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 abstract description 39
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 32
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 5
- 150000002484 inorganic compounds Chemical class 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 230000000007 visual effect Effects 0.000 abstract description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 20
- 238000006243 chemical reaction Methods 0.000 description 17
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000000498 cooling water Substances 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- MTJGVAJYTOXFJH-UHFFFAOYSA-N 3-aminonaphthalene-1,5-disulfonic acid Chemical compound C1=CC=C(S(O)(=O)=O)C2=CC(N)=CC(S(O)(=O)=O)=C21 MTJGVAJYTOXFJH-UHFFFAOYSA-N 0.000 description 1
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 230000009469 supplementation Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G5/00—Compounds of silver
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00004—Scale aspects
- B01J2219/00006—Large-scale industrial plants
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method and a device of silver nitrate, which belong to the technical field of inorganic compound preparation, and the preparation method comprises the following steps: s1, mixing metallic silver with water, and starting stirring; s2, adding nitric acid into the mixture obtained in the step S1 in a sealed atmosphere containing oxygen and in a heating state; s3, cooling the mixture obtained in the step S2, and performing solid-liquid separation; s4, crystallizing silver nitrate from the liquid component obtained in the step S3. According to the preparation method, nitrogen oxides generated in the silver nitrate preparation process are oxidized and reabsorbed in the device, so that nitrogen elements in nitric acid are fully utilized, no nitrogen oxides are discharged in the silver nitrate preparation process, a green production effect is achieved, and meanwhile, when silver nitrate is concentrated and crystallized, a concentration end point is reached through concentration kettle bottom temperature judgment, so that end point observation and judgment are more visual and easy.
Description
Technical Field
The invention relates to the technical field of inorganic compound preparation, in particular to a preparation method and device of silver nitrate.
Background
Silver nitrate is colorless or white crystal, is an important raw material in electronic industry and photosensitive industry, and is prepared by reacting metallic silver with nitric acid. A large amount of nitrogen oxides are discharged in the preparation process, and the environment is greatly polluted.
It is proposed to add partial hydrogen peroxide to the reaction process of dissolving silver powder with nitric acid to prevent the generation of nitrogen oxides, and the main reaction formula is as follows: 2Ag+2HNO 3 +H 2 O 2 ＝2AgNO 3 +2H 2 In order to reduce the generation amount of nitrogen oxide gas, hydrogen peroxide is added, and the ratio of nitric acid to hydrogen peroxide is controlled at (0.78-1.42): 1. however, in the method, because the hydrogen peroxide is added into the silver nitrate solution, the cost of liquid production is increased, and meanwhile, partial nitrogen oxides are discharged. The solid-liquid separation of silver nitrate mainly adopts concentration crystallization, concentration end point judgment of the existing concentration crystallization adopts concentration amount or concentration until the system is subjected to crystal precipitation, and concentration amount control is often caused by fluctuation of nitric acid concentration and condensation effect, so that certain fluctuation of end point judgment is easy to occur in the condition of accumulation in a kettle or insufficient concentration; and concentration to the point that crystal precipitation occurs in the system is difficult to realize industrially.
Therefore, the green preparation device and method for silver nitrate are developed, so that nitrogen element is fully utilized, emission of nitrogen oxides is reduced, and meanwhile, the end point judgment method for concentrating end point silver nitrate is improved, and the method has great environmental effects and application prospects.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides the preparation method of the silver nitrate, which can realize the complete utilization of nitrogen element in the nitric acid, and has no emission of nitrogen oxides in the preparation process, so that the solid-liquid separation of the silver nitrate is easier to control.
The invention also provides a device adopted by the silver nitrate preparation method.
The first aspect of the invention provides a method for preparing silver nitrate, comprising the following steps:
s1, mixing metallic silver with water, and starting stirring;
s2, adding nitric acid into the mixture obtained in the step S1 in a sealed atmosphere containing oxygen and in a heating state;
s3, cooling the mixture obtained in the step S2, and performing solid-liquid separation;
s4, crystallizing silver nitrate from the liquid component obtained in the step S3.
The main chemical reaction process of the preparation method is as follows:
Ag+HNO 3 →AgNO 3 +NO+H 2 O；
NO+O 2 +H 2 O→HNO 3 ；
NO+O 2 →NO 2 ；
NO 2 +H 2 O→HNO 3 +NO。
the preparation method according to the embodiment of the first aspect of the invention has at least the following beneficial effects:
according to the preparation method, the airtight oxygen-containing gas atmosphere is created, the sealing is used for ensuring that oxygen introduced in the next step and nitrogen oxides generated by the reaction cannot overflow outwards, and nitrogen oxides generated in the silver nitrate preparation process can be oxidized and reabsorbed, so that nitrogen elements in nitric acid are fully utilized, no nitrogen oxides are discharged in the silver nitrate preparation process, and the green production effect is achieved.
According to the preparation method, when silver nitrate is crystallized, the concentration end point is judged by the bottom temperature of the silver nitrate concentration kettle, so that the end point observation and judgment are more visual and easy. As the concentration proceeds, the temperature of the material in the concentration kettle gradually increases, when the material is increased to a certain temperature, the concentration end point can be considered to be reached, if the concentration kettle is continuously increased, the silver nitrate is hardened, and if the temperature is not reached, the yield of the silver nitrate is reduced.
According to some embodiments of the invention, in step S1, the metallic silver is at least one of silver ingots, silver particles, and silver powder.
According to some embodiments of the invention, in step S1, the weight ratio of metallic silver to water is (1.0-1.2) to 1.
According to some embodiments of the invention, in the system of step S1, in a rest state, the predetermined position of the stirring paddle is the lowest end above the accumulation surface of the metallic silver, while contacting the liquid surface formed by the water.
The metal silver has high density, stirring cannot be performed, the stirrer is forcibly started to burn out, and the stirring paddle is arranged at a preset position, so that the later nitric acid can be stirred together with water, and the reaction speed is increased.
According to some embodiments of the invention, in step S2, the heating step is performed at a temperature of 60 ℃, and nitric acid is added after the temperature is raised to 60 ℃.
In step S2, the reaction rate can be increased by adding nitric acid after the temperature is raised to the predetermined temperature.
According to some embodiments of the invention, in step S2, the nitric acid has a mass concentration of 62 to 68%.
According to some embodiments of the invention, in step S2, the nitric acid is added in an amount of 95-100% of the metallic silver mass.
According to some embodiments of the invention, in step S2, the nitric acid is added in a manner of uniform dropping, and the dropping time is 3-4 hours.
According to some embodiments of the invention, in step S2, the pressure of the reaction system is 0.2 to 0.4MPa. The system pressure is adjusted by adjusting whether oxygen is introduced or not and the oxygen introduction rate.
According to some embodiments of the invention, in step S2, the incubation reaction is 1 to 1.5 hours after adding nitric acid.
According to some embodiments of the invention, in step S3, the cooling process is performed in a closed environment, i.e. the system valve of step S2 is kept closed.
According to some embodiments of the invention, in step S3, the temperature of the mixture after cooling is 20-25 ℃.
And when the temperature is reduced to the target temperature, decompression is started.
In the step S3, the filter residue after solid-liquid separation is residual metallic silver and can be recycled.
According to some embodiments of the invention, the crystallization comprises heat concentration, cooling crystallization, crystal separation and crystal drying performed sequentially;
according to some embodiments of the invention, in step S4, the temperature of the material in the concentrating kettle at the concentration end point set by heating and concentrating is 120-150 ℃.
Preferably, in step S4, the temperature of the material in the concentrating kettle at the concentration end point set by heating and concentrating is 130-140 ℃.
According to some embodiments of the invention, in step S4, the cooling rate of the cooling crystallization is 20-30 ℃/h.
Preferably, in the step S4, the cooling rate of the cooling crystallization is 20-25 ℃/h.
According to some embodiments of the invention, in step S4, the temperature set by the cooling crystallization is 20-25 ℃, and filtration is started after the temperature is reduced to 20-25 ℃. The filtrate obtained is put into step S2 for reuse.
The second aspect of the invention provides a device of the silver nitrate preparation method, which comprises a nitric acid storage tank, a silver nitrate preparation kettle, a first centrifuge and a silver nitrate concentration kettle which are sequentially connected through pipelines;
the silver nitrate preparation kettle is provided with a stirrer and an oxygen control valve;
a pressure balance pipe is arranged between the nitric acid storage tank and the silver nitrate preparation kettle.
According to some embodiments of the invention, the agitator is a liftable agitator with self-priming paddles.
According to some embodiments of the invention, the nitric acid storage tank is connected with the silver nitrate preparation kettle through a pressure balance pipe. The pressure of the nitric acid storage tank is consistent with that of the silver nitrate preparation kettle.
According to some embodiments of the invention, the oxygen control valve is an automatic linkage control valve.
The silver nitrate preparation kettle and the oxygen switch valve are automatically interlocked in pressure, and when the pressure change reaches a set value, the oxygen switch valve can be automatically started and stopped.
According to some embodiments of the invention, the production apparatus further comprises a mother liquor storage tank, a tail gas treatment column, and a condenser.
According to some embodiments of the invention, the tail gas treatment tower is connected with the silver nitrate preparation kettle; the condenser is connected with the silver nitrate concentration kettle; the mother liquor storage tank is connected with the silver nitrate concentration kettle through a second centrifugal machine.
According to some embodiments of the invention, the mother liquor storage tank is connected to the silver nitrate concentrating tank by a second liquid lift pump.
The NO and the NO generated in the silver nitrate preparation process can be realized by opening and closing the valve 2 The nitric acid is converted into the nitric acid to react with the metallic silver to form the silver nitrate, so that the utilization rate of nitrogen element reaches one hundred percent, and the green preparation of the silver nitrate is realized.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
fig. 1 is a schematic diagram of the workflow of a green silver nitrate production device.
Reference numerals:
a first valve 110; a second valve 120; a third valve 130; a fourth valve 140; a fifth valve 150; a sixth valve 160; a nitric acid tank 200; silver nitrate preparation kettle 300; a stirrer 310; a seal ring 320; a pressure balance tube 330; an oxygen control valve 340; a tail gas treatment tower 350; a first liquid lift pump 410; a second liquid lift pump 420; a third liquid lift pump 430; a first centrifuge 510; a second centrifuge 520; silver nitrate concentrating kettle 600; a mother liquor storage tank 610; a condenser 700.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
Example 1
The embodiment provides a preparation method of silver nitrate, which comprises the following steps:
(1) Before starting up, all valves are in a closed state, 500kg of fresh 30% caustic soda liquid is added into the tail gas treatment tower 350, and the first liquid lift pump 410 is started. Lifting the liftable stirrer 310 with the self-suction stirring paddle to the highest, adding 500kg of silver particles and 500kg of water into the silver nitrate preparation kettle 300, and lowering the liftable stirrer 310 with the self-suction stirring paddle to a preset position (the upper part of the metal silver contacts the water level or below the water level) to start stirring;
(2) Opening a first valve 110 to inject 461.7kg of 62% nitric acid into a nitric acid storage tank 200, closing the first valve 110, opening a pressure oxygen control valve 340 (automatic interlocking type), setting the automatic opening pressure of the valve to be less than or equal to 0.2MPa, setting the automatic closing pressure of the valve to be more than or equal to 0.4MPa, introducing oxygen into a silver nitrate preparation kettle 300, introducing steam to heat, preserving heat when the temperature of the silver nitrate preparation kettle 300 is raised to 60 ℃, opening a second valve 120 to transfer nitric acid into the silver nitrate preparation kettle 300, and carrying out heat preservation reaction for 1.5h after the nitric acid is added for about 4 h;
(3) After the reaction is finished, closing an oxygen control valve 340, introducing cooling water, after the materials are cooled to 25 ℃, opening a fourth valve 140 for pressure relief, after the pressure relief is finished, opening a first centrifugal machine 510 and a second liquid lifting pump 420, opening a third valve 130, and after the filtration is finished, allowing filtrate to enter a silver nitrate concentration kettle 600;
(4) Opening a silver nitrate concentrating kettle 600, stirring, starting heating and concentrating under normal pressure, closing heating when the kettle temperature reaches 135 ℃, introducing cooling water, controlling the cooling speed to be 25 ℃/h, cooling to 20 ℃, opening a second centrifugal machine 520 and a sixth valve 160, transferring the concentrated silver nitrate into the second centrifugal machine 520 for solid-liquid separation, closing the second centrifugal machine 520 and the sixth valve 160, opening a third liquid lifting pump 430, sending mother liquor generated in the second centrifugal machine 520 into the silver nitrate concentrating kettle 600, mixing with the next batch of materials, concentrating, vacuum drying filter residues to obtain a first batch of silver nitrate 609.9Kg, repeating the operation, mixing and concentrating the first batch of silver nitrate concentrated mother liquor, and vacuum drying to obtain a second batch of silver nitrate 786.0Kg, wherein the yield is 99.82%. After the two batches of reaction are finished, the total nitrogen content in the tail gas absorption liquid in the tail gas treatment tower 350 is detected, and is not detected.
The apparatus used in this embodiment is shown in fig. 1.
Example 2
The embodiment provides a preparation method of silver nitrate, which comprises the following steps:
(1) Before starting up, all valves are in a closed state, 500kg of fresh 30% caustic soda liquid is added into the tail gas treatment tower 350, and the first liquid lift pump 410 is started. Lifting the liftable stirrer 310 with the self-priming stirring paddle to the highest, adding 500kg of silver particles and 550kg of water into the silver nitrate preparation kettle 300, lowering the liftable stirrer 310 with the self-priming stirring paddle to a preset position, and starting stirring;
(2) Opening a first valve 110 to inject 449.4kg of 65% nitric acid into a nitric acid storage tank 200, closing the first valve 110, opening a pressure oxygen control valve 340, setting the automatic valve opening pressure to be less than or equal to 0.2MPa, setting the automatic valve closing pressure to be more than or equal to 0.35MPa, introducing oxygen into a silver nitrate preparation kettle 300, introducing steam to heat, keeping the temperature when the temperature of the silver nitrate preparation kettle 300 is raised to 60 ℃, opening a second valve 120 to transfer nitric acid into the silver nitrate preparation kettle 300, wherein the valve opening degree is that nitric acid is added in about 3 hours, and keeping the temperature for 1.5 hours after the addition;
(3) After the reaction is finished, closing an oxygen control valve 340, introducing cooling water, after the materials are cooled to 25 ℃, opening a fourth valve 140 for pressure relief, after the pressure relief is finished, opening a first centrifugal machine 510 and a second liquid lifting pump 420, opening a third valve 130, and after the filtration is finished, allowing filtrate to enter a silver nitrate concentration kettle 600;
(4) Opening a silver nitrate concentrating kettle 600, stirring, starting heating and concentrating under normal pressure, closing heating when the kettle temperature reaches 130 ℃, introducing cooling water, controlling the cooling speed to be 20 ℃/h, cooling to 20 ℃, opening a second centrifugal machine 520 and a sixth valve 160, transferring the concentrated silver nitrate into the second centrifugal machine 520 for solid-liquid separation, closing the second centrifugal machine 520 and the sixth valve 160, opening a third liquid lifting pump 430, sending mother liquor generated in the second centrifugal machine 520 into the silver nitrate concentrating kettle 600, mixing with the next batch of materials, concentrating, vacuum drying filter residues to obtain 601.6Kg of first batch of silver nitrate, repeating the operation, mixing and concentrating the first batch of silver nitrate concentrated mother liquor, and vacuum drying to obtain 789.6Kg of second batch of silver nitrate, wherein the yield is 100.28%. After the two batches of reaction are finished, the total nitrogen content in the tail gas absorption liquid in the tail gas treatment tower 350 is detected, and is not detected.
The apparatus used in this embodiment is shown in fig. 1.
Comparative example 1
The comparative example was essentially a system open system, with no additional oxygen supplementation, and the rest of the procedure and feeds were identical to those of example 1.
(1) Before starting up, all valves are in a closed state. Valve 140 was opened and 500kg of fresh 30% caustic solution was added to the tail gas treatment column 350 and the first liquid lift pump 410 was turned on. Lifting the liftable stirrer 310 with the self-priming stirring paddle to the highest, adding 500kg of silver particles and 500kg of water into the silver nitrate preparation kettle 300, lowering the liftable stirrer 310 with the self-priming stirring paddle to a preset position, and starting stirring;
(2) Opening a first valve 110 to inject 461.7kg of 62% nitric acid into the nitric acid storage tank 200, closing the first valve 110, introducing steam to heat, preserving heat when the temperature of the silver nitrate preparation kettle 300 is raised to 60 ℃, opening a second valve 120 to transfer nitric acid into the silver nitrate preparation kettle 300, adding nitric acid for about 4 hours, and preserving heat for 1.5 hours after adding nitric acid;
(3) After the reaction is finished, cooling water is introduced, after the materials are cooled to 25 ℃, a first centrifugal machine 510 and a second liquid lifting pump 420 are started, a third valve 130 is opened, and after the filtration is finished, filtrate enters a silver nitrate concentration kettle 600;
(4) Opening a silver nitrate concentrating kettle 600, stirring, starting heating and concentrating under normal pressure, closing heating when the kettle temperature reaches 135 ℃, introducing cooling water, controlling the cooling speed to be 25 ℃/h, cooling to 20 ℃, opening a second centrifugal machine 520 and a sixth valve 160, transferring the concentrated silver nitrate into the second centrifugal machine 520 for solid-liquid separation, closing the second centrifugal machine 520 and the sixth valve 160, opening a third liquid lifting pump 430, sending mother liquor generated in the second centrifugal machine 520 into the silver nitrate concentrating kettle 600, mixing with the next batch of materials, concentrating, vacuum drying filter residues to obtain a first batch of silver nitrate 453.1Kg, repeating the operation, mixing and concentrating the first batch of silver nitrate concentrated mother liquor, and vacuum drying to obtain a second batch of silver nitrate 592.3Kg, wherein the yield is 75.22%. After the two batches of reaction are finished, the total nitrogen content in the tail gas absorption liquid in the tail gas treatment tower 350 is detected to be 38167mg/L.
The testing method comprises the following steps:
the first yield is the ratio of the actual silver nitrate mass obtained by adding metallic silver to the theoretical silver nitrate mass obtained.
The second batch yield is the ratio of the actual silver nitrate mass obtained by adding the metal silver and the first batch silver nitrate concentrated solution to the silver nitrate mass obtained by the theory of adding the metal silver into the second batch.
The method for testing the total nitrogen content of the tail gas absorption liquid comprises the following steps: determination of total Nitrogen in Water quality by alkaline Potassium persulfate digestion ultraviolet spectrophotometry in GB/T11894-1989.
Table 1 quality, yield and total nitrogen content of the tail gas absorbing liquid of silver nitrate obtained in examples and comparative examples
As can be seen from Table 1, total nitrogen is not detected in the tail gas absorption liquid after both the reaction batches in example 1 and example 2, and the yield of silver nitrate in the second reaction batch is close to 100%, which indicates that the nitrogen oxide emission is not generated in the preparation of silver nitrate in the examples, and the utilization rate of nitrogen element in nitric acid reaches 100%. In the comparative example, the total nitrogen content in the tail gas absorption liquid after two batches of reaction is high, and the silver nitrate yield of the two batches is obviously lower than that of the example 1 and the example 2, which shows that the discharge of nitrogen oxides is generated during the preparation of the silver nitrate of the comparative example 1, and the nitrogen element utilization rate in the nitric acid is not high. Therefore, the preparation method and the device provided by the invention can realize the complete utilization of nitrogen element in nitric acid, and accord with the concept of green production. While the embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (10)
1. A method for preparing silver nitrate, which is characterized by comprising the following steps:
s1, mixing metallic silver with water, and starting stirring;
s2, adding nitric acid into the mixture obtained in the step S1 in a sealed atmosphere containing oxygen and in a heating state;
s3, cooling the mixture obtained in the step S2, and performing solid-liquid separation;
s4, crystallizing silver nitrate from the liquid component obtained in the step S3.
2. The preparation method according to claim 1, wherein in the step S1, the weight ratio of the metallic silver to the water is 1.0 to 1.2:1.
3. the method according to claim 1, wherein in step S4, the crystallization includes heat concentration, cooling crystallization, crystal separation, and crystal drying which are sequentially performed; preferably, the temperature of the materials in the concentration kettle at the end of the heating concentration is 120-150 ℃.
4. The method according to claim 3, wherein the cooling rate of the cooling crystallization is 20 to 30 ℃/h.
5. The method according to claim 1, wherein in step S2, the atmosphere pressure is 0.2 to 0.4MPa.
6. A production apparatus employed in the production method of silver nitrate according to any one of claims 1 to 5, characterized in that the production apparatus comprises a nitric acid tank (200), a silver nitrate production tank (300), a first centrifuge (510) and a silver nitrate concentration tank (600) which are connected in this order via pipes;
the silver nitrate preparation kettle (300) is provided with a stirrer (310) and an oxygen control valve (340);
a pressure balance pipe (330) is arranged between the nitric acid storage tank (200) and the silver nitrate preparation kettle (300).
7. The apparatus of claim 6, wherein the agitator (310) is a liftable agitator with self-priming paddles.
8. The manufacturing apparatus according to claim 6, wherein the oxygen control valve (340) is an automatic linkage control valve.
9. The production plant according to claim 6, further comprising a mother liquor storage tank (610), a tail gas treatment column (350) and a condenser (700);
the tail gas treatment tower (350) is connected with the silver nitrate preparation kettle (300); the condenser (700) is connected with the silver nitrate concentration kettle (600); the mother liquor storage tank (610) is connected with the silver nitrate concentration kettle (600) through a second centrifugal machine (520).
10. The production apparatus according to claim 9, wherein the mother liquor storage tank (610) is connected to the silver nitrate concentration tank (600) by a second liquid lift pump (420).
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| CN202310319684.0A CN116216767A (en) | 2023-03-29 | 2023-03-29 | Silver nitrate preparation method and device |
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Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1039325A (en) * | 1910-01-29 | 1912-09-24 | Norsk Hydro Elektrisk | Process of making nitrates and nitric acid. |
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| CN111732120A (en) * | 2020-06-17 | 2020-10-02 | 中船重工黄冈贵金属有限公司 | Environment-friendly efficient production method of high-purity silver nitrate |
| CN115072764A (en) * | 2022-07-04 | 2022-09-20 | 广东先导稀材股份有限公司 | Preparation method of metal nitrate |
| CN115108577A (en) * | 2022-06-28 | 2022-09-27 | 桐柏泓鑫新材料有限公司 | High-purity silver nitrate low-energy-consumption preparation method and system |
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| US1039325A (en) * | 1910-01-29 | 1912-09-24 | Norsk Hydro Elektrisk | Process of making nitrates and nitric acid. |
| GB634189A (en) * | 1947-02-21 | 1950-03-15 | Johnson & Sons Smelting Works | Improvements in and relating to the manufacture of silver and bismuth nitrates |
| GB634578A (en) * | 1947-02-21 | 1950-03-22 | Johnson & Sons Smelting Works | Improvements in and relating to chemical reactions involving the evolution of fumes of oxides of nitrogen |
| US5364500A (en) * | 1991-02-04 | 1994-11-15 | Eastman Kodak Company | Process for removing nitrites from a silver nitrate solution |
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| CN208757276U (en) * | 2018-08-07 | 2019-04-19 | 中船重工黄冈贵金属有限公司 | A kind of device of scale reducing nitrogen oxides during preparation of silver nitrate discharge |
| CN111732120A (en) * | 2020-06-17 | 2020-10-02 | 中船重工黄冈贵金属有限公司 | Environment-friendly efficient production method of high-purity silver nitrate |
| CN115108577A (en) * | 2022-06-28 | 2022-09-27 | 桐柏泓鑫新材料有限公司 | High-purity silver nitrate low-energy-consumption preparation method and system |
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