CN221275526U - System for high-efficient recovery fluorine resource in follow photovoltaic fluorine-containing acid pickle - Google Patents
System for high-efficient recovery fluorine resource in follow photovoltaic fluorine-containing acid pickle Download PDFInfo
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- CN221275526U CN221275526U CN202322970766.XU CN202322970766U CN221275526U CN 221275526 U CN221275526 U CN 221275526U CN 202322970766 U CN202322970766 U CN 202322970766U CN 221275526 U CN221275526 U CN 221275526U
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 142
- 239000011737 fluorine Substances 0.000 title claims abstract description 142
- 239000002253 acid Substances 0.000 title claims abstract description 81
- 238000011084 recovery Methods 0.000 title claims abstract description 79
- 235000021110 pickles Nutrition 0.000 title claims description 16
- 239000007788 liquid Substances 0.000 claims abstract description 66
- 239000002699 waste material Substances 0.000 claims abstract description 55
- 238000004064 recycling Methods 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims description 53
- 239000012065 filter cake Substances 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 238000000926 separation method Methods 0.000 claims description 30
- 239000010865 sewage Substances 0.000 claims description 27
- 238000003828 vacuum filtration Methods 0.000 claims description 25
- 239000000706 filtrate Substances 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 17
- 238000004062 sedimentation Methods 0.000 claims description 12
- 238000001802 infusion Methods 0.000 claims description 11
- 238000004806 packaging method and process Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000012856 packing Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000006210 lotion Substances 0.000 claims 7
- 238000000034 method Methods 0.000 abstract description 7
- 238000011282 treatment Methods 0.000 abstract description 5
- 239000002910 solid waste Substances 0.000 abstract description 3
- 239000007787 solid Substances 0.000 description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 8
- 229910052700 potassium Inorganic materials 0.000 description 8
- 239000011591 potassium Substances 0.000 description 8
- 238000010248 power generation Methods 0.000 description 6
- 239000012295 chemical reaction liquid Substances 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 4
- 229910001634 calcium fluoride Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000011112 process operation Methods 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910004074 SiF6 Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 description 2
- 235000011151 potassium sulphates Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004334 fluoridation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004148 unit process Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Abstract
The utility model relates to the technical field of resource recovery in waste acid liquid, in particular to a system for efficiently recovering fluorine resources from photovoltaic fluorine-containing waste acid liquid. In the system for efficiently recycling the fluorine resources from the photovoltaic fluorine-containing waste acid liquid, the operation method is simple, safe and reliable, no new solid waste is generated, the cost is saved, the environment is protected, the fluorine resources in the photovoltaic fluorine-containing waste acid liquid can be efficiently recycled through two reaction treatments, the comprehensive recycling of the fluorine resources in the photovoltaic waste acid is realized, and the waste is changed into valuable.
Description
Technical Field
The utility model relates to the technical field of resource recovery in waste acid liquid, in particular to a system for efficiently recovering fluorine resources from photovoltaic fluorine-containing waste acid liquid.
Background
Along with the continuous progress of human civilization, the development of technology is continuous, and various energy sources are continuously exhausted. In recent years, scientific researchers have largely explored the energy field, and solar energy is favored by people because of safety, environmental protection, inexhaustibility and inexhaustibility, and solar power generation comprises photovoltaic power generation, photochemical power generation and photo-induction power generation, wherein photovoltaic power generation is the main stream of solar power generation nowadays. From the beginning of the 21 st century, the photovoltaic industry in China is developed rapidly with high quality under the strong support of national policies, and according to statistics, the yield of the photovoltaic modules in China is 15 years in the first place of the world continuously, the yield of polysilicon is 11 years in the first place of the world continuously, the newly added loading is 9 years in the first place of the world continuously, and the cumulative loading is 7 years in the first place of the world continuously. However, a large amount of fluorine-containing waste acid is generated in the etching and acid washing processes of the photovoltaic cell manufacturing process, and according to statistics, more than 45 ten thousand tons of photovoltaic fluorine-containing waste acid can be generated in China each year, so that the fluorine resource loss is caused, and the more serious the water pollution is.
The photovoltaic fluorine-containing waste acid is a main waste liquid generated in the photovoltaic industry, and mainly generated in the working procedures of texturing and etching of the polycrystalline silicon solar cell, pickling and etching of the monocrystalline silicon solar cell and the like. The content of the fluorine-containing waste acid component of the photovoltaic cell can be different according to the type and the process of the photovoltaic cell, but the generated waste acid component is basically the same, and generally contains a large amount of fluosilicic acid, hydrofluoric acid, nitric acid, sulfuric acid, hydrochloric acid and a very small amount of metal salt. Unlike fluoride-containing waste water produced in smelting, fluoridation, acid washing of steel, phosphate fertilizer and other industries, the photovoltaic fluoride-containing waste acid has the outstanding characteristics of large water quantity, extremely high fluoride concentration, complex pollution components, high treatment difficulty, low metal impurity content and the like. The research on recycling of the high-concentration fluorine-containing waste acid can relieve the pollution of the waste acid produced by the photovoltaic manufacturing industry to the environment, and simultaneously, a large amount of important fluorine resources can be effectively regenerated, so that the green production of the photovoltaic industry is promoted, the green economic development of the clean energy full-industry chain is realized by assistance, and a large amount of important available fluorine resources can be provided for the chemical industry of China.
At present, the treatment of the photovoltaic fluorine-containing acid pickle becomes a difficult problem for enterprises. If the photovoltaic fluorine-containing waste acid liquid is directly discharged to a waste water treatment system, a great amount of waste is caused, and meanwhile, the environment pollution is also caused.
Disclosure of utility model
The utility model aims to provide a system for efficiently recycling fluorine resources from photovoltaic fluorine-containing acid pickle, so as to solve the problem that the treatment of the photovoltaic fluorine-containing acid pickle in the background technology is faced by enterprises. If the photovoltaic fluorine-containing waste acid liquid is directly discharged to a wastewater treatment system, a great amount of waste is caused, and meanwhile, the problem of environmental pollution is also caused.
In order to achieve the above purpose, the utility model provides a system for efficiently recovering fluorine resources from photovoltaic fluorine-containing spent acid liquid, which comprises a first fluorine resource recovery unit and a second fluorine resource recovery unit, wherein the first fluorine resource recovery unit and the second fluorine resource recovery unit are mutually communicated, the input end of the first fluorine resource recovery unit is connected with a fluorine-containing spent acid liquid ultrasonic settling tank, the input end of the fluorine-containing spent acid liquid ultrasonic settling tank is connected with a pure water overhead tank, and the sewage output ends of the first fluorine resource recovery unit and the second fluorine resource recovery unit are both connected to a sewage collecting tank.
Preferably, the first fluorine resource recovery unit comprises a first reaction kettle, the output end of the first reaction kettle is connected with a first vacuum filtration solid-liquid separation filter device, the output end of the first vacuum filtration solid-liquid separation filter device is connected with a first filter cake washing tank, the product output end of the first filter cake washing tank is connected with a first drying device, and the output end of the first drying device is connected with a first packing machine; the second fluorine resource recovery unit comprises a second reaction kettle, the output end of the second reaction kettle is connected with a second vacuum filtration solid-liquid separation filter device, the output end of the second vacuum filtration solid-liquid separation filter device is connected with a second filter cake washing tank, the product output end of the second filter cake washing tank is connected with a second drying device, and the output end of the second drying device is connected with a second packaging machine.
Preferably, the first vacuum filtration solid-liquid separation filter device is connected with the second reaction kettle, so that the first fluorine resource recovery unit and the second fluorine resource recovery unit form a communicated system.
Preferably, the first fluorine resource recovery unit further comprises a first washing liquor recovery tank, the sewage output end of the first filter cake washing tank is connected to the first washing liquor recovery tank, the clean water output end of the first washing liquor recovery tank is connected to the input end of the fluorine-containing waste acid liquid ultrasonic sedimentation tank, the sewage output end of the first washing liquor recovery tank is connected to the sewage collection tank, the second fluorine resource recovery unit further comprises a second washing liquor recovery tank, the sewage output end of the second washing liquor recovery tank is connected to the sewage collection tank, the clean water output end of the second washing liquor recovery tank is connected to the input end of the second reaction kettle, and valves and liquid conveying pumps are arranged on connected pipelines.
Preferably, a filtrate discharge port of the second vacuum filtration solid-liquid separation filter device is connected with a filtrate recovery tank, and an output end of the filtrate recovery tank is connected with an input end of the second reaction kettle through a pipeline.
Preferably, the fluorine-containing waste acid liquid ultrasonic sedimentation tank comprises a feed inlet and a water inlet, fluorine-containing waste acid enters the fluorine-containing waste acid liquid ultrasonic sedimentation tank through the feed inlet, the pure water elevated tank is connected with the water inlet through a pipeline, and the pure water elevated tank provides water for the device so as to adjust the concentration of a reaction system or a cleaning device.
Preferably, the first reaction kettle and the second reaction kettle are both provided with a stirring device, a liquid level meter, a manhole, a feed port and a sight glass.
Preferably, the first filter cake washing tank and the second filter cake washing tank are two or more stages of washing tanks.
Compared with the prior art, the utility model has the beneficial effects that:
In the system for efficiently recycling fluorine resources from the photovoltaic fluorine-containing waste acid liquid, the operation method is simple, safe and reliable, no new solid waste is generated, the cost is saved, the environment is protected, the fluorine resources in the photovoltaic fluorine-containing waste acid liquid can be efficiently recycled through two reaction treatments, the comprehensive recycling of the fluorine resources in the photovoltaic waste acid is realized, the waste is changed into valuable, the green production of the photovoltaic industry can be promoted, and the green economic development of the clean energy full-industry chain is realized by aid of assistance.
Drawings
FIG. 1 is a schematic diagram of the overall structure of the present utility model;
FIG. 2 is a schematic diagram of the structure of a first fluorine resource recovery unit of the present utility model;
Fig. 3 is a schematic structural diagram of a second fluorine resource recovery unit in the present utility model.
The meaning of each reference sign in the figure is:
1. A first fluorine resource recovery unit; 11. a first reaction kettle; 12. a first vacuum filtration solid-liquid separation filter device; 13. a first filter cake wash tank; 14. a first drying device; 15. a first wash recovery tank; 16. a first packaging machine; 2. a second fluorine resource recovery unit; 21. a second reaction kettle; 22. a second vacuum filtration solid-liquid separation filter device; 23. a second filter cake wash tank; 24. a second drying device; 25. a second wash recovery tank; 26. a filtrate recovery tank; 27. a second packaging machine; 3. a pure water elevated tank; 4. ultrasonic wave settling tank of fluorine-containing acid pickle; 5. and a sewage collecting tank.
Detailed Description
The following description of the embodiments of the present utility model will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
Example 1
The utility model provides a system for efficiently recycling fluorine resources from photovoltaic fluorine-containing waste acid liquid, which is shown in figures 1-3, and comprises a first fluorine resource recycling unit 1 and a second fluorine resource recycling unit 2, wherein the first fluorine resource recycling unit 1 and the second fluorine resource recycling unit 2 are mutually communicated, the input end of the first fluorine resource recycling unit 1 is connected with a fluorine-containing waste acid liquid ultrasonic settling tank 4, the input end of the fluorine-containing waste acid liquid ultrasonic settling tank 4 is connected with a pure water overhead tank 3, and the sewage output ends of the first fluorine resource recycling unit 1 and the second fluorine resource recycling unit 2 are both connected to a sewage collecting tank 5.
In this embodiment, the first fluorine resource recovery unit 1 includes a first reaction kettle 11, an output end of the first reaction kettle 11 is connected with a first vacuum filtration solid-liquid separation filter device 12, an output end of the first vacuum filtration solid-liquid separation filter device 12 is connected with a first filter cake washing tank 13, a product output end of the first filter cake washing tank 13 is connected with a first drying device 14, and an output end of the first drying device 14 is connected with a first packing machine 16; the second fluorine resource recovery unit 2 comprises a second reaction kettle 21, the output end of the second reaction kettle 21 is connected with a second vacuum filtration solid-liquid separation filter device 22, the output end of the second vacuum filtration solid-liquid separation filter device 22 is connected with a second filter cake washing tank 23, the product output end of the second filter cake washing tank 23 is connected with a second drying device 24, the output end of the second drying device 24 is connected with a second packing machine 27, fluorine-containing waste acid enters the fluorine-containing waste acid ultrasonic sedimentation tank 4 through a feed inlet of the fluorine-containing waste acid ultrasonic sedimentation tank 4, a water outlet of the pure water high-level tank 3 is connected with a water inlet of the fluorine-containing waste acid ultrasonic sedimentation tank 4 through a pipeline, an outlet of the fluorine-containing waste acid ultrasonic sedimentation tank 4 is connected with the first reaction kettle 11 through a pipeline, waste acid enters the first reaction kettle 11 for reaction, the reaction liquid enters the first vacuum filtration solid-liquid separation filter device 12 for suction filtration and separation, solid and filtrate are obtained after the reaction, the solid is washed by the first filter cake washing tank 13 and then dried by the first drying device 14, the product 1 is obtained, the fluorine-containing waste acid is produced by the first fluorine resource unit 1 enters the second reaction unit 2 for recovery of the fluorine resource recovery unit, and the second recovery unit 2 is obtained.
Specifically, the first vacuum filtration solid-liquid separation filter device 12 is connected to the second reaction vessel 21, so that the first fluorine resource recovery unit 1 and the second fluorine resource recovery unit 2 form a communicated system.
Further, the first fluorine resource recovery unit 1 further comprises a first washing liquor recovery tank 15, the sewage output end of the first filter cake washing tank 13 is connected to the first washing liquor recovery tank 15, the clean water output end of the first washing liquor recovery tank 15 is connected to the input end of the fluorine-containing waste acid liquid ultrasonic sedimentation tank 4, the sewage output end of the first washing liquor recovery tank 15 is connected to the sewage collection tank 5, the second fluorine resource recovery unit 2 further comprises a second washing liquor recovery tank 25, the sewage output end of the second washing liquor recovery tank 25 is connected to the sewage collection tank 5, the clean water output end of the second washing liquor recovery tank 25 is connected to the input end of the second reaction kettle 21, and valves and liquid pumps are arranged on the connected pipelines.
Further, a filtrate discharge port of the second vacuum filtration solid-liquid separation filter device 22 is connected with a filtrate recovery tank 26, and an output end of the filtrate recovery tank 26 is connected with an input end of the second reaction kettle 21 through a pipeline.
Further, the fluorine-containing acid pickle ultrasonic settling tank 4 comprises a feed inlet and a water inlet, fluorine-containing acid pickle ultrasonic settling tank 4 enters through the feed inlet, the pure water high-level tank 3 is connected with the water inlet through a pipeline, and the pure water high-level tank 3 provides water for the device so as to adjust the concentration of a reaction system or a cleaning device.
Further, the first reaction kettle 11 and the second reaction kettle 21 are respectively provided with a stirring device, a liquid level meter, a manhole, a feed port and a sight glass.
Further, the first cake washing tank 13 and the second cake washing tank 23 are two or more stages of washing tanks.
Example 2
The composition of this example is H 2SiF6：17.60％,HF：4.94％,H2SO4：3.34％,HCl：0.03％,HNO3: 2.23% of photovoltaic fluorine-containing waste acid is used as a raw material. The photovoltaic fluorine-containing waste acid and the potassium sulfate solid are added into the first reaction kettle 11 to react to prepare a potassium fluosilicate product, and the filtrate produced in the previous step and the calcium oxide solid are added into the second reaction kettle 21 to react to prepare a calcium fluoride product.
The first fluorine resource unit recovery process operation, namely the process operation for preparing potassium fluosilicate:
The method comprises the steps of storing the photovoltaic fluorine-containing waste acid in a fluorine-containing waste acid ultrasonic sedimentation tank 4, conveying 500.00kg of the photovoltaic fluorine-containing waste acid into a first reaction kettle 11 through an infusion pump, opening a water outlet valve of a pure water overhead tank 3, adding 468.27kg of water into the fluorine-containing waste acid ultrasonic sedimentation tank 4, opening a stirring device of the first reaction kettle 11, preheating the temperature in the kettle to 40 ℃, slowly adding 117.07kg of potassium sulfate solid into a feed inlet of the reaction kettle, and stirring for reaction at the reaction temperature of 40 ℃ for 2 hours.
After the reaction is finished, the reaction liquid is sent to a first vacuum filtration solid-liquid separation filter device 12 through an infusion pump to carry out suction filtration and separation on solid and liquid, so as to obtain filtrate and filter cakes, the filtrate is sent to a second reaction kettle 21 through the infusion pump, the filter cakes are sent to a first filter cake washing tank 13 to carry out classified washing, washing liquid is recycled or the washing liquid is sent to a sewage collecting tank 5 through the delivery pump, the washed filter cakes are sent to a first drying device 14 to be dried to constant weight at 105 ℃, so as to obtain the product potassium fluosilicate, and the product is packaged by a first packaging machine 16.
A second fluorine resource unit recovery process operation, namely a process operation for preparing calcium fluoride:
300.00kg of filtrate generated by the first recovery fluorine resource unit 1 is added into the second reaction kettle 21 through a conveying pump, a stirring device of the second reaction kettle 21 is opened, the temperature in the kettle is preheated to 30 ℃, 14.31kg of calcium oxide powder is slowly added into a feeding port of the reaction kettle, and the reaction is stirred for 3 hours at the reaction temperature of 30 ℃.
After the reaction is finished, the reaction liquid is sent to a second vacuum filtration solid-liquid separation filter device 22 through an infusion pump to carry out suction filtration and separation on solid and liquid, filtrate and filter cakes are obtained, the filtrate is sent to a second reaction kettle 21 or a sewage collecting tank 5 through the infusion pump, the filter cakes are sent to a second filter cake washing tank 23 to carry out classified washing, washing liquid is recycled or washing liquid is sent to the sewage collecting tank 5 through the conveying pump, the washed filter cakes are sent to a second drying device 24 to be dried to constant weight at 105 ℃, and the product calcium fluoride is obtained, and is packaged by a second packaging machine 27.
And (3) through analysis and detection: the potassium fluosilicate content of the product is up to 99.16%, the calcium fluoride content in the filter cake 2 is 97.31%, and the total fluorine yield is 95.13%.
Example 3
The present embodiment provides a composition of H 2SiF6：21.16％,HF：8.40％,H2SO4：4.50％,HCl：1.62％,HNO3: 1.57 percent of photovoltaic fluorine-containing waste acid with the rest of water as raw material. The fluosilicic acid solution is prepared by adding the photovoltaic fluorine-containing waste acid and silicon dioxide powder into the first reaction kettle 11 to react, and the fluosilicic acid solution prepared in the previous step and 20% potassium chloride solution are added into the second reaction kettle 21 to react to prepare a potassium fluosilicate product.
The first recovery fluorine resource unit process operation, namely the process operation for preparing the fluosilicic acid solution:
The photovoltaic fluorine-containing waste acid is stored in a fluorine-containing waste acid ultrasonic settling tank 4, 500.00kg of the photovoltaic fluorine-containing waste acid is sent to a first reaction kettle 11 through an infusion pump, a stirring device of the first reaction kettle 11 is started, the temperature in the kettle is preheated to 40 ℃, 25.20kg of silicon dioxide powder is slowly added into a feed inlet of the reaction kettle, and stirring reaction is carried out at normal temperature for 1 hour.
After the reaction is finished, the reaction liquid is sent to a first vacuum filtration solid-liquid separation filter device 12 through an infusion pump to carry out suction filtration and separation on solid and liquid, so that fluosilicic acid solution and filter residues are obtained, and the fluosilicic acid solution is sent to a second reaction kettle 21 through the infusion pump, and the filter residues are recycled.
And a second fluorine resource unit recovery process operation, namely a process operation for preparing potassium fluosilicate:
300.00kg of fluosilicic acid solution generated by the first recovery fluorine resource unit is added into the second reaction kettle 21 through a conveying pump, a stirring device of the second reaction kettle 21 is opened, the temperature in the kettle is preheated to 40 ℃, 157.20kg of 20% potassium chloride solution is slowly added into a feed port of the reaction kettle, and the reaction is stirred for 2 hours at the reaction temperature of 40 ℃.
After the reaction is finished, the reaction liquid is sent to a second vacuum filtration solid-liquid separation filter device 22 through an infusion pump to carry out suction filtration and separation on solid and liquid, so as to obtain filtrate and filter cakes, the filtrate is sent to a second reaction kettle 21 or a sewage collecting tank 5 through the infusion pump, the filter cakes are sent to a second filter cake washing tank 23 to carry out classified washing, washing liquid is recycled or washing liquid is sent to the sewage collecting tank 5 through the conveying pump, the washed filter cakes are sent to a second drying device 24 to be dried to constant weight at 105 ℃, so as to obtain a potassium fluosilicate product, and the product is packaged by a second packaging machine 27.
And (3) through analysis and detection: the potassium fluosilicate content of the product is up to 99.60 percent, and the total fluorine yield is 96.05 percent.
The embodiment realizes the high-efficiency recycling of fluorine resources in fluorine-containing waste acid in the photovoltaic industry, has simple and reliable operation method, does not generate new solid waste, and has the characteristics of safety and environmental protection.
Finally, it should be noted that, in the present embodiment, the first packaging machine 16, the second packaging machine 27, and the like, the electronic components in the above components are all common standard components or components known to those skilled in the art, the structure and principle thereof are all known to those skilled in the art through technical manuals or known through routine experiment methods, at the idle position of the present device, all the electrical components are connected through wires, and the specific connection means should refer to the sequence of operation between the electrical components in the working principle to complete the electrical connection, which is known in the art.
The foregoing has shown and described the basic principles, principal features and advantages of the utility model. It will be understood by those skilled in the art that the present utility model is not limited to the above-described embodiments, and that the above-described embodiments and descriptions are only preferred embodiments of the present utility model, and are not intended to limit the utility model, and that various changes and modifications may be made therein without departing from the spirit and scope of the utility model as claimed. The scope of the utility model is defined by the appended claims and equivalents thereof.
Claims (8)
1. A system for efficiently recycling fluorine resources from photovoltaic fluorine-containing acid pickle is characterized in that: including first fluorine resource recovery unit (1) and second fluorine resource recovery unit (2), first fluorine resource recovery unit (1) and second fluorine resource recovery unit (2) are linked together, the input of first fluorine resource recovery unit (1) is connected with fluorine-containing spent acid liquid ultrasonic wave subsider (4), the input of fluorine-containing spent acid liquid ultrasonic wave subsider (4) is connected with pure water elevated tank (3), the sewage output of first fluorine resource recovery unit (1) and second fluorine resource recovery unit (2) all is connected to sewage collecting tank (5).
2. The system for efficiently recovering fluorine resources from a photovoltaic fluorine-containing acid pickle of claim 1, wherein the system comprises: the first fluorine resource recovery unit (1) comprises a first reaction kettle (11), the output end of the first reaction kettle (11) is connected with a first vacuum filtration solid-liquid separation filter device (12), the output end of the first vacuum filtration solid-liquid separation filter device (12) is connected with a first filter cake washing tank (13), the product output end of the first filter cake washing tank (13) is connected with a first drying device (14), and the output end of the first drying device (14) is connected with a first packing machine (16); the second fluorine resource recovery unit (2) comprises a second reaction kettle (21), the output end of the second reaction kettle (21) is connected with a second vacuum filtration solid-liquid separation filter device (22), the output end of the second vacuum filtration solid-liquid separation filter device (22) is connected with a second filter cake washing tank (23), the product output end of the second filter cake washing tank (23) is connected with a second drying device (24), and the output end of the second drying device (24) is connected with a second packaging machine (27).
3. The system for efficiently recovering fluorine resources from a photovoltaic fluorine-containing acid pickle according to claim 2, wherein: the first vacuum filtration solid-liquid separation filter device (12) is connected with the second reaction kettle (21), so that the first fluorine resource recovery unit (1) and the second fluorine resource recovery unit (2) form a communicated system.
4. The system for efficiently recovering fluorine resources from a photovoltaic fluorine-containing acid pickle according to claim 2, wherein: the first fluorine resource recovery unit (1) still includes first lotion recovery pond (15), the sewage output of first filter cake washing tank (13) is connected to first lotion recovery pond (15), the clear water output of first lotion recovery pond (15) is connected to the input of fluorine-containing spent acid liquid ultrasonic wave subsider (4), the sewage output of first lotion recovery pond (15) is connected to sewage collecting tank (5), second fluorine resource recovery unit (2) still includes second lotion recovery pond (25), the sewage output of second lotion recovery pond (25) is connected to sewage collecting tank (5), the clear water output of second lotion recovery pond (25) is connected to the input of second reation kettle (21), all is provided with valve and infusion pump on the pipeline of connection.
5. The system for efficiently recovering fluorine resources from photovoltaic fluorine-containing acid pickle of claim 3, wherein: the filtrate discharge port of the second vacuum filtration solid-liquid separation filter device (22) is connected with a filtrate recovery tank (26), and the output end of the filtrate recovery tank (26) is connected with the input end of the second reaction kettle (21) through a pipeline.
6. The system for efficiently recovering fluorine resources from a photovoltaic fluorine-containing acid pickle of claim 1, wherein the system comprises: the fluorine-containing waste acid liquid ultrasonic sedimentation tank (4) comprises a feed inlet and a water inlet, fluorine-containing waste acid enters the fluorine-containing waste acid liquid ultrasonic sedimentation tank (4) through the feed inlet, the pure water elevated tank (3) is connected with the water inlet through a pipeline, and the pure water elevated tank (3) provides water for the device so as to adjust the concentration of a reaction system or the cleaning device.
7. The system for efficiently recovering fluorine resources from a photovoltaic fluorine-containing acid pickle according to claim 2, wherein: the first reaction kettle (11) and the second reaction kettle (21) are respectively provided with a stirring device, a liquid level meter, a manhole, a feed inlet and a sight glass.
8. The system for efficiently recovering fluorine resources from a photovoltaic fluorine-containing acid pickle according to claim 2, wherein: the first filter cake washing tank (13) and the second filter cake washing tank (23) are two or more than two washing tanks.
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| Publication Number | Publication Date |
|---|---|
| CN221275526U true CN221275526U (en) | 2024-07-05 |
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