CN103771373B - A kind of electron-level phosphoric acid Hot-blast Heating crystallization apparatus - Google Patents

A kind of electron-level phosphoric acid Hot-blast Heating crystallization apparatus Download PDF

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CN103771373B
CN103771373B CN201310744658.9A CN201310744658A CN103771373B CN 103771373 B CN103771373 B CN 103771373B CN 201310744658 A CN201310744658 A CN 201310744658A CN 103771373 B CN103771373 B CN 103771373B
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acid
phosphoric acid
crystallizer
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CN103771373A (en
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林军
吴小海
苏杰文
王文营
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GUANGXI MINGLI CHEMICALS CO Ltd
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GUANGXI MINGLI CHEMICALS CO Ltd
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Abstract

The invention discloses a kind of electron-level phosphoric acid Hot-blast Heating crystallization apparatus, comprise crystallizer, go out sour pump, acid-regulating tank and recycle pump, it is characterized in that: also include storage heater; Described crystallizer includes crystallization case, U-shaped crystallizer, washes brilliant device, pipe connecting and stiffening ring.The present invention is directed to the deficiency of existing phosphoric acid crystallizer, a kind of crystalline rate that can improve phosphoric acid is provided, reduce energy consumption, the electron-level phosphoric acid product of multiple pureness specifications can be obtained to meet the different demands in market simultaneously, create the electron-level phosphoric acid Hot-blast Heating crystallization apparatus of good economic benefit, this device processing ease, and the constant product quality of producing, purity are high, be suitable for large-scale industrial production, and better economic benefit.

Description

A kind of electron-level phosphoric acid Hot-blast Heating crystallization apparatus
Technical field
The invention belongs to technical field of inorganic chemical industry, relate to a kind of electron-level phosphoric acid Hot-blast Heating crystallization apparatus.
Background technology
Phosphoric acid is the important component part of chemical industry, is important basic chemical industry raw material.The production method of phosphoric acid is divided into thermal phosphoric acid and phosphoric acid by wet process two kinds.It is raw material that thermal phosphoric acid refers to Rock Phosphate (72Min BPL), is first processed into element phosphor, then with the phosphoric acid that element phosphor processes; Phosphoric acid by wet process refers to Rock Phosphate (72Min BPL) and mineral acid for raw material, the phosphoric acid directly processed.The thick product of phosphoric acid by wet process is impure more, mainly for the production of fertilizer; Thermal phosphoric acid but has the advantages such as product concentration is high, impurity is few, can be used for manufacturing food and PHOSPHORIC ACID TECH.GRADE product salt.The production method of thermal phosphoric acid has three kinds: method one is the perfect combustion method absorbing phosphoric acid processed after directly burning with phosphorous furnace gas with water; Method two is by phosphorous furnace gas and appropriate air mixed, make phosphorus steam and phosphine gas oxidized, then gas oxidation products Vanadium Pentoxide in FLAKES dilute phosphoric acid is absorbed and obtained phosphoric acid; Method three is that the phosphorus in phosphorous furnace gas is condensed into liquid phosphorus, generates Vanadium Pentoxide in FLAKES with air combustion, then uses water (or acid) to absorb the liquid phosphorus combustion method of obtained phosphoric acid.At present, the liquid phosphorus combustion method that adopts produces thermal phosphoric acid more.In phosphorous acid production by BEP, existing phosphorus supply method is high-order phosphorus supply method.Namely, after the molten phosphorus in phosphorus-melting groove melting being transported to header tank with high-pressure pump or pressurized air, roasting kiln epimere is flowed into high pressure spraying, spraying and burning.The advantage of this method is: melt phosphorus through spraying, sufficient combustion; But its shortcoming is: owing to adopting power machine conveying, one is the input increasing equipment funds; Two is increase energy consumption; Three is that delivery safety performance requriements is high.In phosphorous acid production by BEP, the quality of the combustion position of yellow phosphorus in roasting kiln, to the quality of phosphoric acid product and the yield important of phosphorus.Yellow phosphorus burning is insufficient, the problem such as may cause that the color of phosphoric acid product is partially yellow, readily oxidizable substance exceeds standard, chimney emits tobacco, acid glue at the bottom of roasting kiln is too much.In currently available technology, the liquid phosphorus combustion method that adopts produces thermal phosphoric acid more.Namely, after the molten phosphorus in phosphorus-melting groove melting being transported to header tank with high-pressure pump or pressurized air, roasting kiln burning is flowed into high pressure spraying.Though yellow phosphorus enters roasting kiln in the mode of high pressure spraying in this method, better dispersed, enter the yellow phosphorus of roasting kiln still in droplet-like, itself and air are difficult to reach the state fully contacted, and then have impact on the combustion efficacy of yellow phosphorus to a certain extent.Given this, we are from phosphoric acid production reality for many years, and a kind of electron-level phosphoric acid baffle crystallization device has been invented in research, through reading up the literature, not having and using this electron-level phosphoric acid baffle crystallization device.Adopt apparatus of the present invention that yellow phosphorus is gasified and fully mix afterfire with air, avoid in traditional combustion mode, the disadvantageous effect that yellow phosphorus burning does not thoroughly bring, create good economic benefit and social benefit.
Chinese patent: number of patent application 201120108876.X, notification number CN202390205 U, day for announcing 2012.08. 22, this utility model discloses a kind of device producing electron-level phosphoric acid, comprise phosphoric acid subsider, crystallizer A, crystallizer B and product groove, it is characterized in that: phosphoric acid subsider is connected to crystallizer A by pipeline A, strainer A is connected with below crystallizer A, strainer A discharge port connects complex acid groove A, complex acid groove A is connected to crystallizer B by pipeline, filter B is connected with below crystallizer B, filter B discharge port connects complex acid groove B, complex acid groove B is connected to product groove by pipeline B, crystallizer A, crystallizer B5 with chuck respectively with refrigerating unit, heating unit is connected.Also there is complex structure, inconvenient operation in this utility model, the shortcoming that efficiency is not high.
Chinese patent: number of patent application 201110096758.6, notification number CN102198937 A, day for announcing 2011.09. 28, this invention proposes a kind of multi-stage static and dissolves crystallization process and prepare electron-level phosphoric acid.Raw material phosphor acid solution body disposable is added in prilling tower, prilling tower chuck leads to cooling/heating medium and controls phosphoric acid liquid temperature: when phosphoric acid liquid cooling reaches 15 ~ 280C, constant temperature adds crystal seed to prilling tower: every grade of operation that two to level Four static state thereafter dissolves crystallization comprises: material decrease temperature crystalline → constant temperature → discharge portion adheres to mother liquor → intensification separately and dissolves → constant temperature, then the operation of next stage is proceeded at this temperature again, in process, mother liquor divides N substandard quality to discharge, discharge mother liquor step by step, progressively improve the purity of phosphoric acid crystal.In last tower, remaining crystal is product, and heating makes crystal melting, and collects.The crystallizer complex structure of this invention, inconvenient operation, consume energy high, that efficiency is not high shortcoming.
Summary of the invention
The object of the invention is to the deficiency for existing phosphoric acid crystallizer, a kind of crystalline rate that can improve phosphoric acid is provided, reduce energy consumption, the electron-level phosphoric acid product that simultaneously can obtain multiple pureness specifications, to meet the different demands in market, creates the electron-level phosphoric acid Hot-blast Heating crystallization apparatus of good economic benefit.
To achieve these goals, present invention employs following technical scheme:
A kind of electron-level phosphoric acid Hot-blast Heating crystallization apparatus, comprises crystallizer, goes out sour pump, acid-regulating tank and recycle pump, wherein: also include Hot-blast Heating fusing system; Described crystallizer includes crystallization case, U-shaped crystallizer, washes brilliant device, pipe connecting and stiffening ring; Described crystallizer is provided with hot-blast outlet, crystal seed input port, hot-wind inlet, acid mouth, cold medium inlet and cold media outlet; The acid mouth of described crystallizer by valve with go out sour pump and be connected; The top of described acid-regulating tank and top are provided with opening for feed, water-in, venting port and recycle acid import, and the bottom of acid-regulating tank is provided with recycle acid outlet and phosphoric acid product outlet; Described phosphoric acid product outlet connects products pot; Described recycle acid import is connected by recycle pump and recycle acid valve with recycle acid outlet acid-proof pipe, described recycle pump also with wash brilliant device and be connected; The described sour pump that goes out is connected with opening for feed and liquid discharge pipe respectively.
Above-described Hot-blast Heating fusing system includes air filter, hotblast stove, heating duct and gas blower.
Above-described U-shaped crystallizer uses pipe connecting connect rear parallel connection or be composed in series by several U-tube, is suspended in crystallizer.
Above-describedly wash brilliant device and comprise water inlet pipe and shower, shower is parallel is located at U-tube top, and shower is evenly provided with spray header; Described wash brilliant device by valve with go out sour pump and be connected.
The outlet of above-described heating duct extends to the bottom of crystallizer.
Above-described shower is stainless steel tube.
Above-described U-tube is high strength glass material.
Above-described crystallization case is high strength glass material.
Principle of work:
Utilize the Tc of impurity in phosphoric acid lower than the Tc of pure phosphoric acid and the melt temperature of the impurity principle higher than pure phosphoric acid melt temperature, namely during crystallisation by cooling, pure phosphoric acid crystallizes out prior to impurity, during melting, impurity is separated out prior to pure phosphoric acid, simultaneously by adopting U-tube to add cold medium as crystalline carrier, make xln be suspended in U-tube, the high liquid phase of foreign matter content can be made thoroughly to discharge when crystalline substance, liquid two-phase laminated flow.Brilliant device is washed by arranging in crystallizer, to crystal column surface and the spray washing of the remaining liquid phase of crystallizer, the situation that the liquid phase avoiding foreign matter content higher and the miscible quality product caused of clean crystals decline.And molten brilliant time adopt Hot-blast Heating fusion technology to guarantee heating and melting time crystallizer in temperature can overallly balancedly to rise, ensure that the effect that sweating is purified largely, thus the purification efficiency of raising phosphoric acid crystallization.
Beneficial effect of the present invention:
1. the present invention adds cold medium as making crystalline carrier by adopting U-tube, xln is made to be suspended in U-tube, the high liquid phase of foreign matter content can be made thoroughly to discharge when crystalline substance, liquid two-phase laminated flow, solve the crystalline substance of the existence of straight tube crystallization in the past, liquid separation does not thoroughly cause product quality not high, the problem that purification efficiency is lower.
2. the present invention arranges and washes brilliant device in crystallizer, to crystal column surface and the spray washing of the remaining liquid phase of crystallizer, avoids the situation that the higher liquid phase of foreign matter content and the miscible quality product caused of clean crystals decline.
3. adopt the crystallization of Hot-blast Heating fusion technology heating and melting, guarantee that the temperature in crystallizer can rise in overall equilibrium, ensure that the effect that sweating is purified largely, thus improve the purification efficiency of phosphoric acid crystallization.
Accompanying drawing explanation
Accompanying drawing 1 is assembly structure schematic diagram of the present invention;
Accompanying drawing 2 of the present inventionly washes brilliant device schematic diagram.
Identify in figure: 1. products pot, 2. acid-regulating tank, 3. recycle pump, 4. wash brilliant device, 5. crystallizer, 6. air filter, 7. gas blower, 8. hotblast stove, 9. go out sour pump, 20. phosphoric acid product outlets, 21. opening for feeds, 22. water-ins, 23. venting ports, 24. recycle acid outlets, 25. recycle acid imports, 41. showers, 42. spray headers, 50. raw material acid entrances, 51. hot-blast outlets, 52. cold medium inlets, 53. crystal seed input ports, 54.U type pipe, 55. pipe connectings, 56. stiffening rings, 57. cold media outlets, 58. hot-wind inlets, 59. acid mouths, 90. liquid discharge pipes.
Embodiment
With reference to the accompanying drawings, the specific embodiment of the present invention is further described in detail.
Embodiment 1:
A kind of electron-level phosphoric acid Hot-blast Heating crystallization apparatus, comprises crystallizer 5, goes out sour pump 9, acid-regulating tank 2, recycle pump 3 and Hot-blast Heating fusing system; Hot-blast Heating fusing system includes air filter 6, hotblast stove 8, heating duct and gas blower 7, and the outlet of heating duct extends to the bottom of crystallizer 5; Described crystallizer 5 includes crystallization case, U-shaped crystallizer, washes brilliant device 4, pipe connecting 55 and stiffening ring 56, wash brilliant device 4 and comprise water inlet pipe and shower 41, shower 41 is parallel is located at U-tube 54 top, shower 41 is stainless steel tube, shower 41 is evenly provided with spray header 42, described wash brilliant device 4 by valve with go out sour pump 9 and be connected; U-shaped crystallizer composes in parallel after using pipe connecting 55 to connect by several U-tube 54, and U-tube 54 is high strength glass material, is suspended in crystallizer 5; Described crystallizer 5 is provided with hot-blast outlet 51, crystal seed input port 53, hot-wind inlet 58, acid mouth 59, cold medium inlet 52 and cold media outlet 57; The acid mouth 59 of described crystallizer 5 by valve with go out sour pump 9 and be connected; The top of described acid-regulating tank 2 and top are provided with opening for feed 21, water-in 22, venting port 23 and recycle acid import 25, and the bottom of acid-regulating tank 2 is provided with recycle acid outlet 24 and phosphoric acid product outlet 20; Described phosphoric acid product outlet 20 connects products pot 1; Described recycle acid import 25 and recycle acid are exported 24 and are connected by recycle pump 3 and recycle acid valve with acid-proof pipe, described recycle pump 3 also with wash brilliant device 4 and be connected; The described sour pump 9 that goes out is connected with opening for feed 21 and liquid discharge pipe 90 respectively.
Embodiment 2:
A kind of electron-level phosphoric acid Hot-blast Heating crystallization apparatus, comprises crystallizer 5, goes out sour pump 9, acid-regulating tank 2, recycle pump 3 and Hot-blast Heating fusing system; Hot-blast Heating fusing system includes air filter 6, hotblast stove 8, heating duct and gas blower 7, and the outlet of heating duct extends to the bottom of crystallizer 5; Described crystallizer 5 includes crystallization case, U-shaped crystallizer, washes brilliant device 4, pipe connecting 55 and stiffening ring 56, wash brilliant device 4 and comprise water inlet pipe and shower 41, shower 41 is parallel is located at U-tube 54 top, shower 41 is stainless steel tube, shower 41 is evenly provided with spray header 42, described wash brilliant device 4 by valve with go out sour pump 9 and be connected; U-shaped crystallizer is composed in series after using pipe connecting 55 to connect by several U-tube 54, and U-tube 54 is high strength glass material, is suspended in crystallizer 5; Described crystallizer 5 is provided with hot-blast outlet 51, crystal seed input port 53, hot-wind inlet 58, acid mouth 59, cold medium inlet 52 and cold media outlet 57; The acid mouth 59 of described crystallizer 5 by valve with go out sour pump 9 and be connected; The top of described acid-regulating tank 2 and top are provided with opening for feed 21, water-in 22, venting port 23 and recycle acid import 25, and the bottom of acid-regulating tank 2 is provided with recycle acid outlet 24 and phosphoric acid product outlet 20; Described phosphoric acid product outlet 20 connects products pot 1; Described recycle acid import 25 and recycle acid are exported 24 and are connected by recycle pump 3 and recycle acid valve with acid-proof pipe, described recycle pump 3 also with wash brilliant device 4 and be connected; The described sour pump 9 that goes out is connected with opening for feed 21 and liquid discharge pipe 90 respectively.
Embodiment 3:
A kind of electron-level phosphoric acid Hot-blast Heating crystallization apparatus, comprises crystallizer 5, goes out sour pump 9, acid-regulating tank 2, recycle pump 3 and Hot-blast Heating fusing system; Hot-blast Heating fusing system includes air filter 6, hotblast stove 8, heating duct and gas blower 7, and the outlet of heating duct extends to the bottom of crystallizer 5; Described crystallizer 5 includes crystallization case, U-shaped crystallizer, washes brilliant device 4, pipe connecting 55 and stiffening ring 56, wash brilliant device 4 and comprise water inlet pipe and shower 41, shower 41 is parallel is located at U-tube 54 top, shower 41 is stainless steel tube, shower 41 is evenly provided with spray header 42, described wash brilliant device 4 by valve with go out sour pump 9 and be connected; U-shaped crystallizer uses pipe connecting 55 connect rear parallel connection and be composed in series by several U-tube 54, and U-tube 54 is high strength glass material, is suspended in crystallizer 5; Described crystallizer 5 is provided with hot-blast outlet 51, crystal seed input port 53, hot-wind inlet 58, acid mouth 59, cold medium inlet 52 and cold media outlet 57; The acid mouth 59 of described crystallizer 5 by valve with go out sour pump 9 and be connected; The top of described acid-regulating tank 2 and top are provided with opening for feed 21, water-in 22, venting port 23 and recycle acid import 25, and the bottom of acid-regulating tank 2 is provided with recycle acid outlet 24 and phosphoric acid product outlet 20; Described phosphoric acid product outlet 20 connects products pot 1; Described recycle acid import 25 and recycle acid are exported 24 and are connected by recycle pump 3 and recycle acid valve with acid-proof pipe, described recycle pump 3 also with wash brilliant device 4 and be connected; The described sour pump 9 that goes out is connected with opening for feed 21 and liquid discharge pipe 90 respectively.
Above-described embodiment, just one of more preferably concrete mode of the present invention, the usual change that those skilled in the art carry out within the scope of technical solution of the present invention and replacement all should be included in protection scope of the present invention.

Claims (5)

1. an electron-level phosphoric acid Hot-blast Heating crystallization apparatus, comprises crystallizer (5), goes out sour pump (9), acid-regulating tank (2) and recycle pump (3), it is characterized in that: also include Hot-blast Heating fusing system; Described crystallizer (5) includes crystallization case, U-shaped crystallizer, washes brilliant device (4), pipe connecting (55) and stiffening ring (56); Described crystallizer (5) is provided with hot-blast outlet (51), crystal seed input port (53), hot-wind inlet (58), acid mouth (59), cold medium inlet (52) and cold media outlet (57); The acid mouth (59) of described crystallizer (5) by valve with go out sour pump (9) and be connected; The top of described acid-regulating tank (2) and top are provided with opening for feed (21), water-in (22), venting port (23) and recycle acid import (25), and the bottom of acid-regulating tank (2) is provided with recycle acid outlet (24) and phosphoric acid product outlet (20); Described phosphoric acid product outlet (20) connects products pot (1); Described recycle acid import (25) is exported (24) and is connected by recycle pump (3) and recycle acid valve with acid-proof pipe with recycle acid, described recycle pump (3) also with wash brilliant device (4) and be connected; The described sour pump (9) that goes out is connected with opening for feed (21) and liquid discharge pipe (90) respectively;
Described Hot-blast Heating fusing system includes air filter (6), hotblast stove (8), heating duct and gas blower (7);
Described U-shaped crystallizer uses pipe connecting (55) connect rear parallel connection and/or be composed in series by several U-tube (54), is suspended in crystallizer (5);
Described brilliant device (4) of washing comprises water inlet pipe and shower (41), and shower (41) is parallel is located at U-tube (54) top, shower (41) is evenly provided with spray header (42); Described wash brilliant device (4) by valve with go out sour pump (9) and be connected.
2. electron-level phosphoric acid Hot-blast Heating crystallization apparatus according to claim 1, is characterized in that: the outlet of described heating duct extends to the bottom of crystallizer (5).
3. electron-level phosphoric acid Hot-blast Heating crystallization apparatus according to claim 1, is characterized in that: described shower (41) is stainless steel tube.
4. electron-level phosphoric acid Hot-blast Heating crystallization apparatus according to claim 1, is characterized in that: described U-tube (54) is high strength glass material.
5. electron-level phosphoric acid Hot-blast Heating crystallization apparatus according to claim 1, is characterized in that: described crystallization case is high strength glass material.
CN201310744658.9A 2013-12-30 2013-12-30 A kind of electron-level phosphoric acid Hot-blast Heating crystallization apparatus Active CN103771373B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102580345A (en) * 2012-01-13 2012-07-18 四川大学 Crystallization tower for purifying phosphoric acid
CN102795609A (en) * 2011-05-23 2012-11-28 杨志勇 Apparatus for producing high purity electronic grade phosphoric acid
CN203781850U (en) * 2013-12-30 2014-08-20 广西明利化工有限公司 Electronic grade phosphoric acid hot blast heating crystallization device

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102795609A (en) * 2011-05-23 2012-11-28 杨志勇 Apparatus for producing high purity electronic grade phosphoric acid
CN102580345A (en) * 2012-01-13 2012-07-18 四川大学 Crystallization tower for purifying phosphoric acid
CN203781850U (en) * 2013-12-30 2014-08-20 广西明利化工有限公司 Electronic grade phosphoric acid hot blast heating crystallization device

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