A kind of preparation method of calamine powder
Through ultrasonic cleaning, calcination and purification treatment of porous carbon magnetic adsorption materials, the impact and purity problems of impurities in the preparation of calamine powder are solved, and high-quality preparation of calamine powder is achieved.
Patent Information
- Application Number
- CN202310019325.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-01-06
- Publication Date
- 2025-02-07
- Estimated Expiration
- 2043-01-06
AI Technical Summary
The existing preparation methods of calamine powder are easily affected by impurities on the surface of calamine raw materials, reducing its cleanliness, and the metal ions inside will reduce the purity of calamine powder.
The impurities are removed by ultrasonic cleaning and calcining steps, the impurities are separated by multiple screening and grinding, and purification is performed using porous carbon magnetic adsorption materials to adsorb heavy metal ions.
It improves the cleanliness and purity of calamine powder, reduces the influence of impurities, and ensures the high-quality preparation of calamine powder.
Smart Images

Figure CN116270731B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of calamine powder, and particularly relates to a preparation method of calamine powder. Background Art
[0002] Calamine is a carbonate mineral of the calcite family, mainly containing zinc carbonate. After mining, wash, dry and remove the debris. This product is a block aggregate, irregular block, grayish white or light red. The surface is powdery, dull, uneven, porous, and honeycomb-like. It is light and fragile. Odorless, slightly astringent. Functions and indications: detoxification, improving eyesight, removing cataracts, absorbing moisture, relieving itching and healing sores. It is used for red and swollen eyes, red and rotten eye edges, cataracts, ulcers that do not heal, pus dripping, wet sores, and skin itching.
[0003] For example, a method for preparing calamine powder disclosed in the authorization announcement number CN114956158A achieves that the obtained calamine powder has a high ZnO content, fluffy particles, is not easy to agglomerate, and has good dispersibility. The method is simple and easy to implement and is suitable for industrial large-scale production. However, it does not solve the problems that still exist in the existing calamine powder preparation method and preparation device: in the calamine powder preparation method, calamine powder is easily affected by impurities on the surface of the calamine raw material, reducing its cleanliness. At the same time, the metal ions inside the calamine will reduce the purity of the calamine powder. For this reason, we propose a method for preparing calamine powder. Summary of the invention
[0004] The object of the present invention is to provide a method for preparing calamine powder to solve the problems raised in the above-mentioned background technology.
[0005] To achieve the above object, the present invention provides the following technical solution: a method for preparing calamine powder, comprising the following steps:
[0006] S1. Cleaning: The calamine ore raw material is placed in an ultrasonic cleaner, washed with acetic acid aqueous solution for 6-10min, filtered, and the obtained solid is washed 2-4 times to obtain a bright surface of calamine;
[0007] S2 calcining: the cleaned calamine ore is placed in a calcining furnace, calcined at a temperature of 700-1000 ℃ for 2-4 hours, and naturally cooled to room temperature to obtain calcined calamine;
[0008] S3 crushing: The calcined calamine was crushed by a grinder and screened through a 80-120 mesh sieve to obtain calcined calamine powder;
[0009] S4 first grinding: the calcined calamine powder was added to the grinder, an appropriate amount of water was added to the grinder, the grinder was turned on, the calcined calamine powder was ground, the grinder was turned off after grinding, the mixture of calcined calamine powder and water after grinding was allowed to stand for 15-20 minutes to obtain an upper slurry and a lower calamine powder;
[0010] S5. Second grinding: using a peristaltic pump to pump the upper slurry into the cyclone, by adjusting the power of the peristaltic pump to control the pressure and flow rate at the cyclone inlet, to obtain a calamine slurry with a particle size less than 110 mesh, a calamine slurry with a particle size greater than 110 mesh, discharged from the lower portion of the cyclone into the grinder to continue grinding, the calamine slurry was transported to a settling tank, allowed to stand for 2-4 hours for stratification to obtain an upper aqueous solution and a lower calamine powder;
[0011] S6 drying: the lower layer of calamine powder dehydrated by a dehydrator to obtain calamine powder, the calamine powder set temperature in a drying oven 80-100 ℃ for drying, to obtain dried calamine powder;
[0012] S7. Dissolving: Under stirring conditions at 35-55 ° C, add 8% dilute hydrochloric acid to the calamine powder, stir until dissolved, and cool to room temperature;
[0013] S8. Filtration: Filter to remove insoluble solid impurities, add sodium hydroxide solution to the filtrate, stir, let stand and filter;
[0014] S9. Purification: add porous carbon magnetic adsorption material to the filtrate, stir for 15-30 minutes, remove the porous carbon magnetic adsorption material with a magnet, adjust the pH of the solution to 8.6-9.4 with sodium carbonate, filter, wash the solid with water 2-4 times, dry the obtained solid at 80-100°C to a constant temperature, crush it with a grinder, and pass it through an 80-100 mesh sieve to obtain the calamine powder product.
[0015] Preferably, the power of the ultrasonic cleaner in S1 is 400-600W, and the mass fraction of the acetic acid aqueous solution is 3-6%.
[0016] Preferably, in said S3, adding an appropriate amount of water into the grinder is specifically: the amount of water is 8-12 times the amount of calcined calamine added.
[0017] Preferably, the mass fraction of the sodium hydroxide solution in S8 is 8-10%, the stirring speed is 200-400 r / min, the stirring time is 40-60 min, and the standing time is 20-40 min.
[0018] Preferably, the preparation method of the porous carbon magnetic adsorption material added in the purification of S9 is:
[0019] S101. Zinc nitrate hexahydrate, ferric acetylacetonate and dimethylimidazole were dissolved in ethanol respectively, and the three solutions were mixed at room temperature to form a milky suspension, which was stirred for 10-30 min, centrifuged and washed with ethanol, and repeated three times to obtain a red precipitate, which was dried at 50-80°C for 40-60 min to obtain Fe-ZIF-8 powder;
[0020] S102. Place the Fe-ZIF-8 powder in a tubular furnace and calcine it at elevated temperature for 2-3 hours under a nitrogen atmosphere to obtain a porous carbon magnetic adsorption material.
[0021] Preferably, the weight ratio of zinc nitrate hexahydrate, ferric acetylacetonate and dimethylimidazole in S101 is 6:4:3.
[0022] Preferably, the temperature increase in S102 is specifically: increasing the temperature to 700-900° C. at a rate of 3-5° C.·min.
[0023] Compared with the prior art, the present invention has the following beneficial effects:
[0024] (1) The method adopted by the present invention is to prepare calamine powder. By cleaning calamine ore, the cleanliness of the calamine ore can be ensured, and the influence of impurities on the surface of the calamine ore on the preparation of calamine powder can be reduced. Meanwhile, by purification treatment, the porous carbon magnetic adsorption material can be used to adsorb heavy metal ions, thereby further increasing the purity of the prepared calamine powder.
[0025] (2) The preparation device of the present invention can screen the calamine powder by setting a screening plate, and the screening plate is driven to vibrate by a vibration motor, which can increase the screening efficiency and prevent the situation of non-dropping of the material. At the same time, by setting a first discharge port and a first conveyor belt, unqualified calamine powder can be transported for reprocessing. At the same time, by setting a second discharge port and a second conveyor belt, qualified calamine powder can be transported for packaging. BRIEF DESCRIPTION OF THE DRAWINGS
[0026] Figure 1 is a flow chart of the present invention;
[0027] Figure 2 It is a structural schematic diagram of the present invention;
[0028] Figure 3 For the present invention Figure 2 Enlarged view of point A in the middle.
[0029] In the figure: 1. screening box; 2. feeding funnel; 3. screening plate; 4. first discharge port; 5. containing tank; 6. supporting plate; 7. vibration motor; 8. connecting plate; 9. first discharge plate; 10. first conveyor belt; 11. guide plate; 12. second discharge port; 13. second discharge plate; 14. second conveyor belt; 15. slide plate; 16. slide rail. DETAILED DESCRIPTION
[0030] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0031] Example 1
[0032] See also Figure 1 The present invention provides a technical solution: a method for preparing calamine powder, comprising the following steps:
[0033] S1. Cleaning: The calamine ore raw material was placed in an ultrasonic cleaner, washed with acetic acid aqueous solution for 6 min, filtered, and the obtained solid was washed twice to obtain a bright surface of calamine;
[0034] S2 calcining: the cleaned calamine ore was placed in a calcining furnace, calcined at a temperature of 700 ℃ for 2 hours, and naturally cooled to room temperature to obtain calcined calamine;
[0035] S3 crushing: The calcined calamine was crushed by a grinder and screened through an 80-mesh sieve to obtain calcined calamine powder;
[0036] S4 first grinding: the calcined calamine powder was added to the grinder, an appropriate amount of water was added to the grinder, the grinder was turned on, the calcined calamine powder was ground, the grinder was turned off after grinding, the mixture of calcined calamine powder and water after grinding was allowed to stand for 15 minutes to obtain an upper slurry and a lower calamine powder;
[0037] S5. Second grinding: using a peristaltic pump to pump the upper slurry into the cyclone, by adjusting the power of the peristaltic pump to control the pressure and flow rate at the cyclone inlet, to obtain a calamine slurry with a particle size less than 110 mesh, a calamine slurry with a particle size greater than 110 mesh, discharged from the lower portion of the cyclone into the grinder to continue grinding, the calamine slurry was transported to a settling tank, allowed to stand for 2 hours for stratification, to obtain an upper aqueous solution and a lower calamine powder;
[0038] S6 drying: the lower layer of calamine powder was dehydrated by a dehydrator to obtain calamine powder, the calamine powder was dried in a drying oven at a temperature of 80 ° C to obtain dried calamine powder;
[0039] S7. Dissolving: Under stirring conditions at 35°C, add 8% by mass of dilute hydrochloric acid to the calamine powder, stir until dissolved, and cool to room temperature;
[0040] S8. Filtration: Filter to remove insoluble solid impurities, add sodium hydroxide solution to the filtrate, stir, let stand and filter;
[0041] S9. Purification: Add porous carbon magnetic adsorption material to the filtrate, stir for 15 minutes, remove the porous carbon magnetic adsorption material with a magnet, adjust the pH of the solution to 8.6 with sodium carbonate, filter, wash the solid twice with water, dry the obtained solid at 80°C to a constant temperature, crush it with a grinder, and pass it through an 80-mesh sieve to obtain the calamine powder product.
[0042] In this embodiment, preferably, the power of the ultrasonic cleaner in S1 is 400W, and the mass fraction of the acetic acid aqueous solution is 3%.
[0043] In this embodiment, preferably, the step of adding an appropriate amount of water to the grinder in S3 is as follows: the amount of water is 8 times the amount of the added calcined calamine.
[0044] In this embodiment, preferably, the mass fraction of the sodium hydroxide solution in S8 is 8%, the stirring speed is 200 r / min, the stirring time is 40 min, and the standing time is 20 min.
[0045] In this embodiment, preferably, the preparation method of the porous carbon magnetic adsorption material added in the purification of S9 is:
[0046] S101. Zinc nitrate hexahydrate, ferric acetylacetonate and dimethylimidazole were dissolved in ethanol respectively, and the three solutions were mixed at room temperature to form a milky suspension, which was stirred for 10 min, centrifuged and washed with ethanol, and the mixture was repeated three times to obtain a red precipitate, which was dried at 50°C for 40 min to obtain Fe-ZIF-8 powder;
[0047] S102. Place the Fe-ZIF-8 powder in a tubular furnace and calcine it at elevated temperature for 2 hours under a nitrogen atmosphere to obtain a porous carbon magnetic adsorption material.
[0048] In this embodiment, preferably, the weight ratio of zinc nitrate hexahydrate, ferric acetylacetonate and dimethylimidazole in S101 is 6:4:3.
[0049] In this embodiment, preferably, the temperature increase in S102 is specifically: increasing the temperature to 900° C. at a rate of 3° C.·min.
[0050] Example 2
[0051] See also Figure 1 The present invention provides a technical solution: a method for preparing calamine powder, comprising the following steps:
[0052] S1. Cleaning: The calamine ore raw material was placed in an ultrasonic cleaner, washed with acetic acid aqueous solution for 10 min, filtered, and the obtained solid was washed 4 times to obtain a bright surface of calamine;
[0053] S2 calcination: the cleaned calamine ore was placed in a calciner, calcined at a temperature of 1000 ℃ for 4 hours, and naturally cooled to room temperature to obtain calcined calamine;
[0054] S3 crushing: The calcined calamine was crushed by a grinder and screened through a 120-mesh sieve to obtain calcined calamine powder;
[0055] S4 first grinding: the calcined calamine powder was added to the grinder, an appropriate amount of water was added to the grinder, the grinder was turned on, the calcined calamine powder was ground, the grinder was turned off after grinding, the mixture of calcined calamine powder and water after grinding was allowed to stand for 20 minutes to obtain an upper slurry and a lower calamine powder;
[0056] S5. Second grinding: using a peristaltic pump to pump the upper slurry into the cyclone, by adjusting the power of the peristaltic pump to control the pressure and flow rate at the cyclone inlet, to obtain a calamine slurry with a particle size less than 110 mesh, a calamine slurry with a particle size greater than 110 mesh, discharged from the lower portion of the cyclone into the grinder to continue grinding, the calamine slurry was transported to a settling tank, allowed to stand for 4 hours for stratification, to obtain an upper aqueous solution and a lower calamine powder;
[0057] S6 drying: the lower layer of calamine powder was dehydrated by a dehydrator to obtain calamine powder, the calamine powder was placed in a drying oven at a temperature of 100 ℃ to obtain dried calamine powder;
[0058] S7. Dissolving: At 55°C, under stirring conditions, add 8% by mass of dilute hydrochloric acid to the calamine powder, stir until dissolved, and cool to room temperature;
[0059] S8. Filtration: Filter to remove insoluble solid impurities, add sodium hydroxide solution to the filtrate, stir, let stand and filter;
[0060] S9. Purification: Add porous carbon magnetic adsorption material to the filtrate, stir for 30 minutes, remove the porous carbon magnetic adsorption material with a magnet, adjust the pH of the solution to 9.4 with sodium carbonate, filter, wash the solid with water 4 times, dry the obtained solid at 100°C to a constant temperature, crush it with a grinder, and pass it through a 100-mesh sieve to obtain the calamine powder product.
[0061] In this embodiment, preferably, the power of the ultrasonic cleaner in S1 is 600W, and the mass fraction of the acetic acid aqueous solution is 6%.
[0062] In this embodiment, preferably, the step of adding an appropriate amount of water to the grinder in S3 is as follows: the amount of water is 12 times the amount of the added calcined calamine.
[0063] In this embodiment, preferably, the mass fraction of the sodium hydroxide solution in S8 is 10%, the stirring speed is 400 r / min, the stirring time is 60 min, and the standing time is 40 min.
[0064] In this embodiment, preferably, the preparation method of the porous carbon magnetic adsorption material added in the purification of S9 is:
[0065] S101. Zinc nitrate hexahydrate, ferric acetylacetonate and dimethylimidazole were dissolved in ethanol respectively, and the three solutions were mixed at room temperature to form a milky suspension, which was stirred for 30 min, centrifuged and washed with ethanol, and the mixture was repeated three times to obtain a red precipitate, which was dried at 80°C for 60 min to obtain Fe-ZIF-8 powder;
[0066] S102. Place the Fe-ZIF-8 powder in a tubular furnace and calcine it at elevated temperature for 3 hours under a nitrogen atmosphere to obtain a porous carbon magnetic adsorption material.
[0067] In this embodiment, preferably, the weight ratio of zinc nitrate hexahydrate, ferric acetylacetonate and dimethylimidazole in S101 is 6:4:3.
[0068] In this embodiment, preferably, the temperature increase in S102 is specifically: increasing the temperature to 700° C. at a rate of 3° C.·min.
[0069] Example 3
[0070] See also Figure 1 The present invention provides a technical solution: a method for preparing calamine powder, comprising the following steps:
[0071] S1. Cleaning: The calamine ore raw material was placed in an ultrasonic cleaner, washed with acetic acid aqueous solution for 8 min, filtered, and the obtained solid was washed 3 times to obtain a bright surface of calamine;
[0072] S2 calcination: the cleaned calamine ore was placed in a calciner, calcined at a temperature of 800 ° C for 3 hours, and naturally cooled to room temperature to obtain calcined calamine;
[0073] S3 crushing: The calcined calamine was crushed by a grinder and screened through a 100 mesh sieve to obtain calcined calamine powder;
[0074] S4 first grinding: the calcined calamine powder was added to the grinder, an appropriate amount of water was added to the grinder, the grinder was turned on, the calcined calamine powder was ground, the grinder was turned off after grinding, the mixture of calcined calamine powder and water after grinding was allowed to stand for 18 minutes to obtain an upper slurry and a lower calamine powder;
[0075] S5. Second grinding: using a peristaltic pump to pump the upper slurry into the cyclone, by adjusting the power of the peristaltic pump to control the pressure and flow rate at the cyclone inlet, to obtain a calamine slurry with a particle size less than 110 mesh, a calamine slurry with a particle size greater than 110 mesh, discharged from the lower portion of the cyclone into the grinder to continue grinding, the calamine slurry was transported to a settling tank, allowed to stand for 3 hours for stratification, to obtain an upper aqueous solution and a lower calamine powder;
[0076] S6 drying: the lower layer of calamine powder was dehydrated by a dehydrator to obtain calamine powder, the calamine powder was dried in a drying oven at a temperature of 90 ° C to obtain dried calamine powder;
[0077] S7. Dissolving: Under stirring conditions at 445°C, add 8% dilute hydrochloric acid to the calamine powder, stir until dissolved, and cool to room temperature;
[0078] S8. Filtration: Filter to remove insoluble solid impurities, add sodium hydroxide solution to the filtrate, stir, let stand and filter;
[0079] S9. Purification: Add porous carbon magnetic adsorption material to the filtrate, stir for 20 minutes, remove the porous carbon magnetic adsorption material with a magnet, adjust the solution to pH 9 with sodium carbonate, filter, wash the solid 3 times with water, dry the obtained solid at 90°C to a constant temperature, crush it with a grinder, and pass it through a 90-mesh sieve to obtain the calamine powder product.
[0080] In this embodiment, preferably, the power of the ultrasonic cleaner in S1 is 500W, and the mass fraction of the acetic acid aqueous solution is 4%.
[0081] In this embodiment, preferably, the step of adding an appropriate amount of water to the grinder in S3 is as follows: the amount of water is 10 times the amount of the added calcined calamine.
[0082] In this embodiment, preferably, the mass fraction of the sodium hydroxide solution in S8 is 9%, the stirring speed is 300 r / min, the stirring time is 50 min, and the standing time is 30 min.
[0083] In this embodiment, preferably, the preparation method of the porous carbon magnetic adsorption material added in the purification of S9 is:
[0084] S101. Zinc nitrate hexahydrate, ferric acetylacetonate and dimethylimidazole were dissolved in ethanol respectively, and the three solutions were mixed at room temperature to form a milky suspension, which was stirred for 20 min, centrifuged and washed with ethanol, and the mixture was repeated three times to obtain a red precipitate, which was dried at 60°C for 50 min to obtain Fe-ZIF-8 powder;
[0085] S102. Place the Fe-ZIF-8 powder in a tubular furnace and calcine it at elevated temperature for 2.5 hours under a nitrogen atmosphere to obtain a porous carbon magnetic adsorption material.
[0086] In this embodiment, preferably, the weight ratio of zinc nitrate hexahydrate, ferric acetylacetonate and dimethylimidazole in S101 is 6:4:3.
[0087] In this embodiment, preferably, the temperature increase in S102 is specifically: increasing the temperature to 800° C. at a rate of 4° C.·min.
[0088] Example 4
[0089] See also Figure 2-3 The present invention provides a technical solution: a calamine powder preparation device, comprising a screening box 1, a feeding funnel 2 is connected to the top of the screening box 1, a screening plate 3 is arranged inside the screening box 1, a first feeding port 4 is opened on one side of the screening box 1, and a receiving groove 5 is opened on the other side of the screening box 1, the lower surfaces of both ends of the screening plate 3 are respectively slidably arranged inside the first feeding port 4 and the receiving groove 5, the outer surface of the screening box 1 is welded with a supporting plate 6, and the upper surface of the supporting plate 6 is fixedly provided with a A vibration motor 7 is provided, and the output end of the vibration motor 7 is transmission-connected to the lower surface of one end of the screening plate 3 through a connecting plate 8; a first feeding plate 9 is fixedly provided on the outer side of the first feeding port 4, and a first conveyor belt 10 is provided below the first feeding plate 9; a guide plate 11 is provided at the bottom of the screening box 1, and a second feeding port 12 is provided at the bottom of the guide plate 11; a second feeding plate 13 is fixedly provided on the outer side of the second feeding port 12, and a second conveyor belt 14 is provided below the second feeding plate 13.
[0090] In order to facilitate the screening of the material, in the present embodiment, preferably, the screening plate 3 is configured as a mesh plate, and the screening plate 3 is tiltedly arranged inside the screening box 1 .
[0091] In order to facilitate the vibration motor 7 to drive the screening plate 3 to vibrate and move, in the present embodiment, preferably, the lower surfaces at both ends of the screening plate 3 are fixedly connected with slide plates 15, and the inner bottoms of the first discharge port 4 and the accommodating groove 5 are fixedly provided with slide rails 16, and the bottom of the slide plate 15 is slidably provided on the slide rails 16.
[0092] Principles and advantages of the present invention:
[0093] The method adopted by the present invention is to prepare calamine powder. By cleaning the calamine ore, the cleanliness of the calamine ore can be ensured, and the influence of impurities on the surface of the calamine ore on the preparation of the calamine powder can be reduced. At the same time, through purification treatment, the porous carbon magnetic adsorption material can be used to adsorb heavy metal ions, so that the purity of the prepared calamine powder can be further increased. The preparation device of the present invention can screen the calamine powder through the provided screening plate 3, and the screening plate 3 is driven to vibrate by the vibration motor 7, so that the screening efficiency can be increased and the situation of non-dropping can be prevented. At the same time, by providing a first feeding port 4 and a first conveyor belt 10, unqualified calamine powder can be transported for reprocessing. At the same time, by providing a second feeding port 12 and a second conveyor belt 14, qualified calamine powder can be transported for packaging.
[0094] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing calamine powder, characterized in that: The following steps are involved: S1. Cleaning: The calamine ore raw material is placed in an ultrasonic cleaner, washed with acetic acid aqueous solution for 6-10min, filtered, and the obtained solid is washed 2-4 times to obtain a bright surface of calamine; S2 calcining: the cleaned calamine ore is placed in a calcining furnace, calcined at a temperature of 700-1000 ℃ for 2-4 hours, and naturally cooled to room temperature to obtain calcined calamine; S3 crushing: The calcined calamine was crushed by a grinder and screened through a 80-120 mesh sieve to obtain calcined calamine powder; S4 first grinding: the calcined calamine powder was added to the grinder, an appropriate amount of water was added to the grinder, the grinder was turned on, the calcined calamine powder was ground, the grinder was turned off after grinding, the mixture of calcined calamine powder and water after grinding was allowed to stand for 15-20 minutes to obtain an upper slurry and a lower calamine powder; S5. Second grinding: using a peristaltic pump to pump the upper slurry into the cyclone, by adjusting the power of the peristaltic pump to control the pressure and flow rate at the cyclone inlet, to obtain a calamine slurry with a particle size less than 110 mesh, a calamine slurry with a particle size greater than 110 mesh, discharged from the lower portion of the cyclone into the grinder to continue grinding, the calamine slurry was transported to a settling tank, allowed to stand for 2-4 hours for stratification, to obtain an upper aqueous solution and a lower calamine powder; S6 drying: the lower layer of calamine powder dehydrated by a dehydrator to obtain calamine powder, the calamine powder set temperature in a drying oven 80-100 ℃ for drying, to obtain dried calamine powder; S7. Dissolving: Under stirring conditions at 35-55 ° C, add 8% dilute hydrochloric acid to the calamine powder, stir until dissolved, and cool to room temperature; S8. Filtration: Filter to remove insoluble solid impurities, add sodium hydroxide solution to the filtrate, stir, let stand and filter; S9. Purification: adding a porous carbon magnetic adsorption material to the filtrate, stirring for 15-30 minutes, removing the porous carbon magnetic adsorption material with a magnet, adjusting the solution to pH 8.6-9.4 with sodium carbonate, filtering, washing the solid 2-4 times, drying the obtained solid at 80-100 ° C to a constant temperature, crushing it with a grinder, passing it through a 80-100 mesh sieve, and obtaining a calamine powder product; The preparation method of the porous carbon magnetic adsorption material added in the purification of S9 is: S101. Zinc nitrate hexahydrate, ferric acetylacetonate and dimethylimidazole were dissolved in ethanol respectively, and the three solutions were mixed at room temperature to form a milky suspension, which was stirred for 10-30 min, centrifuged and washed with ethanol, and repeated three times to obtain a red precipitate, which was dried at 50-80°C for 40-60 min to obtain Fe-ZIF-8 powder; S102. Place the Fe-ZIF-8 powder in a tubular furnace and calcine it at elevated temperature for 2-3 hours under a nitrogen atmosphere to obtain a porous carbon magnetic adsorption material.
2. A method for preparing calamine powder according to claim 1, characterized in that: The power of the ultrasonic cleaner in S1 is 400-600W, and the mass fraction of the acetic acid aqueous solution is 3-6%.
3. A method for preparing calamine powder according to claim 1, characterized in that: In the step S4, adding an appropriate amount of water to the grinder is specifically: the amount of water is 8-12 times the amount of the added calcined calamine.
4. A method for preparing calamine powder according to claim 1, characterized in that: The mass fraction of the sodium hydroxide solution in S8 is 8-10%, the stirring speed is 200-400r / min, the stirring time is 40-60min, and the standing time is 20-40min.
5. A method for preparing calamine powder according to claim 1, characterized in that: The weight ratio of zinc nitrate hexahydrate, ferric acetylacetonate and dimethylimidazole in the S101 is 6:4:
3.
6. A method for preparing calamine powder according to claim 1, characterized in that: The temperature increase in S102 is specifically: increasing the temperature to 700-900° C. at a rate of 3-5° C.·min.
Citation Information
Patent Citations
Preparation method of calamine powder
CN114956158A
Preparation method and application of calamine powder
CN115120613A