Silver nitrate impurity removal agent and preparation method thereof
By preparing large-pore adsorption resins loaded with silver oxide particles, the replacement reaction is used to remove metal impurities in silver nitrate, the existing silver nitrate removal process is solved, and the efficient and stable impurity removal effect and high quality are achieved Production of pure silver nitrate.
Patent Information
- Application Number
- CN202411664682.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-20
- Publication Date
- 2025-02-14
AI Technical Summary
The existing silver nitrate removal process is complex, has high cost, and is easy to introduce new impurities, which makes it difficult to improve the purity of silver nitrate.
Large-porous adsorption resins are prepared by using raw materials such as silver oxide, styrene, divinyl benzene, toluene and gelatin, and silver oxide particles are loaded, and metal impurities in silver nitrate are removed by a replacement reaction.
The efficient and stable silver nitrate removal is achieved, the impurity removal process is simplified, the cost is reduced, and new impurities are not introduced, ensuring the production of high-purity silver nitrate.
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Figure CN119430267A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of silver nitrate impurity removal and relates to a silver nitrate impurity remover and a preparation method thereof. Background Art
[0002] With the rapid development of modern science and technology, the purity requirements of silver nitrate in various industries are constantly increasing. High-purity silver nitrate has broad application prospects in the electronics industry, analytical chemistry, medicine, environmental protection and other industries.
[0003] To improve the purity of silver nitrate, it is necessary to remove as many impurities as possible from silver nitrate. However, the current process for removing impurities from silver nitrate is relatively complicated, costly, and has strict technical requirements, which makes it difficult to remove impurities from silver nitrate. In addition, new impurities are easily introduced during the partial removal process, which still affects the final purity of silver nitrate. In the process of removing impurities from silver nitrate, the impurity remover has a key influence on the impurity removal process and the impurity removal effect.
[0004] Therefore, it is necessary to provide a silver nitrate impurity remover and a preparation method thereof, so as to prepare an impurity remover that is simple to use and has a good impurity removal effect, so as to simplify the silver nitrate impurity removal process and reduce the impurity removal cost. Summary of the invention
[0005] In order to overcome the problems in the background technology, the present invention prepares silver nitrate impurity remover by using silver oxide, styrene, divinylbenzene, toluene, gelatin as raw materials, wherein styrene is used as a polymerization monomer, divinylbenzene is used as a cross-linking agent, toluene is used as a pore-forming agent, and gelatin is used as a dispersant. Each raw material is cross-linked and polymerized to form a porous skeleton structure of a macroporous adsorption resin, and silver oxide particles are loaded in the porous skeleton structure of a macroporous adsorption resin during the preparation process. Silver oxide particles are used to replace metal impurity ions in a silver nitrate solution, and metal impurity ions such as Fe, Cu, and Pb in the silver nitrate system are replaced, and impurity elements are adsorbed by a macroporous resin to achieve silver nitrate impurity removal. The replacement reaction follows the metal activity order, and a metal with high activity can replace a metal with low activity, which can occur at room temperature. Therefore, the replacement reaction has high stability and relatively loose reaction conditions, and thus, it is only necessary to add the impurity remover prepared by the present invention to the silver nitrate solution to be removed impurities, and silver nitrate can be removed impurities (mainly removing the impurity metals in the silver nitrate system), without the need to specially regulate the conditions, and it is simple to use, and the impurity removal effect is good.
[0006] In order to achieve the above object, the present invention is implemented by the following technical solutions:
[0007] The present invention provides a method for preparing a silver nitrate impurity remover, the method comprising the following steps:
[0008] (1) silver oxide, styrene, and divinylbenzene are mixed to form a mixed liquid, and then toluene and gelatin are added to the mixed liquid to obtain a mixture;
[0009] (2) heating the mixture obtained in step (1) under an oxygen pressurized environment, allowing the mixture to react to obtain a reaction product;
[0010] (3) The reaction product in step (2) is separated by suction filtration, and the obtained solid product is the silver nitrate impurity remover.
[0011] Preferably, in step (1), silver oxide, styrene and divinylbenzene are mixed in a mass ratio of silver oxide:styrene:divinylbenzene=1:2-5:8-15, and the amount of toluene and gelatin added is 0.5% of the total mass of the mixed liquid.
[0012] Preferably, in step (2), the oxygen pressurization pressure is 1.5 to 1.7 kPa.
[0013] Preferably, in step (2), the heating temperature is 180-200° C. and the reaction time is 2-4 hours.
[0014] Another aspect of the present invention provides a silver nitrate impurity remover, which is composed of silver oxide particles and a macroporous adsorption resin, wherein the silver oxide particles are loaded in a porous skeleton structure of the macroporous adsorption resin.
[0015] Beneficial effects of the present invention:
[0016] 1. The silver nitrate impurity remover prepared by the preparation method of the present invention is simple to use, has good impurity removal stability, and has good impurity removal effect. It can be directly used for impurity removal in the process of preparing high-purity silver nitrate, effectively simplifying the silver nitrate impurity removal process and reducing the impurity removal cost.
[0017] 2. During the impurity removal process using the silver nitrate impurity remover prepared by the present invention, silver oxide particles are replaced with impurity elements, silver ions are introduced into the silver nitrate system, and the macroporous adsorption resin does not participate in the reaction, thereby not introducing new impurities.
[0018] 3. The preparation method of the present invention is relatively simple, the raw materials are easy to obtain, and it is suitable for industrial application and promotion.
[0019] 4. The present invention can remove metal impurities in the silver nitrate system at a rate of 95-98%. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] Figure 1 It is a schematic diagram of the microstructure of the silver nitrate impurity remover of the present invention;
[0021] Figure 2 This is a SEM image of the silver oxide particles in the present invention. DETAILED DESCRIPTION
[0022] The present invention is further described in detail below in conjunction with specific embodiments.
[0023] All chemical reagents not specifically described in the examples of the present invention were commercially available analytically pure.
[0024] Example 1
[0025] This embodiment prepares silver nitrate impurity remover by the following method:
[0026] (1) Silver oxide, styrene and divinylbenzene are weighed and mixed in a mass ratio of silver oxide:styrene:divinylbenzene = 1:2:8 to obtain a mixed liquid, and 0.5% of toluene and 0.5% of divinylbenzene are added to the mixed liquid to obtain a mixture.
[0027] (2) The mixture was placed in a reactor, and oxygen was introduced into the reactor until the oxygen pressure in the reactor reached 1.5 kPa. The mixture was then heated to 180° C. and reacted for 4 hours before the reaction product was taken out.
[0028] (3) The reaction product is filtered and the solid product obtained is collected, which is the silver nitrate impurity remover.
[0029] Example 2
[0030] This embodiment adopts the same method as that of embodiment 1 to prepare silver nitrate impurity remover, except that: in this embodiment, the mass ratio of silver oxide, styrene and divinylbenzene is 1:5:15, the oxygen pressurization pressure is 1.5 kPa, the mixture heating temperature is 200°C, and the reaction time is 2h.
[0031] The structure and impurity removal effect of the silver nitrate impurity remover prepared in this embodiment are similar to those in Example 1.
[0032] Example 3
[0033] This embodiment adopts the same method as that of embodiment 1 to prepare silver nitrate impurity remover, except that: in this embodiment, the mass ratio of silver oxide, styrene and divinylbenzene is 1:3:10, the oxygen pressurization pressure is 1.6 kPa, the mixture heating temperature is 190°C, and the reaction time is 3 hours.
[0034] The structure and impurity removal effect of the silver nitrate impurity remover prepared in this embodiment are similar to those in Example 1.
[0035] The silver nitrate impurity remover prepared in Example 1 was selected, and the silver nitrate impurity remover was added to a silver nitrate solution with a pH value of 3, and the solution was allowed to stand at room temperature for 10 hours for impurity removal, and then the silver nitrate was filtered to remove solid impurities, and the filtrate was placed in a water bath, and stirred and evaporated at 95° C. After a layer of crystal film appeared in the filtrate, the heating was turned off, and the stirring was continued until the filtrate was naturally cooled and crystallized, and the cooled product was centrifuged, and then dried at 70° C. for 8 hours to obtain silver nitrate crystals, and the metal impurity content in the silver nitrate crystals was detected to be less than 0.0005%.
[0036] The silver nitrate impurity remover prepared in Example 1 was selected and added to a silver nitrate solution of pH=4, and allowed to stand at room temperature for 10 hours for impurity removal. After impurity removal, silver nitrate crystals were prepared by the same method as above, and the metal impurity content in the silver nitrate crystals was detected to be less than 0.0004%.
[0037] The silver nitrate impurity remover prepared in Example 1 was selected and added to a silver nitrate solution of pH=5, and allowed to stand at room temperature for 10 hours for impurity removal. After impurity removal, silver nitrate crystals were prepared by the same method as above, and the metal impurity content in the silver nitrate crystals was detected to be less than 0.0002%.
[0038] like Figure 1 As shown, the specific structure of the impurity remover of the present invention is that silver oxide particles are loaded on the surface and pores of the porous skeleton structure of the macroporous adsorption resin. After the impurity remover is introduced into the silver nitrate solution, the silver oxide particles loaded in the skeleton structure are replaced with the impurity elements in the solution, and the impurity elements are adsorbed on the macroporous adsorption resin and removed.
[0039] pass Figure 2 It can be seen that the present invention preferably uses silver oxide particles of uniform size and good dispersion to improve the uniformity of the distribution of the silver oxide particles on the surface and in the pores of the macroporous adsorption resin, thereby helping to improve the impurity removal efficiency.
[0040] In summary, the silver nitrate impurity remover prepared by the present invention is simple to use, the impurity removal process is less affected by the environment, there is no need to perform special regulation on the impurity removal environment, the impurity removal stability is good, and at the same time, a high metal impurity removal rate is achieved, the silver nitrate impurity removal process can be effectively simplified, and the impurity removal cost can be reduced. The silver nitrate impurity remover of the present invention is suitable for industrial application and promotion.
[0041] Finally, it should be noted that the above preferred embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail through the above preferred embodiments, those skilled in the art should understand that various changes can be made in form and details without departing from the scope defined by the claims of the present invention.
Claims
1. A method for preparing a silver nitrate impurity remover, characterized in that: The preparation method comprises the following steps: (1) silver oxide, styrene, and divinylbenzene are mixed to form a mixed liquid, and then toluene and gelatin are added to the mixed liquid to obtain a mixture; (2) heating the mixture obtained in step (1) under an oxygen pressurized environment, allowing the mixture to react to obtain a reaction product; (3) The reaction product in step (2) is separated by suction filtration, and the obtained solid product is the silver nitrate impurity remover.
2. The preparation method according to claim 1, characterized in that: In the step (1), silver oxide, styrene and divinylbenzene are mixed in a mass ratio of silver oxide:styrene:divinylbenzene=1:2-5:8-15, and the amount of toluene and gelatin added is 0.5% of the total mass of the mixed liquid.
3. The preparation method according to claim 1, characterized in that: In the step (2), the oxygen pressure is 1.5 to 1.7 kPa.
4. The preparation method according to claim 1, characterized in that: In the step (2), the heating temperature is 180-200° C. and the reaction time is 2-4 hours.
5. The silver nitrate impurity remover prepared by the preparation method according to any one of claims 1 to 4, characterized in that: The silver nitrate impurity remover is composed of silver oxide particles and macroporous adsorption resin, and the silver oxide particles are loaded in the porous skeleton structure of the macroporous adsorption resin.