CN107715549B - Potassium fluosilicate/sodium fluosilicate separation device and application thereof - Google Patents
Potassium fluosilicate/sodium fluosilicate separation device and application thereof Download PDFInfo
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- CN107715549B CN107715549B CN201710804597.9A CN201710804597A CN107715549B CN 107715549 B CN107715549 B CN 107715549B CN 201710804597 A CN201710804597 A CN 201710804597A CN 107715549 B CN107715549 B CN 107715549B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/01—Filters with filtering elements which move during the filtering operation with translationally moving filtering elements, e.g. pistons
- B01D33/03—Filters with filtering elements which move during the filtering operation with translationally moving filtering elements, e.g. pistons with vibrating filter elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/04—Combinations of filters with settling tanks
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
- C01B25/223—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen only one form of calcium sulfate being formed
- C01B25/225—Dihydrate process
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Abstract
The invention discloses a potassium fluosilicate/sodium separation device and application thereof, wherein the separation device is arranged at the bottom of a flash cooling slurry return pipe and comprises a separation pipe, the separation pipe comprises an inlet section and an outlet section, a gate valve is arranged between the inlet section and the outlet section, the outlet of the outlet section is provided with the gate valve, a screening device is arranged outside the outlet of the outlet section of the separation pipe, and a spraying device is arranged between the screening device and the outlet of the separation pipe. The potassium fluosilicate/sodium separation device provided by the invention is simple in structure and convenient to use, and can effectively separate potassium fluosilicate/sodium scaling substances from reaction slurry by being arranged at the bottom of the flash cooling slurry return pipe, so that the damage of the potassium sodium salt scaling substances to a reaction tank and a pipeline is avoided, and the production efficiency is improved.
Description
Technical Field
The invention relates to a separation device and application thereof, in particular to a potassium/sodium fluosilicate separation device and application thereof, and belongs to the technical field of wet-process phosphoric acid production equipment.
Background
Phosphoric acid is a basic raw material for preparing various industrial and agricultural phosphorus products, and the production processes of phosphoric acid at home and abroad mainly comprise a hot method and a wet method at present, and compared with the hot method and the wet method, the wet method phosphoric acid has the process characteristics that the product cost is relatively low, but the quality is poor. At present, the industrial phosphoric acid is prepared internationally by a wet method, and the wet phosphoric acid is mainly used for producing agricultural fertilizers in China. The wet-process phosphoric acid is prepared by decomposing phosphate rock powder with inorganic acid, separating out crude phosphoric acid, and purifying to obtain a phosphoric acid product, wherein the phosphoric acid product is mainly sulfuric acid process wet-process phosphoric acid, and the ore decomposition reaction formula is as follows:
Ca5F(PO4)3+5H2SO4+nH2O＝3H3PO4+5CaSO4·nH2O+HF↑
where the value of n depends on the crystalline form of calcium sulfate and may be 0,1/2, 2. Under different reaction temperatures and phosphoric acid concentrations, anhydrous calcium sulfate, calcium sulfate hemihydrate and calcium sulfate dihydrate can be generated. At present, more than 80 percent of phosphoric acid in China is produced by a wet phosphoric acid dihydrate method.
In the wet-process phosphoric acid production with high potassium and sodium content phosphate ore as raw material, fluorine in ore pulp is reacted to generate fluosilicic acid, and then the fluosilicic acid and potassium and sodium impurities in the phosphate ore are combined in a reaction tank to form potassium/sodium fluosilicate saturated solution, wherein the chemical formula is R2SiF6(R is K, Na) in the form of white granules or crystalline powder, which decomposes at high temperature (above 300 ℃) into RF and SiF4. When the amount of the catalyst is small, the catalyst is expressed as crystalline powder and is attached to the inner surfaces of a pipeline and a container, and the pipeline is easy to block after a long time, so that the generated load is influenced; the slurry is granular when in large quantity, and is difficult to separate after settling in the reaction tank, so that the effective volume of the reaction tank is directly influenced, the stirring strength is reduced, and great hidden danger is caused. When acidolysis slurry is filtered and separated, water is rapidly vaporized under the action of vacuum, the temperature drops suddenly to 25-30 ℃, a hard and compact potassium/sodium fluosilicate scale layer can be separated out in a filtering pipeline system, a pipeline is blocked, and the production load is influenced, so that the method becomes a main process problem in the wet-process phosphoric acid production of the phosphorite with high potassium and sodium contents.
Disclosure of Invention
In view of the above, the present invention provides a potassium fluosilicate/sodium separation device and its application to solve the above mentioned problems in the background art.
In order to solve the technical problems, the technical scheme of the invention is that the potassium fluosilicate/sodium fluosilicate separation device comprises a separation tube, the separation tube comprises an inlet section and an outlet section, a gate valve is arranged between the inlet section and the outlet section, the gate valve is arranged at an outlet of the outlet section, a screening device is arranged outside an outlet of the outlet section of the separation tube, and a spraying device is arranged between the screening device and an outlet of the separation tube.
Furthermore, the device also comprises an air source supply control system, wherein the gate valve is a pneumatic gate valve and is connected with the air source supply control system.
Preferably, the gate valve installed between the inlet section and the outlet section of the separation pipe is a pneumatic knife gate valve.
Preferably, the gate valve installed at the outlet of the outlet section of the separation pipe is a gas-tight valve.
Preferably, the screening device is a vibrating screen.
Preferably, the inlet section has a diameter of 500mm and a length of 500mm, and the outlet section has a diameter of 150mm and a length of 5000 mm.
Preferably, the inlet section and the outlet section are connected in a conical buffer way, and the height of the conical buffer way is 250 mm.
Meanwhile, the invention also provides an application method of the potassium fluosilicate/sodium separation device, which is characterized in that the potassium fluosilicate/sodium separation device is arranged at the bottom of the flash cooling slurry return pipe.
Preferably, at least two potassium fluosilicate/sodium separation devices are arranged at the bottom of the flash cooling slurry return pipe at intervals.
Further, the absolute pressure of the flash-cooling slurry return pipe is kept to be-40 KPa.
In the wet-process phosphoric acid dihydrate production process, the reaction temperature of phosphorite, sulfuric acid and phosphoric acid in a reaction tank is kept at 75-80 ℃, and the dihydrate calcium sulfate (CaS 0) can be generated through the reaction4·2H2O) crystallization and phosphoric acid. The phosphorus ore pulp is metered and added into a first chamber of a rectangular reaction tank after the ratio of the phosphorus ore pulp to raw material sulfuric acid is adjusted, wherein the rectangular reaction tank consists of six identical chambers, and each chamber is provided with a stirrer with 3 layers of blades. The temperature of the reaction slurry can be increased due to heat generated by sulfuric acid dilution and exothermic reaction, and in order to control the reaction temperature to be 75-80 ℃ and ensure that dihydrate calcium sulfate crystals are obtained, the temperature of the reaction slurry must be controlled to be higher than that of the reaction slurryAnd cooling the reaction slurry.
The flash evaporation principle is widely applied to the generation of phosphoric acid by a dihydrate wet method, the effect is to remove a large amount of heat generated by the reaction, the reaction slurry is pumped into a flash evaporation chamber from a reaction six-chamber by an axial flow pump, under the action of negative pressure, a large amount of heat is taken away by the gas phase after flash evaporation, the reaction slurry returns to a reaction first chamber through a flash cooling slurry return pipe, and the cycle is repeated. The potassium fluosilicate/sodium separation device is designed at the position of the flash cooling slurry return pipe. Through measurement and calculation, the specific gravity of the potassium fluosilicate/sodium scaling substances is usually more than 2.6g/mL, the relative density of reaction slurry is usually not more than 1.6g/mL, by utilizing the specific gravity difference, under the negative pressure action of a slurry return pipe (keeping absolute pressure of 40kPa), the potassium fluosilicate/sodium scaling substances with large specific gravity are preferentially settled and enter a separation pipe connected with a flash cooling slurry return pipe, and the reaction slurry returns to a reaction tank along with the flash cooling slurry return pipe; slurry carried in the potassium fluosilicate/sodium scaling compound is recycled after being washed by a spraying device and filtered and separated by a vibrating screen; finally, the obtained potassium sodium salt, namely the potassium fluosilicate/sodium scaling substance is directly transferred out of the system. In the process, the air source supply control system automatically controls and adjusts the opening and closing of the pneumatic knife gate valve and the air pinch valve according to the amount of the potassium and sodium salt, so that the effects of opening and closing the knife gate valve up and down and opening the knife gate valve up and down can be realized, the return amount of reaction slurry is reasonably controlled, and the normal production is ensured.
Compared with the prior art, the potassium fluosilicate/sodium separation device provided by the invention has a simple structure and is convenient to use, and potassium fluosilicate/sodium scaling substances are effectively separated from reaction slurry by mounting the potassium fluosilicate/sodium separation device at the bottom of the flash cooling slurry return pipe, so that the damage of the potassium sodium salt scaling substances to a reaction tank and a pipeline is avoided, and the production efficiency is improved.
Drawings
FIG. 1 is a schematic structural view of a potassium/sodium fluorosilicate separation apparatus of the present invention;
FIG. 2 is a schematic view of the installation of the potassium fluosilicate/sodium fluosilicate separation device of the present invention.
Illustration of the drawings:
1-a reaction tank, 2-an axial flow pump, 3-a flash cooling evaporation chamber, 4-a flash cooling slurry return pipe and a 5-potassium/sodium fluosilicate separation device;
11-six chambers of a reaction tank, 12-one chamber of the reaction tank;
51-a separation pipe, 52-a pneumatic knife gate valve, 53-an air pinch valve, 54-a spraying device and 55-a vibrating screen;
511-the entrance section, 512-the exit section.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments. It should be noted that the following preferred embodiments should not be construed as limiting the invention, which is to be limited only by the scope of the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Referring to fig. 1, the invention provides a potassium/sodium fluosilicate separation device, which comprises a separation pipe 51, wherein the separation pipe comprises an inlet section 511 and an outlet section 512, a pneumatic knife gate valve 52 is arranged between the inlet section 511 and the outlet section 512, an air pinch valve 53 is arranged at the outlet of the outlet section, a small-sized vibrating screen 55 is arranged outside the outlet of the outlet section 512 of the separation pipe, and a spraying device 54 is arranged between the vibrating screen 55 and the outlet of the separation pipe 51. And an air source supply control system is also included, and the pneumatic knife gate valve 52 and the air clamp valve 53 are respectively connected with the air source supply control system.
Preferably, the inlet section 511 has a diameter of 500mm and a length of 500mm, and the outlet section 512 has a diameter of 150mm and a length of 5000 mm.
Preferably, the inlet section 511 and the outlet section 512 are connected in a conical buffer manner, and the height of the conical buffer is 250 mm.
Referring to fig. 2, the application method of the potassium fluosilicate/sodium separation device provided by the invention is to install the potassium fluosilicate/sodium separation device 5 at the bottom of the flash cooling slurry return pipe 4.
Preferably, at least two potassium fluosilicate/sodium separation devices are arranged at the bottom of the flash cooling slurry return pipe at intervals.
Further, the absolute pressure of the flash-cooling slurry return pipe is kept to be-40 KPa.
Referring to fig. 2, the axial-flow pump 2 pumps the reaction slurry from the six chambers 11 of the reaction tank to the flash evaporation chamber 3, under the action of negative pressure, a large amount of heat is taken away by the flash evaporated gas phase, and the reaction slurry returns to the first chamber 12 of the reaction tank through the flash evaporation slurry return pipe 4, and the process is circulated. The potassium fluosilicate/sodium separation device 5 of the invention is arranged at the bottom of the flash cooling slurry return pipe 4. Through measurement and calculation, the specific gravity of the potassium fluosilicate/sodium scaling substances is usually more than 2.6g/mL, the relative density of reaction slurry is usually not more than 1.6g/mL, by utilizing the specific gravity difference, under the negative pressure action of the flash cooling slurry return pipe (keeping the absolute pressure of 40kPa), the potassium fluosilicate/sodium scaling substances with large specific gravity preferentially settle into a separation pipe 51 connected with the flash cooling slurry return pipe, and the reaction slurry returns to the reaction tank 1 along with the flash cooling slurry return pipe 4; slurry carried in the potassium fluosilicate/sodium scaling compound is washed by a spraying device 54 and filtered and separated by a vibrating screen 55 and then recovered; finally, the obtained potassium sodium salt, namely the potassium fluosilicate/sodium scaling substance is directly transferred out of the system. In the process, the air source supply control system automatically controls and adjusts the opening and closing of the pneumatic knife gate valve 52 and the air pinch valve 53 according to the amount of the potassium and sodium salt, so that the effects of opening and closing the upper part and the lower part and opening the upper part can be realized, the return amount of reaction slurry is reasonably controlled, and the normal production is ensured.
The practical use of the production line of dihydrate wet-process phosphoric acid of the applicant's Van Fudazhou chemical industry, Limited liability company shows that the production line provided with the separation device has the advantages that the cleaning period of equipment for the filtering process and the concentration process and pipelines is prolonged by 1.5 times, the cleaning time is shortened to 30-35% of the original cleaning time, and the production efficiency is greatly improved.
Claims (9)
1. A potassium fluosilicate/sodium separator which is characterized in that: the device comprises a separation pipe, wherein the separation pipe comprises an inlet section and an outlet section, a gate valve is arranged between the inlet section and the outlet section, a gate valve is arranged at an outlet of the outlet section, a screening device is arranged outside an outlet of the outlet section of the separation pipe, and a spraying device is arranged between the screening device and the outlet of the separation pipe; the potassium fluosilicate/sodium separation device is arranged at the bottom of the flash cooling slurry return pipe; the absolute pressure in the flash cooling slurry return pipe is less than 0.
2. The potassium fluosilicate/sodium separation device as claimed in claim 1, wherein: the gate valve is a pneumatic gate valve and is connected with the air source supply control system.
3. The potassium/sodium fluorosilicate separation apparatus as set forth in claim 1 or 2, wherein: the gate valve arranged between the inlet section and the outlet section of the separation pipe is a pneumatic knife gate valve.
4. The potassium/sodium fluorosilicate separation apparatus as set forth in claim 1 or 2, wherein: and the gate valve arranged at the outlet of the outlet section of the separation pipe is an air-clamp valve.
5. The potassium fluosilicate/sodium separation device as claimed in claim 1, wherein: the screening device is a vibrating screen.
6. The potassium fluosilicate/sodium separation device as claimed in claim 1, wherein: the diameter of the inlet section is 500mm, the length is 500mm, the diameter of the outlet section is 150mm, and the length is 5000 mm.
7. The potassium fluosilicate/sodium separation device as claimed in claim 1, wherein: the inlet section is in conical buffer connection with the outlet section, and the height of the conical section is 250 mm.
8. The potassium fluosilicate/sodium separation device as claimed in claim 1, wherein: and two potassium/sodium fluosilicate separation devices are installed at the bottom of the flash cooling slurry return pipe at intervals.
9. The potassium fluosilicate/sodium separation device according to claim 1 or 8, wherein: the absolute pressure of the flash cooling slurry return pipe is kept to be-40 KPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710804597.9A CN107715549B (en) | 2017-09-08 | 2017-09-08 | Potassium fluosilicate/sodium fluosilicate separation device and application thereof |
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| CN201710804597.9A CN107715549B (en) | 2017-09-08 | 2017-09-08 | Potassium fluosilicate/sodium fluosilicate separation device and application thereof |
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| CN107715549B true CN107715549B (en) | 2021-02-23 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5891021A (en) * | 1981-11-27 | 1983-05-30 | Toyo Soda Mfg Co Ltd | Manufacture of wet process phosphoric acid |
| CN102390821A (en) * | 2011-08-08 | 2012-03-28 | 云南云天化国际化工股份有限公司 | Method for producing dihydrate wet-process phosphoric acid |
| CN202212352U (en) * | 2011-08-22 | 2012-05-09 | 山东昌邑石化有限公司 | Balancing agent filter |
| CN102380233B (en) * | 2011-09-21 | 2013-09-25 | 云南大红山管道有限公司 | Dewatering treatment device for low-concentration pulp in pipes and treatment method of dewatering treatment device |
| CN202263430U (en) * | 2011-09-21 | 2012-06-06 | 云南大红山管道有限公司 | Dehydrating treatment device for low-concentration slurry in pipeline |
| CN202643330U (en) * | 2012-06-28 | 2013-01-02 | 贵州开磷（集团）有限责任公司 | Device for preparing high-purity ammonium fluosilicate |
| CN105776221B (en) * | 2016-04-01 | 2017-09-22 | 龚家竹 | A kind of method of fluorine resource reclaim in production of phosphate fertilizer |
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