CN116715266A - Method for preparing silver carbonate - Google Patents
Method for preparing silver carbonate Download PDFInfo
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- CN116715266A CN116715266A CN202310918270.XA CN202310918270A CN116715266A CN 116715266 A CN116715266 A CN 116715266A CN 202310918270 A CN202310918270 A CN 202310918270A CN 116715266 A CN116715266 A CN 116715266A
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- silver carbonate
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- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 title claims abstract description 41
- 229910001958 silver carbonate Inorganic materials 0.000 title claims abstract description 41
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 58
- 239000002270 dispersing agent Substances 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 21
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 87
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 60
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 39
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 39
- 239000012498 ultrapure water Substances 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 229920000058 polyacrylate Polymers 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 4
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- -1 fatty acid ester Chemical class 0.000 claims description 4
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 10
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 abstract description 10
- 238000001556 precipitation Methods 0.000 abstract description 6
- 229910001923 silver oxide Inorganic materials 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000005253 cladding Methods 0.000 abstract 2
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000011946 reduction process Methods 0.000 abstract 1
- 238000003763 carbonization Methods 0.000 description 10
- 238000000889 atomisation Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 6
- 229910001948 sodium oxide Inorganic materials 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 238000005086 pumping Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G5/00—Compounds of silver
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a method for preparing silver carbonate, which is prepared from raw material silver oxide or silver carbonate through steps of dispersing and precipitating, filtering and drying. According to the invention, the particle size of the silver powder can be refined through fractional dispersion precipitation, and nano controllable preparation of the silver powder is realized by controlling the coating agent, the dispersing agent, the reducing agent, the temperature, the time and the stirring parameters in the liquid phase reduction process. The microscopic reaction in the preparation process mainly comprises cladding, dissociating, reducing and re-cladding. The nanometer silver powder prepared by the invention has the advantages of fine granularity, uniform particle size and controllable morphology, and the product is mainly applied to the fields of electronic paste, conductive ink and the like.
Description
Technical Field
The invention belongs to the technical field of material engineering, and particularly relates to a method for preparing silver carbonate.
Background
The high-precision complex hard curved surface conformal circuit is a ten-big engineering technical problem which is urgently needed to be overcome in China, and the development and application of the high-purity nano silver carbonate for the electronic circuit are very large in market space around the urgent needs of development of the electronic information industry in China. Compared with the traditional liquid phase reduction of silver nitrate and silver oxide, the silver carbonate has the characteristics of high activity, high dispersion, large specific surface area, high tap density and the like when used for preparing nano silver powder through liquid phase reduction. The traditional silver carbonate preparation process is mainly prepared by adopting a reaction of silver nitrate and carbon alkali, and the patent CN101746809A adopts direct precipitation of silver nitrate and sodium carbonate to prepare silver carbonate; the patent CN104841467A adopts silver nitrate and sodium bicarbonate to directly precipitate and prepare silver carbonate; the patent CN105396547A adopts silver nitrate and sodium carbonate to prepare silver carbonate by precipitation; the patent 103274447 adopts industrial silver nitrate, silver oxide is prepared by adding sodium hydroxide for precipitation after complexation and impurity removal, and then silver carbonate is prepared by reacting the silver oxide with sodium carbonate, and the purity of the prepared silver carbonate is 99.5%.
The foreign silver carbonate production technology is complete and mature, the produced silver powder has high cleanliness, uniform particle size distribution, uniform morphology and good dispersibility, and the types of products are various (according to granularity, purity and structure division). At present, only silver carbonate with poor granularity uniformity, large particle size and relatively low purity can be prepared in China, and the industrial production and application of the nano high-purity silver carbonate production line are not realized yet. Therefore, it is necessary to develop a method capable of solving the above technical problems.
Disclosure of Invention
The invention aims to provide a method for preparing silver carbonate.
The invention aims at realizing the following steps of pretreatment, convection contact reaction, main reaction and post-treatment, and specifically comprises the following steps:
A. pretreatment:
1) Preparing a high-purity silver nitrate solution with the concentration of 1-500 g/L to obtain a solution a;
2) Preparing 1-500 g/L of high-purity potassium hydroxide or sodium hydroxide solution to obtain a solution b;
3) Weighing a dispersing agent according to the weight of the solid silver nitrate, and dissolving the dispersing agent in alcohol to obtain a dispersing agent solution c;
B. convective contact reaction:
1) Atomizing the solution a by an atomizer to obtain an atomized high-purity silver nitrate solution d;
2) Atomizing the solution b by an atomizer to obtain atomized high-purity potassium hydroxide or sodium hydroxide solution e;
3) The atomized high-purity silver nitrate solution d and the atomized high-purity potassium hydroxide or sodium hydroxide solution e flow into a closed reaction kettle, and the two paths of atomized gases are in convection contact reaction to generate nano high-purity Ag 2 O；
C. The main reaction:
1) Nano high-purity Ag 2 Stirring and washing O with high-purity water until the content of Na or K as an impurity is less than 10ppm to obtain a material f;
2) Adding the dispersant solution c into the material f to obtain slurry g;
3) Placing the slurry in a pressure reaction kettle, and introducing CO with the purity of 99.999 percent 2 Carrying out carbonation reaction on the gas to obtain silver carbonate h;
D. post-treatment: and (3) carrying out centrifugal filtration on the silver carbonate h to obtain a filter cake, and drying the filter cake to obtain the target high-purity nano silver carbonate.
The specific operation is as follows:
(1) Preparing a high-purity silver nitrate solution; (2) preparing high-purity alkali solution; (3) atomizing the high-purity silver nitrate solution; (4) atomizing the high-purity alkali solution; (5) Atomized high-purity silver nitrate solution and atomized high-purity alkali solution are simultaneously introduced into a closed large reactor, and gaseous silver nitrate and sodium hydroxide/potassium hydroxide precipitate are subjected to convection reaction to produce nano-scale Ag 2 O falls into the reaction kettle; (6) washing and filtering; (7) Ag (silver) 2 O, size mixing; (8) Ag (silver) 2 Pumping the O slurry into a pressure kettle; (7) High-purity CO is introduced 2 Carbonizing gas and dispersant solution at high temperature; (8) centrifugal filtration; and (9) drying. The silver carbonate prepared by the method has high purity, small particle size, uniform particle size distribution, regular and uniform morphology and monodisperse particles. The preparation process flow of the method is short and simple, and the working procedures are easy to refine.
The method comprises the following specific steps:
(1) Preparing 1 g/L-500 g/L of high-purity silver nitrate solution.
(2) Preparing 1 g/L-500 g/L high-purity potassium hydroxide/sodium solution.
(3) A certain amount of dispersing agent is weighed according to the weight of the solid silver nitrate, and is dissolved in alcohol at a certain temperature to form a dispersing agent solution.
(4) Atomizing the high-purity silver nitrate solution by an atomizer.
(5) The high purity potassium hydroxide/sodium solution was atomized with an atomizer.
(6) The atomized high-purity silver nitrate solution and the atomized high-purity potassium hydroxide/sodium solution flow into a closed reaction kettle, and the two paths of atomized gases are in convection contact reaction to generate nano high-purity Ag 2 O。
(7) Adding high-purity water into a precipitation reaction kettle, stirring and washing Ag 2 O, (the washing liquid-solid ratio is more than 10:1, the washing times are more than 4 times, and the washing is carried out until the impurity Na or K is less than 10 ppm).
(8) After washing and filtering, pouring the dispersant solution into the high-purity nano Ag which is mixed into slurry 2 O.
(9) Slurried Ag 2 The O slurry is pumped into the pressure reaction kettle by a pump.
(10) Introducing into99.999% high purity CO 2 And (3) carbonating and converting the gas under a certain condition to prepare the silver carbonate.
(11) After the reaction, the silver carbonate is centrifugally filtered.
(12) The silver carbonate is put into a drying oven for drying (the temperature and the time are controlled, and the temperature cannot be higher than 150 ℃).
The chemical reaction principle of the invention:
2AgNO 3 +2NaOH→Ag 2 O+2NaNO 3 +H 2 O；
2AgNO 3 +2KOH→Ag 2 O+2KNO 3 +H 2 O；
Ag 2 O+CO 2 →Ag 2 CO 3 (under the water system)
The atomized precipitation is that atomized silver nitrate solution and atomized high-purity alkali solution are contacted in parallel flow to generate nano-grade AgO particles; the hydrothermal carbonization is to slurry the filtered and washed nanometer silver oxide powder with high-purity water, pump the slurry into a reaction kettle, and introduce high-purity CO under the condition of stirring 2 The gas (which is both a reaction auxiliary material and a stirring medium) realizes the conversion of nano AgO to nano silver carbonate. The nano silver carbonate prepared by the method has small particle size, fine and uniform particle size and controllable morphology, and the product is mainly applied to the fields of composite catalysts, electronic paste, conductive ink and the like.
Drawings
FIG. 1 is a schematic diagram of the process flow of the present invention.
Detailed Description
The invention is further illustrated, but is not limited in any way, by the following examples, and any alterations or substitutions based on the teachings of the invention are within the scope of the invention.
The method comprises the steps of pretreatment, convection contact reaction, main reaction and post-treatment, and specifically comprises the following steps:
A. pretreatment:
1) Preparing a high-purity silver nitrate solution with the concentration of 1-500 g/L to obtain a solution a;
2) Preparing 1-500 g/L of high-purity potassium hydroxide or sodium hydroxide solution to obtain a solution b;
3) Weighing a dispersing agent according to the weight of the solid silver nitrate, and dissolving the dispersing agent in alcohol to obtain a dispersing agent solution c;
B. convective contact reaction:
1) Atomizing the solution a by an atomizer to obtain an atomized high-purity silver nitrate solution d;
2) Atomizing the solution b by an atomizer to obtain atomized high-purity potassium hydroxide or sodium hydroxide solution e;
3) The atomized high-purity silver nitrate solution d and the atomized high-purity potassium hydroxide or sodium hydroxide solution e flow into a closed reaction kettle, and the two paths of atomized gases are in convection contact reaction to generate nano high-purity Ag 2 O；
C. The main reaction:
1) Nano high-purity Ag 2 Stirring and washing O with high-purity water until the content of Na or K as an impurity is less than 10ppm to obtain a material f;
2) Adding the dispersant solution c into the material f to obtain slurry g;
3) Placing the slurry in a pressure reaction kettle, and introducing CO with the purity of 99.999 percent 2 Carrying out carbonation reaction on the gas to obtain silver carbonate h;
D. post-treatment: and (3) carrying out centrifugal filtration on the silver carbonate h to obtain a filter cake, and drying the filter cake to obtain the target high-purity nano silver carbonate.
The dispersing agent is polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), hydroxyethyl cellulose (HEC), polyethylene glycol (PEG-6000), polyacrylamide, ammonium polyacrylate, tween 80, sodium dodecyl benzene sulfonate, polyethylene glycol fatty acid ester or fatty acid polyoxyethylene ester.
And D, drying at the temperature of not higher than 150 ℃ for 10-20 hours.
The invention is further illustrated by the following examples:
example 1
(1) 40g of high purity silver nitrate was weighed and dissolved in 400ml of high purity water at which point C AgNO3 =100g/L。
(2) 9.5g of high purity sodium hydroxide was weighed and dissolved in 400ml of high purity water at which point C NaOH =23.75g/L。
(3) 1g of dispersant ammonium polyacrylate was weighed into a 0.5L beaker, added with 0.2L of absolute alcohol, and dissolved at 25 ℃ to form a dispersant solution.
(4) Atomizing the high-purity silver nitrate solution by an atomizer.
(5) Atomizing the high-purity sodium hydroxide solution by an atomizer.
(6) The atomized high-purity silver nitrate solution and the atomized high-purity strong sodium oxide solution are introduced into a 5L sealed reaction kettle, the stirring speed of the reaction kettle is 100r/min, 200ml of high-purity water is poured into the reaction kettle in advance, and the temperature of the reaction kettle is 60 ℃. The atomized high purity silver nitrate solution and the atomized high purity strong sodium oxide solution are convective.
(7) After atomization, standing for 40min, and extracting supernatant.
(8) 600ml of high-purity water is added into the atomization reaction kettle, and the stirring and washing are carried out for 10min at the stirring speed of 100r/min. After stirring and washing, standing for 40min, and then extracting the supernatant. This was repeated 6 times, at which time the Na ion concentration was 8ppm.
(9) 200ml of high-purity water is added into an atomization reaction kettle, 200ml of dispersing agent solution is added for size mixing, and the Ag after size mixing is carried out 2 And pumping the O slurry into a hydrothermal reaction kettle.
(10) The temperature of the hydrothermal reaction kettle is 120 ℃, and the stirring rotating speed is 100r/min; hydrothermal carbonization is carried out for 20 hours under the condition of high-purity CO2 gas pressure of 99.999 percent and 0.1Mpa, then the reaction rotating speed is reduced to 20r/min, and carbonization is carried out for 20 hours.
(11) And discharging high-purity nano silver carbonate slurry after the hydrothermal carbonization is finished, and centrifugally filtering on a 10000r/min ceramic centrifuge.
(12) After the filtration is finished, the wet silver carbonate filter cake is contained in a tray and is dried for 12 hours at 100 ℃.
Example 2
(1) 120g of high purity silver nitrate was weighed and dissolved in 400ml of high purity water at which point C AgNO3 =300g/L。
(2) Weighing 20g of high purity sodium hydroxide, dissolving in 400ml of high purity water, at this time C NaOH =50g/L。
(3) 3g of dispersant ammonium polyacrylate was weighed into a 0.5L beaker, added with 0.2L of absolute alcohol, and dissolved at 25 ℃ to form a dispersant solution.
(4) Atomizing the high-purity silver nitrate solution by an atomizer.
(5) Atomizing the high-purity sodium hydroxide solution by an atomizer.
(6) The atomized high-purity silver nitrate solution and the atomized high-purity strong sodium oxide solution are introduced into a 5L sealed reaction kettle, the stirring speed of the reaction kettle is 120r/min, 250ml of high-purity water is poured into the reaction kettle in advance, and the temperature of the reaction kettle is 80 ℃. The atomized high purity silver nitrate solution and the atomized high purity strong sodium oxide solution are convective.
(7) After atomization, standing for 60min, and extracting supernatant.
(8) 800ml of high-purity water is added into the atomization reaction kettle, stirred and washed for 20min, and the stirring rotation speed is 120r/min. After stirring and washing, standing for 60min, and then extracting the supernatant. This was repeated 5 times, at which time the Na ion concentration was 6ppm.
(9) Adding 800ml of high-purity water into an atomization reaction kettle, adding 250ml of dispersing agent solution for size mixing, and mixing the size-mixed Ag 2 And pumping the O slurry into a hydrothermal reaction kettle.
(10) The temperature of the hydrothermal reaction kettle is 140 ℃, and the stirring rotating speed is 120r/min; hydrothermal carbonization is carried out for 10 hours under the condition of high-purity CO2 gas pressure of 99.999 percent and 0.2Mpa, then the reaction rotating speed is reduced to 60r/min, and carbonization is carried out for 30 hours.
(11) And discharging high-purity nano silver carbonate slurry after the hydrothermal carbonization is finished, and centrifugally filtering on a 10000r/min ceramic centrifuge.
(12) After the filtration is finished, the wet silver carbonate filter cake is contained in a tray and is dried for 20 hours at 80 ℃.
Example 3
(1) 200g of high purity silver nitrate was weighed and dissolved in 1000ml of high purity water at which time C AgNO3 =200g/L。
(2) 40g of high purity sodium hydroxide was weighed and dissolved in 500ml of high purity water at which time C NaOH =80g/L。
(3) 5g of dispersant ammonium polyacrylate was weighed into a 2.5L beaker, added with 0.5L of absolute alcohol, and dissolved at 25 ℃ to form a dispersant solution.
(4) Atomizing the high-purity silver nitrate solution by an atomizer.
(5) Atomizing the high-purity sodium hydroxide solution by an atomizer.
(6) The atomized high-purity silver nitrate solution and the atomized high-purity strong sodium oxide solution are introduced into a 5L sealed reaction kettle, the stirring speed of the reaction kettle is 80r/min, 500ml of high-purity water is poured into the reaction kettle in advance, and the temperature of the reaction kettle is 60 ℃. The atomized high purity silver nitrate solution and the atomized high purity strong sodium oxide solution are convective.
(7) After atomization, standing for 70min, and extracting supernatant.
(8) 1000ml of high-purity water is added into the atomization reaction kettle, and the stirring and washing are carried out for 20min, and the stirring rotating speed is 80r/min. After stirring and washing, standing for 60min, and then extracting the supernatant. This was repeated 5 times, at which time the Na ion concentration was 7ppm.
(9) Adding 3000ml of high-purity water into an atomization reaction kettle, adding 1000ml of dispersing agent solution for size mixing, and mixing the size-mixed Ag 2 And pumping the O slurry into a hydrothermal reaction kettle.
(10) The temperature of the hydrothermal reaction kettle is 80 ℃, and the stirring rotating speed is 140r/min; hydrothermal carbonization is carried out for 15 hours under the condition of high-purity CO2 gas pressure of 99.999 percent and 0.1Mpa, then the reaction rotating speed is reduced to 40r/min, and carbonization is carried out for 20 hours.
(11) And discharging high-purity nano silver carbonate slurry after the hydrothermal carbonization is finished, and centrifugally filtering on a 10000r/min ceramic centrifuge.
(12) After the filtration is finished, the wet silver carbonate filter cake is contained in a tray and is dried for 10 hours at 110 ℃.
Claims (3)
1. A method for preparing silver carbonate, comprising the steps of pretreatment, convection contact reaction, main reaction and post-treatment, and specifically comprising the steps of:
A. pretreatment:
1) Preparing a high-purity silver nitrate solution with the concentration of 1-500 g/L to obtain a solution a;
2) Preparing 1-500 g/L of high-purity potassium hydroxide or sodium hydroxide solution to obtain a solution b;
3) Weighing a dispersing agent according to the weight of the solid silver nitrate, and dissolving the dispersing agent in alcohol to obtain a dispersing agent solution c;
B. convective contact reaction:
1) Atomizing the solution a by an atomizer to obtain an atomized high-purity silver nitrate solution d;
2) Atomizing the solution b by an atomizer to obtain atomized high-purity potassium hydroxide or sodium hydroxide solution e;
3) The atomized high-purity silver nitrate solution d and the atomized high-purity potassium hydroxide or sodium hydroxide solution e flow into a closed reaction kettle, and the two paths of atomized gases are in convection contact reaction to generate nano high-purity Ag 2 O；
C. The main reaction:
1) Nano high-purity Ag 2 Stirring and washing O with high-purity water until the content of Na or K as an impurity is less than 10ppm to obtain a material f;
2) Adding the dispersant solution c into the material f to obtain slurry g;
3) Placing the slurry in a pressure reaction kettle, and introducing CO with the purity of 99.999 percent 2 Carrying out carbonation reaction on the gas to obtain silver carbonate h;
D. post-treatment: and (3) carrying out centrifugal filtration on the silver carbonate h to obtain a filter cake, and drying the filter cake to obtain the target high-purity nano silver carbonate.
2. The method for preparing silver carbonate according to claim 1, wherein the dispersing agent is polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), hydroxyethyl cellulose (HEC), polyethylene glycol (PEG-6000), polyacrylamide, ammonium polyacrylate, tween 80, sodium dodecyl benzene sulfonate, polyethylene glycol fatty acid ester or fatty acid polyoxyethylene ester.
3. The method for preparing silver carbonate according to claim 1, wherein the drying in the step D is performed at a temperature of not higher than 150 ℃ for 10 to 20 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310918270.XA CN116715266A (en) | 2023-07-25 | 2023-07-25 | Method for preparing silver carbonate |
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