CN104511207B - Aluminum fluoride trihydrate slurry filtration method - Google Patents
Aluminum fluoride trihydrate slurry filtration method Download PDFInfo
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- CN104511207B CN104511207B CN201310701917.XA CN201310701917A CN104511207B CN 104511207 B CN104511207 B CN 104511207B CN 201310701917 A CN201310701917 A CN 201310701917A CN 104511207 B CN104511207 B CN 104511207B
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- aluminum fluoride
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- fluoride trihydrate
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Abstract
The invention discloses a kind of aluminum fluoride trihydrate slurry filtration method, relate to technical field of aluminum fluoride production, comprise the following steps: the aluminum fluoride trihydrate slurry pipeline transport that hexafluosilicic acid and aluminium hydroxide generate in reactive tank is cushioned to slip feeder trough；Slip delivers to dense groove again, and slip is the dense slip of settlement separate formation and clear liquid in dense groove, and clear liquid overflow goes out to drain in a collecting tank, and dense slip flows out from the bottom of dense groove；Filter through vacuum and obtain aluminum fluoride trihydrate crystalline solid；Clear liquid settles in collecting tank, separates and obtains waste liquid and the underflow containing tiny aluminum fluoride trihydrate crystalline solid, and waste liquid is discharged from collecting tank top, and underflow returns the crystal seed in reactive tank as aluminum fluoride trihydrate crystallization；It is repeated in the operation of above-mentioned steps.The present invention is compared to prior art, improves aluminum fluoride trihydrate crystalline condition, improves slip solid content, improves slurry filtration effect, improve aluminium fluoride productivity.
Description
Technical field
The present invention relates to technical field of aluminum fluoride production, the hexafluosilicic acid of especially a kind of by-product of phosphoric acid plant in a wet process is raw material, produces with A-P wet processing in the production procedure of aluminium fluoride, improves the process of aluminum fluoride trihydrate slurry filtration effect.
Background technology
Domestic aluminium fluoride production technology mainly has dry method, wet method, hexafluosilicic acid method.Aluminum fluoride by dry process production technology is: concentrated sulphuric acid and fluorite reaction, obtains hydrogen fluoride gas, and the purified aluminium hydroxide with drying and dehydrating of hydrogen fluoride gas reacts, and directly obtains aluminium fluoride product.Traditional wet method aluminium fluoride production technology is: concentrated sulphuric acid and fluorite reaction, and the hydrogen fluoride gas of generation is purified, water absorbs and obtains Fluohydric acid., and Fluohydric acid. reacts with aluminum hydroxide slurry and prepares intermediate products AIF3·3H20, AIF3·3H2AIF is prepared after 0 drying dehydration3Product.Hexafluosilicic acid method aluminium fluoride production technology (also known as phosphate fertilizer by-product method) skill is: the waste gas containing fluoride SiF that will produce in production of phosphate fertilizer4Through water cyclic absorption, preparing silicate fluoride solution, silicate fluoride solution reacts with aluminum hydroxide slurry, generates aluminun fluoride solution and silica gel precipitation；Aluminun fluoride solution after separation silica gel carries out crystallization again and obtains AIF3·3H20, AIF3·3H2Finished product aluminium fluoride is prepared after 0 drying and dehydrating.
Owing to dry and wet technique needs to consume fluorite, production cost is high, and environmental pollution is big, and the primary raw material hexafluosilicic acid that hexafluosilicic acid method technique uses derives from the side-product in production of phosphate fertilizer, so production cost is very low, and good product quality, there is very much the market competitiveness.
In the wet method phosphoric acid manufacture process of phosphate fertilizer industry, often produce 1 ton of P2O5By-product fluosilicic acid (100%H2SiF6) about 0.05 ton, for reclaiming this part fluorine resource, Wet-process Phosphoric Acid Production needs auxiliary construction aluminium fluoride device environmental protection facility.It is 22% that the hexafluosilicic acid of traditional Wet Processes of Phosphoric Acid by-product absorbs in the design of liquid concentration, produces aluminium fluoride for aluminium fluoride device.In recent years, due to the decline of phosphorus ore quality, impurity content increases, and causes that hexafluosilicic acid yield declines.Silicate fluoride solution concentration is high, it is easy to reaches to comprise and can not absorb hexafluosilicic acid gas by recirculation, for improving hexafluosilicic acid yield, need to reduce silicate fluoride solution concentration, namely be dropped to 20% by intrinsic 22%.Existing aluminum fluoride trihydrate slurry filtration method is, is entered by the aluminum fluoride trihydrate shurry pump that hexafluosilicic acid and aluminium hydroxide raw material reaction generate after cushioning in slip feeder trough, is directly filtrated to get aluminum fluoride trihydrate crystalline solid.Due to the reduction of silicate fluoride solution concentration, causing that aluminium fluoride slurry liquid concentration reduces, slip solid content is only 20%, causes that aluminium fluoride slurry liquid filter effect is deteriorated, even cannot filter, and the driving rate of device declines, and finally affects product yield and quality.The aluminium fluoride that this method obtains have a daily output of about 12 tons.
Summary of the invention
It is an object of the invention to provide a kind of aluminum fluoride trihydrate slurry filtration method, the problem that this method can solve existing aluminum fluoride trihydrate slurry filtration weak effect.
In order to solve the problems referred to above, the technical solution used in the present invention is: this aluminum fluoride trihydrate slurry filtration method comprises the following steps:
A, the aluminum fluoride trihydrate slurry pipeline transport that hexafluosilicic acid and aluminium hydroxide generate in reactive tank is cushioned to slip feeder trough；
B, buffered slurry pipeline transport are to dense groove, and slip is the dense slip of settlement separate formation and clear liquid in dense groove, and the clear liquid of generation goes out from dense groove top overflow, and drains in a collecting tank, and dense slip flows out from the bottom of dense groove；
C, outflow dense slip through vacuum filter obtain aluminum fluoride trihydrate crystalline solid；
D, clear liquid settle in collecting tank, separate and obtain waste liquid and the underflow containing tiny aluminum fluoride trihydrate crystalline solid, and waste liquid is discharged from collecting tank top, and underflow returns the crystal seed in reactive tank as aluminum fluoride trihydrate crystallization；
E, it is repeated in the operation of above-mentioned steps A to step D.
In the technical scheme of above-mentioned aluminum fluoride trihydrate slurry filtration method, technical scheme is it may also is that the slip sedimentation time of step B is 6 minutes～8 minutes more specifically.
Further, the vacuum pressure in step C is 0.02MPa～0.04MPa.
Owing to have employed technique scheme, the present invention compared with prior art has the advantages that
1, utilize dense groove that aluminum fluoride trihydrate slip is settled, aluminum fluoride trihydrate solution is made to obtain sufficient crystallization time and space, crystalline condition is greatly improved, crystal is neat, thick, the solution solid content of concentration improves, slip solid content reaches about 30%, improves aluminum fluoride trihydrate slurry filtration effect, improves aluminium fluoride product quality.
2, the clear liquid that the overflow of dense groove goes out settles in collecting tank, separates the underflow containing tiny aluminum fluoride trihydrate crystalline solid obtained and returns the interior crystal seed as aluminum fluoride trihydrate crystallization of reactive tank, can improve crystalline condition, improve again aluminium fluoride productivity；Aluminium fluoride yield reaches the daily output of 14～15 tons, and productivity improves about 20%.
3, overcome the deficiency of A-P wet production aluminium fluoride technique, it is possible to use the hexafluosilicic acid raw material of lower concentration, improve the aluminium fluoride device adaptability to low dose fluoride silicic acid.
4, due to the reduction of hexafluosilicic acid concentration, improve hexafluosilicic acid yield for phosphoric acid plant fluorine recovery system and create advantage.
5, vacuum pressure arranges and ranges for 0.02MPa～0.04MPa, can reach the filter effect of the best, slurry can be made to reach best solid, liquid separating effect.
Accompanying drawing explanation
Fig. 1 is the flow chart of this aluminum fluoride trihydrate slurry filtration method.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the invention will be further described:
Embodiment 1
The equipment that aluminum fluoride trihydrate slurry filtration flow process shown in Fig. 1 uses mainly includes reactive tank 1, shurry pump 2, slip feeder trough 3, feed pump 4, dense groove 5, slurries filtration machine 6, vacuum pump 7 and collecting tank 8；Reactive tank 1 is connected with slip feeder trough 3 by shurry pump 2, and slip feeder trough 3 is connected with dense groove 5 by feed pump 4, and the overfall of dense groove 5 connects with collecting tank 8；Collecting tank 8 is that a top is provided with overfall, bottom is provided with the cell body of discharging opening, and the overfall of collecting tank 8 is connected to wastewater disposal basin by pipeline, and the discharging opening of collecting tank 8 connects with reactive tank 8；The discharging opening of dense groove 8 connects with slurries filtration machine 6, and slurries filtration machine 6 adopts rotary drum vacuum filter, and rotary drum vacuum filter carries out evacuation by the vacuum pump 7 being attached thereto.
Aluminum fluoride trihydrate slurry filtration step in the present embodiment is as follows:
A, aluminum fluoride trihydrate slip hexafluosilicic acid and aluminium hydroxide raw material generated in reactive tank are delivered to slip feeder trough through shurry pump and cushion, and increase crystalline spaces；
B, buffered slip are delivered to dense groove through feed pump, after slip settles 6 minutes in dense groove, separate and form dense slip and clear liquid, and the clear liquid of generation goes out from dense groove top overflow, and drains in a collecting tank, and dense slip flows out from the bottom of dense groove；Slip crystalline solid after concentration improves, and crystal is neat, thick, and the dense slip solid content gone out from dense concentrated flow is improved；
C, outflow dense slip enter slurry filtration machine and carry out vacuum filtration, vacuum pressure controls as 0.02MPa, filters and obtains aluminum fluoride trihydrate crystalline solid and deliver to subsequent processing again and be processed further；
D, clear liquid settle in collecting tank, separating and obtain waste liquid and the underflow containing tiny aluminum fluoride trihydrate crystalline solid, waste liquid drains into wastewater disposal basin from collecting tank top, and underflow returns the crystal seed in reactive tank as aluminum fluoride trihydrate crystallization, crystalline condition can be improved, improve again aluminium fluoride productivity；
E, it is repeated in the operation of above-mentioned steps A to step D.
After testing, in the present embodiment, the dense slip solid content gone out from dense concentrated flow reaches 29%, aluminium fluoride have a daily output of 14 tons.
Embodiment 2
In the present embodiment, after the slip in step B settles 8 minutes in dense groove；Vacuum pressure in step C controls as 0.04Mpa；All the other features are identical with embodiment 1.
After testing, in the present embodiment, the dense slip solid content gone out from dense concentrated flow reaches 30%, crystal neat, thick (parameter), aluminium fluoride have a daily output of 15 tons.
Claims (3)
1. an aluminum fluoride trihydrate slurry filtration method, it is characterised in that comprise the following steps:
A, the aluminum fluoride trihydrate slurry pipeline transport that hexafluosilicic acid and aluminium hydroxide generate in reactive tank is cushioned to slip feeder trough；
B, buffered slurry pipeline transport are to dense groove, and slip is the dense slip of settlement separate formation and clear liquid in dense groove, and the clear liquid of generation goes out from dense groove top overflow, and drains in a collecting tank, and dense slip flows out from the bottom of dense groove；
C, outflow dense slip through vacuum filter obtain aluminum fluoride trihydrate crystalline solid；
D, clear liquid settle in collecting tank, separate and obtain waste liquid and the underflow containing tiny aluminum fluoride trihydrate crystalline solid, and waste liquid is discharged from collecting tank top, and underflow returns the crystal seed in reactive tank as aluminum fluoride trihydrate crystallization；
E, it is repeated in the operation of above-mentioned steps A to step D.
2. aluminum fluoride trihydrate slurry filtration method according to claim 1, it is characterised in that: the slip sedimentation time of step B is 5 minutes～7 minutes.
3. aluminum fluoride trihydrate slurry filtration method according to claim 1 and 2, it is characterised in that: the vacuum pressure in step C is 0.02MPa～0.04MPa.
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| CN201310701917.XA CN104511207B (en) | 2013-12-19 | 2013-12-19 | Aluminum fluoride trihydrate slurry filtration method |
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| CN201310701917.XA CN104511207B (en) | 2013-12-19 | 2013-12-19 | Aluminum fluoride trihydrate slurry filtration method |
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| CN104511207B true CN104511207B (en) | 2016-07-13 |
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| CN115010157A (en) * | 2022-06-22 | 2022-09-06 | 中石化南京工程有限公司 | System and method for producing anhydrous aluminum fluoride by using fluosilicic acid |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5427757A (en) * | 1990-12-31 | 1995-06-27 | Phosphate Engineering And Construction Co. | Process for the production of phosphoric acid and hydrogen fluoride from phosphate rock and fluosilicic acid |
| JP4316393B2 (en) * | 2004-01-21 | 2009-08-19 | 森田化学工業株式会社 | Calcium fluoride manufacturing method, recycling method and recycling method |
| CN101591031A (en) * | 2008-05-26 | 2009-12-02 | 贵阳铝镁设计研究院 | Preparation process for high-white aluminum hydroxide |
| CN102398913A (en) * | 2010-09-14 | 2012-04-04 | 贵阳铝镁设计研究院有限公司 | Process for extracting metallurgical grade alumina through treatment of high alumina fly ash by using sulfuric acid method |
| CN202687999U (en) * | 2012-08-16 | 2013-01-23 | 贵阳铝镁设计研究院有限公司 | High-sulfur seed precipitation mother liquor intensified salt elimination and desulfurization production device |
| CN203678138U (en) * | 2013-12-19 | 2014-07-02 | 广西鹿寨化肥有限责任公司 | Aluminum fluoride trihydrate slurry filtering equipment |
-
2013
- 2013-12-19 CN CN201310701917.XA patent/CN104511207B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5427757A (en) * | 1990-12-31 | 1995-06-27 | Phosphate Engineering And Construction Co. | Process for the production of phosphoric acid and hydrogen fluoride from phosphate rock and fluosilicic acid |
| JP4316393B2 (en) * | 2004-01-21 | 2009-08-19 | 森田化学工業株式会社 | Calcium fluoride manufacturing method, recycling method and recycling method |
| CN101591031A (en) * | 2008-05-26 | 2009-12-02 | 贵阳铝镁设计研究院 | Preparation process for high-white aluminum hydroxide |
| CN102398913A (en) * | 2010-09-14 | 2012-04-04 | 贵阳铝镁设计研究院有限公司 | Process for extracting metallurgical grade alumina through treatment of high alumina fly ash by using sulfuric acid method |
| CN202687999U (en) * | 2012-08-16 | 2013-01-23 | 贵阳铝镁设计研究院有限公司 | High-sulfur seed precipitation mother liquor intensified salt elimination and desulfurization production device |
| CN203678138U (en) * | 2013-12-19 | 2014-07-02 | 广西鹿寨化肥有限责任公司 | Aluminum fluoride trihydrate slurry filtering equipment |
Non-Patent Citations (1)
| Title |
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| "A-P湿法氟化铝生产工艺的改进与优化";欧建冬等;《硫磷设计与粉体工程》;20110131;第42-45页 * |
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