CN203833622U - Partition-plate crystallization device for electronic-grade phosphoric acid - Google Patents

Partition-plate crystallization device for electronic-grade phosphoric acid Download PDF

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Publication number
CN203833622U
CN203833622U CN201320882566.2U CN201320882566U CN203833622U CN 203833622 U CN203833622 U CN 203833622U CN 201320882566 U CN201320882566 U CN 201320882566U CN 203833622 U CN203833622 U CN 203833622U
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China
Prior art keywords
acid
cold
phosphoric acid
crystallizer
dividing plate
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CN201320882566.2U
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Chinese (zh)
Inventor
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 utility model discloses a partition-plate crystallization device for electronic-grade phosphoric acid. The partition-plate crystallization device comprises a crystallizer, an acid yielding pump, an acid regulating tank, a cold medium tank and a circulating pump, wherein the crystallizer comprises a crystallization box, a partition plate, a crystal washing device and a stiffening ring, an acid outlet of the crystallizer is connected with the acid yielding pump through a valve, and a cold/hot medium inlet and a cold/hot medium outlet of the crystallizer are connected with the cold medium tank; a phosphoric acid product outlet of the acid regulating tank is connected with a product tank, a circulating acid inlet and a circulating acid outlet of the acid regulating tank are connected with circulating acid valves through the circulating pump by acid-resistant pipes, the circulating pump is further connected with the crystallizer, and the acid yielding pump is further connected with a charging opening and a liquid discharging pipe. According to the partition-plate crystallization device for the electronic-grade phosphoric acid, the crystallization efficiency of the phosphoric acid can be improved, the energy consumption is lowered, electronic-grade phosphoric acid products of a variety of purity specifications can be simultaneously obtained, so as to meet different needs of the market, and good economic benefit is created; the partition-plate crystallization device is easy to operate, and the produced products are stable in quality and high in purity, so that the partition-plate crystallization device is applicable to large-scale industrial production; the economic benefit is relatively good.

Description

A kind of electron-level phosphoric acid dividing plate crystallization apparatus
Technical field
The utility model belongs to technical field of inorganic chemical industry, relates to a kind of electron-level phosphoric acid dividing plate 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 two kinds of thermal phosphoric acid and phosphoric acid by wet processes.Thermal phosphoric acid refers to take Rock Phosphate (72Min BPL) as raw material, is first processed into element phosphor, then the phosphoric acid processing with element phosphor; Phosphoric acid by wet process refers to that take Rock Phosphate (72Min BPL) and mineral acid is raw material, the phosphoric acid directly processing.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 that after directly burning with phosphorous furnace gas, water absorbs phosphoric acid processed; Method two is by phosphorous furnace gas and appropriate air mixed, makes phosphorus steam and phosphine gas oxidized, then gas oxidation products Vanadium Pentoxide in FLAKES is made to phosphoric acid with dilute phosphoric acid absorption; Method three is that the phosphorus in phosphorous furnace gas is condensed into liquid phosphorus, with air combustion, generates Vanadium Pentoxide in FLAKES, and then water (or acid) absorbs the liquid phosphorus combustion method that makes phosphoric acid.At present, adopt liquid phosphorus combustion method to produce thermal phosphoric acid more.In thermal phosphoric acid is produced, existing phosphorus supply method is high-order phosphorus supply method.With high-pressure pump or pressurized air, the molten phosphorus in phosphorus-melting groove melting is transported to after header tank, with high pressure spraying, flows into roasting kiln epimere, spraying and burning.The advantage of this method is: molten phosphorus is through sprinkling, sufficient combustion; But its shortcoming is: owing to adopting power machine to carry, and the one, the input of increase equipment funds; The 2nd, strengthened energy consumption; The 3rd, delivery safety performance requriements is high.In thermal phosphoric acid is produced, the quality of the combustion position of yellow phosphorus in roasting kiln, the yield important to the quality of phosphoric acid product and phosphorus.The problems such as yellow phosphorus burning is insufficient may cause that the color of phosphoric acid product is partially yellow, readily oxidizable substance exceeds standard, chimney emits tobacco, acid glue is too much at the bottom of roasting kiln.In currently available technology, adopt liquid phosphorus combustion method to produce thermal phosphoric acid more.With high-pressure pump or pressurized air, the molten phosphorus in phosphorus-melting groove melting is transported to after header tank, with high pressure spraying, flows into roasting kiln burning.Though yellow phosphorus enters roasting kiln in the mode of high pressure spraying in this method, better dispersed, the yellow phosphorus that enters roasting kiln is still droplet-like, and it is difficult to reach with air the state fully contacting, and then has affected to a certain extent the combustion efficacy of yellow phosphorus.Given this, we are from phosphoric acid production reality for many years, and a kind of electron-level phosphoric acid dividing plate crystallization apparatus has been invented in research, through reading up the literature, do not have this electron-level phosphoric acid dividing plate crystallization apparatus of use.Adopt apparatus of the present invention to make yellow phosphorus gasification fully mix afterfire with air, avoided in traditional combustion mode, the disadvantageous effect that yellow phosphorus burning does not thoroughly bring, creates 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 of 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, crystallizer A below is connected with strainer A, strainer A discharge port connects complex acid groove A, complex acid groove A is connected to crystallizer B by pipeline, crystallizer B below is connected with filter 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 has proposed a kind of multi-stage static and has dissolved crystallization process and prepare electron-level phosphoric acid.Raw material phosphor acid solution body disposable is added in prilling tower, the logical cool/heat medium of prilling tower chuck is controlled phosphoric acid liquid temperature: when the cooling of phosphoric acid liquid reaches 15 ~ 280C, constant temperature adds crystal seed to prilling tower: two every grade of operations that dissolve crystallization to level Four static state thereafter comprise: material decrease temperature crystalline → constant temperature → discharge portion adheres to dissolve → constant temperature of mother liquor → intensification separately, then at this temperature, proceed again the operation of next stage, in process, mother liquor divides the inferior quality of N to discharge, discharge step by step mother liquor, progressively improve the purity of phosphoric acid crystal.In last tower, last crystal is product, and heating makes crystal melting, and collects.The crystallizer complex structure of this invention, inconvenient operation, shortcoming high, that efficiency is not high consumes energy.
Summary of the invention
The purpose of this utility model is the deficiency for existing phosphoric acid crystallizer, a kind of crystalline rate that can improve phosphoric acid is provided, reduce energy consumption, can obtain the electron-level phosphoric acid product of multiple pureness specifications to meet the different demands in market simultaneously, create the electron-level phosphoric acid dividing plate crystallization apparatus of good economic benefit.
To achieve these goals, the utility model has adopted following technical scheme:
An electron-level phosphoric acid dividing plate crystallization apparatus, comprises crystallizer, goes out sour pump, acid-regulating tank, cold medium tank and recycle pump, it is characterized in that: described crystallizer includes crystallization case, dividing plate, washes brilliant device and stiffening ring; Described crystallizer is also provided with and adds crystal seed mouth, acid mouth, cold and hot medium inlet and cold and hot 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; The outlet of described recycle acid import and recycle acid is connected with recycle acid valve by recycle pump with acid-proof pipe, described recycle pump also with wash brilliant device and be connected; The described sour pump that goes out is connected with liquid discharge pipe with opening for feed respectively.
Above-described dividing plate is longitudinally evenly distributed on crystallizer inside, and crystallizer interior separation is become to several little lattice, and described little lattice are made as respectively crystal lattice and cold and hot medium lattice.
Above-described dividing plate is provided with more than four.
The setting of reporting to the leadship after accomplishing a task of above-described crystal lattice and cold and hot medium lattice.
Above-described crystal lattice top is provided with acid inlet, and crystal lattice bottom is provided with acid mouth.
Above-described water-in is located at cold and hot medium lattice bottom, and water outlet is located at cold and hot medium lattice top.
Above-described cold and hot medium inlet is connected with into cold medium tube, enters thermal medium pipe and drain tube, and described cold medium inlet is connected to cold medium tank by water pump; Described cold and hot medium inlet connects heat extraction medium tube and cold medium back flow pipe, and described cold medium back flow pipe connects cold medium tank.
Above-describedly wash brilliant device and comprise water inlet pipe and shower, the parallel crystal lattice top that is located at of shower, is evenly provided with spray header on shower; Described wash brilliant device by valve with go out sour pump and be connected.
Principle of work:
The Tc of utilizing impurity in phosphoric acid is the principle higher than pure phosphoric acid melt temperature lower than the Tc of pure phosphoric acid and the melt temperature of impurity, while being crystallisation by cooling, pure phosphoric acid crystallizes out prior to impurity, during melting, impurity is separated out prior to pure phosphoric acid, by adopting dividing plate crystallizer to make phosphoric acid crystallization in separator face, increase unit crystallization area, improved crystalline rate.By arranging, wash brilliant device in crystallizer, to crystal column surface and store up the spray washing of the remaining liquid phase of sour lattice, to avoid the situation of liquid phase that foreign matter content is higher and the miscible quality product decline causing of pure crystal.Effectively utilize phosphorus production waste heat as the thermal source of crystal melting, greatly reduce the production energy consumption of electron-level phosphoric acid.
The beneficial effects of the utility model:
1. the utility model crystallizer adopts dividing plate that whole crystallizer is separated into a plurality of little lattice, and crystal lattice and cold and hot medium lattice are arranged alternately, and make phosphoric acid crystallization in separator face, have increased unit crystallization area, have improved crystalline rate.
2. in crystallizer, arrange and wash brilliant device, to the spray washing of the remaining liquid phase of plane of crystal and crystal lattice bottom and get rid of, avoided the situation of liquid phase that foreign matter content is higher and the miscible quality product decline causing of pure crystal.
Accompanying drawing explanation
Accompanying drawing 1 is structural representation of the present utility model;
Accompanying drawing 2 is structural representations of spray equipment of the present utility model.
In figure, identify: 1. products pot, 2. acid-regulating tank, 3. recycle pump, 4. wash brilliant device, 5. crystallizer, 6. cold medium tank, 7. go out sour pump, 20. phosphoric acid product outlets, 21. opening for feeds, 22. water-ins, 23. venting ports, 24. phosphoric acid outlets, 25. recycle acid imports, 30. 2 acid inlet tubes, 50. former phosphoric acid opening for feeds, 51 stiffening rings, 52. add crystal seed mouth, 53. dividing plates, 54. cold and hot medium lattice, 55. crystal lattices, 56. cold and hot medium lattice, 57. cold and hot medium leakage fluid drams, 58. cold and hot medium fluid inlets, 59. acid mouths, 60. heat extraction medium tube, 61. cold medium back flow pipes, 62. water pumps, 63. enter cold medium tube, 64. drain tube, 65. enter thermal medium pipe, 70. liquid discharge pipes.
Embodiment
With reference to the accompanying drawings, embodiment of the present utility model is further described in detail.
Embodiment 1:
A kind of electron-level phosphoric acid dividing plate crystallization apparatus, comprise crystallizer 5, go out sour pump 7, acid-regulating tank 2, cold medium tank 6 and recycle pump 3, it is characterized in that: described crystallizer 5 includes crystallization case, dividing plate 53, washes brilliant device 4 and stiffening ring 51, and dividing plate 53 and crystallizer 5 are high strength glass material, described dividing plate 53 is provided with four, four dividing plates 53 are longitudinally evenly distributed on crystallizer 5 inside, crystallizer 5 interior separations are become to five little lattice, described little lattice are arranged alternately respectively crystal lattice and cold and hot medium lattice 54, 56, crystallizer 5 is also provided with and adds crystal seed mouth 52, acid mouth 59, cold and hot medium inlet and cold and hot media outlet, acid inlet is located at crystal lattice top, acid mouth 59 is located at crystal lattice bottom, water-in 22 is located at cold and hot medium lattice 54, 56 bottoms, water outlet is located at cold and hot medium lattice 54, 56 tops, the acid mouth 59 of crystallizer 5 by valve with go out sour pump 7 and be connected, described cold and hot medium inlet is connected with into cold medium tube 63, enter thermal medium pipe 65 and drain tube 64, cold medium inlet is connected to cold medium tank 6 by water pump 62, cold and hot medium inlet connects heat extraction medium tube 60 and cold medium back flow pipe 61, cold medium back flow pipe 61 connects cold medium tank 6, wash brilliant device 4 and comprise water inlet pipe and shower, the parallel crystal lattice top that is located at of shower, is evenly provided with spray header on shower, described wash brilliant device 4 by valve with go out sour pump 7 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, the bottom of acid-regulating tank 2 is provided with recycle acid outlet and phosphoric acid product outlet 20, phosphoric acid product outlet 20 connects products pot 1, the outlet of recycle acid import 25 and recycle acid is connected with recycle acid valve by recycle pump 3 with acid-proof pipe, described recycle pump 3 also with wash brilliant device 4 and be connected, the described sour pump 7 that goes out is connected with liquid discharge pipe 70 with opening for feed 21 respectively.
Embodiment 2:
A kind of electron-level phosphoric acid dividing plate crystallization apparatus, comprise crystallizer 5, go out sour pump 7, acid-regulating tank 2, cold medium tank 6 and recycle pump 3, it is characterized in that: described crystallizer 5 includes crystallization case, dividing plate 53, washes brilliant device 4 and stiffening ring 51, and dividing plate 53 and crystallizer 5 are high strength glass material; Described dividing plate 53 is provided with five, five dividing plates 53 are longitudinally evenly distributed on crystallizer 5 inside, crystallizer 5 interior separations are become to six little lattice, described little lattice are arranged alternately respectively crystal lattice and cold and hot medium lattice 54,56, and crystallizer 5 is also provided with and adds crystal seed mouth 52, acid mouth 59, cold and hot medium inlet and cold and hot media outlet; Acid inlet is located at crystal lattice top, acid mouth 59 is located at crystal lattice bottom, water-in 22 is located at cold and hot medium lattice 54,56 bottoms, water outlet is located at cold and hot medium lattice 54,56 tops, the acid mouth 59 of crystallizer 5 by valve with go out sour pump 7 and be connected, described cold and hot medium inlet is connected with into cold medium tube 63, enters thermal medium pipe 65 and drain tube 64, cold medium inlet is connected to cold medium tank 6 by water pump 62, cold and hot medium inlet connects heat extraction medium tube 60 and cold medium back flow pipe 61, and cold medium back flow pipe 61 connects cold medium tank 6; Wash brilliant device 4 and comprise water inlet pipe and shower, the parallel crystal lattice top that is located at of shower, is evenly provided with spray header on shower; Described wash brilliant device 4 by valve with go out sour pump 7 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, the bottom of acid-regulating tank 2 is provided with recycle acid outlet and phosphoric acid product outlet 20, phosphoric acid product outlet 20 connects products pot 1, the outlet of recycle acid import 25 and recycle acid is connected with recycle acid valve by recycle pump 3 with acid-proof pipe, described recycle pump 3 also with wash brilliant device 4 and be connected; The described sour pump 7 that goes out is connected with liquid discharge pipe 70 with opening for feed 21 respectively.
Embodiment 3:
A kind of electron-level phosphoric acid dividing plate crystallization apparatus, comprise crystallizer 5, go out sour pump 7, acid-regulating tank 2, cold medium tank 6 and recycle pump 3, it is characterized in that: described crystallizer 5 includes crystallization case, dividing plate 53, washes brilliant device 4 and stiffening ring 51, and dividing plate 53 and crystallizer 5 are high strength glass material; Described dividing plate 53 is provided with six, six dividing plates 53 are longitudinally evenly distributed on crystallizer 5 inside, crystallizer 5 interior separations are become to seven little lattice, described little lattice are arranged alternately respectively crystal lattice and cold and hot medium lattice 54,56, and crystallizer 5 is also provided with and adds crystal seed mouth 52, acid mouth 59, cold and hot medium inlet and cold and hot media outlet; Acid inlet is located at crystal lattice top, acid mouth 59 is located at crystal lattice bottom, water-in 22 is located at cold and hot medium lattice 54,56 bottoms, water outlet is located at cold and hot medium lattice 54,56 tops, the acid mouth 59 of crystallizer 5 by valve with go out sour pump 7 and be connected, described cold and hot medium inlet is connected with into cold medium tube 63, enters thermal medium pipe 65 and drain tube 64, cold medium inlet is connected to cold medium tank 6 by water pump 62, cold and hot medium inlet connects heat extraction medium tube 60 and cold medium back flow pipe 61, and cold medium back flow pipe 61 connects cold medium tank 6; Wash brilliant device 4 and comprise water inlet pipe and shower, the parallel crystal lattice top that is located at of shower, is evenly provided with spray header on shower; Described wash brilliant device 4 by valve with go out sour pump 7 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, the bottom of acid-regulating tank 2 is provided with recycle acid outlet and phosphoric acid product outlet 20, phosphoric acid product outlet 20 connects products pot 1, the outlet of recycle acid import 25 and recycle acid is connected with recycle acid valve by recycle pump 3 with acid-proof pipe, described recycle pump 3 also with wash brilliant device 4 and be connected; The described sour pump 7 that goes out is connected with liquid discharge pipe 70 with opening for feed 21 respectively.
Above-described embodiment, is more preferably one of concrete mode of the present utility model, and the common variation that those skilled in the art carry out within the scope of technical solutions of the utility model and replacement all should be included in protection domain of the present utility model.

Claims (8)

1. an electron-level phosphoric acid dividing plate crystallization apparatus, comprise crystallizer (5), go out sour pump (7), acid-regulating tank (2), cold medium tank (6) and recycle pump (3), it is characterized in that: described crystallizer (5) includes crystallization case, dividing plate (53), washes brilliant device (4) and stiffening ring (51); Described crystallizer (5) is also provided with and adds crystal seed mouth (52), acid mouth (59), cold and hot medium inlet and cold and hot media outlet; Described acid mouth (59) by valve with go out sour pump (7) 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 outlet (24) is connected with recycle acid valve by recycle pump (3) with acid-proof pipe, described recycle pump (3) also with wash brilliant device (4) and be connected; The described sour pump (7) that goes out is connected with liquid discharge pipe (70) with opening for feed (21) respectively.
2. electron-level phosphoric acid dividing plate crystallization apparatus according to claim 1, it is characterized in that: described dividing plate (53) is longitudinally evenly distributed on crystallizer (5) inside, crystallizer (5) interior separation is become to several little lattice, and described little lattice are made as respectively crystal lattice and cold and hot medium lattice (54,56).
3. electron-level phosphoric acid dividing plate crystallization apparatus according to claim 2, is characterized in that: described dividing plate (53) is provided with more than four.
4. electron-level phosphoric acid dividing plate crystallization apparatus according to claim 2, is characterized in that: the setting of reporting to the leadship after accomplishing a task of described crystal lattice and cold and hot medium lattice (54,56).
5. electron-level phosphoric acid dividing plate crystallization apparatus according to claim 1, is characterized in that: described crystal lattice top is provided with acid inlet, and crystal lattice bottom is provided with acid mouth (59).
6. electron-level phosphoric acid dividing plate crystallization apparatus according to claim 1, is characterized in that: described water-in (22) is located at cold and hot medium lattice (54,56) bottom, and water outlet is located at cold and hot medium lattice (54,56) top.
7. electron-level phosphoric acid dividing plate crystallization apparatus according to claim 1, it is characterized in that: described cold and hot medium inlet is connected with into cold medium tube (63), enters thermal medium pipe (65) and drain tube (64), and described cold medium inlet is connected to cold medium tank (6) by water pump (62); Described cold and hot medium inlet connects heat extraction medium tube (60) and cold medium back flow pipe (61), and described cold medium back flow pipe (61) connects cold medium tank (6).
8. electron-level phosphoric acid dividing plate crystallization apparatus according to claim 1, is characterized in that: the described brilliant device (4) of washing comprises water inlet pipe and shower, and the parallel crystal lattice top that is located at of shower, is evenly provided with spray header (42) on shower (41); Described wash brilliant device (4) by valve with go out sour pump (7) and be connected.
CN201320882566.2U 2013-12-30 2013-12-30 Partition-plate crystallization device for electronic-grade phosphoric acid Expired - Fee Related CN203833622U (en)

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CN201320882566.2U CN203833622U (en) 2013-12-30 2013-12-30 Partition-plate crystallization device for electronic-grade phosphoric acid

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Application Number Priority Date Filing Date Title
CN201320882566.2U CN203833622U (en) 2013-12-30 2013-12-30 Partition-plate crystallization device for electronic-grade phosphoric acid

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103771374A (en) * 2013-12-30 2014-05-07 广西明利化工有限公司 Electronic grade phosphoric acid clapboard crystallizing device

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103771374A (en) * 2013-12-30 2014-05-07 广西明利化工有限公司 Electronic grade phosphoric acid clapboard crystallizing device
CN103771374B (en) * 2013-12-30 2016-04-20 广西明利化工有限公司 A kind of electron-level phosphoric acid baffle crystallization device

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