CN106139635A - The device of a kind of monazite caustic digestion liquid crystallisation by cooling precipitation and technique thereof - Google Patents

The device of a kind of monazite caustic digestion liquid crystallisation by cooling precipitation and technique thereof Download PDF

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Publication number
CN106139635A
CN106139635A CN201510193875.2A CN201510193875A CN106139635A CN 106139635 A CN106139635 A CN 106139635A CN 201510193875 A CN201510193875 A CN 201510193875A CN 106139635 A CN106139635 A CN 106139635A
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Prior art keywords
cooling
monazite
caustic digestion
digestion liquid
temperature
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CN201510193875.2A
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李效平
王凯
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YONGZHOU XIANGJIANG RIVER RARE EARTH Co Ltd
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YONGZHOU XIANGJIANG RIVER RARE EARTH Co Ltd
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Priority to CN201510193875.2A priority Critical patent/CN106139635A/en
Publication of CN106139635A publication Critical patent/CN106139635A/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention relates to device and technique that a kind of monazite caustic digestion liquid crystallisation by cooling separates out, this device includes with lower part: storage tank, feed pump, temperature measurer, moisture separation device, shower nozzle, air distribution plate, motor cover and kuppe, blower fan, stirring, discharging opening and crystalline portion.Use said apparatus to carry out monazite caustic digestion liquid crystallisation by cooling to separate out, crystallization and the separation of tertiary sodium phosphate can be realized;This technique uses the efficient spray type of cooling and stirred crystallization precipitation process to combine, using cooling water the most in a large number, liquid is atomized rear abundant same air contact, has the advantages that cooling effectiveness is high, the evaporation and concentration to about solution 3-5% moisture can be realized, be beneficial to the concentration of next step alkali liquor;Flux of alkaline liquor and air mass flow, good energy-conserving effect can be decomposed according to chilling temperature regulation.

Description

The device of a kind of monazite caustic digestion liquid crystallisation by cooling precipitation and technique thereof
Technical field
The present invention relates to device and technique that monazite caustic digestion liquid crystallisation by cooling separates out, it is achieved the fast quickly cooling of solution But crystallization sodium phosphate skill, belongs to Rare Earth Mine and smelts production field.
Background technology
Monazite is a kind of industry Ree-phospeate Minerals, and industrial general employing Caustic soda decomposition method processes solitary Stone concentrate.(" rare earth ", the first edition first volume, metallurgical industry publishing house 1978, P221-237.)
During soda processes processes monazite, equipment corrosion, labor protection are all easier to environmental conservation solve, special Not being that accompanying element phosphorus reclaims with the form of tertiary sodium phosphate, in rare-earth smelting works, this technique is called without public The alkaline process of evil.
In Caustic soda catabolic process, rare earth generates water-fast hydroxide with thorium, and phosphorus is transformed into water solublity Tertiary sodium phosphate (see (1), (2) reaction equation:
REPO4+ 3NaOH=RE (OH)3↓+Na3PO4 (1)
Th3(PO4)4+ 12NaOH=3Th (OH)4↓+4Na3PO4 (2)
Meanwhile, for ensureing efficient-decomposition, catabolic process alkali liquor is the most excessive, therefore, and alkali liquor and tertiary sodium phosphate Separation just become indispensable link.
Production process mainly realizes crystallization and the separation of tertiary sodium phosphate by decomposing alkali liquor cooling, generally adopts With the indirect crystallisation by cooling of reactor, with cooling still chuck or coil pipe logical fall cold water, under agitation decrease temperature crystalline analysis Go out sodium phosphate, carry out solid-liquid separation and obtain sodium phosphate crystal, and the alkali liquor re-evaporation reclaimed concentrates and is back to point Solve monazite operation to recycle.This crystallization mode is applicable to the product that yield is less, and advantage is operation letter Single, shortcoming is that yield is little, energy consumption is high, floor space is big.
Summary of the invention
The present invention provides the device that a kind of monazite caustic digestion liquid crystallisation by cooling separates out, described device include with Lower part: storage tank, feed pump, temperature measurer, moisture separation device, shower nozzle, air distribution plate, motor cover and Kuppe, blower fan, stirring, discharging opening and crystalline portion.
Described device carries out the technique that monazite caustic digestion liquid crystallisation by cooling separates out, and described processing step is such as Under:
1) alkali liquor after being decomposed by monazite in storage tank with feed pump is sprayed by the shower nozzle on device top Atomization, atomized drop is at below 0.3mm;
2) air is blasted described device by blower fan, realizes band by air distribution plate with drop Rapid contact and becomes popular Amount, by reducing air velocity at moisture separation device, it is achieved gas and drop separation;
3) drop after cooling enters through the guide functions of motor cover and kuppe (7) under gravity The crystalline portion of described device, uniformly separates out tertiary sodium phosphate crystal, the tricresyl phosphate obtained under the effect of stirring Sodium crystal is through discharge hole for discharge;
4) temperature of decomposed solution in crystallization kettle is measured by temperature measurer, by caustic digestion fluid flow and air Flow-control carries out temperature adjustment.
Described caustic digestion liquid feeding temperature is 60 DEG C-90 DEG C.
Described air themperature is 5-25 DEG C.
The temperature entering the caustic digestion liquid in crystalline portion after described cooling is 15-35 DEG C.
Described caustic digestion flow quantity and the ratio of air mass flow are at 1:800-1:3500.
Described blower fan (8) and feed pump use VFC, and temperature control instrument can cold according in crystalline portion But the temperature feedback control blower fan intake of caustic digestion liquid and feed pump flow after..
Electric system and the caustic digestion liquid of stirring are isolated by described motor cover and kuppe, and periphery divides simultaneously It is furnished with water conservancy diversion duct and will decompose alkali liquor importing crystalline portion.
Described temperature control instrument possesses thermometric and controls machine and the function of feed pump flow according to temperature.
Beneficial effects of the present invention is as follows:
This patent and traditional water-cooled crystallization mode compare, and advantage is as follows:
1, use the efficient spray type of cooling and stirred crystallization precipitation process to combine, use cooling water the most in a large number, Liquid is atomized rear abundant same air contact, has the advantages that cooling effectiveness is high;
2, under stirring action, it is ensured that the sodium phosphate crystal formation of precipitation is complete, does not wrap up alkali liquor, impurity content Low, there is the advantage being prone to discharging.
3, the evaporation and concentration to about solution 3-5% moisture can be realized, be beneficial to the concentration of next step alkali liquor;
4, flux of alkaline liquor and air mass flow, good energy-conserving effect can be decomposed according to chilling temperature regulation.
Accompanying drawing explanation
Fig. 1 illustrates the device that a kind of monazite caustic digestion liquid crystallisation by cooling separates out, and it includes 1, storage tank;2、 Feed pump;3, temperature measurer;4, moisture separation device;5, shower nozzle;6, air distribution plate 7;, motor Cover and kuppe;8, blower fan;9, stirring;10, discharging opening;11, crystalline portion.
Detailed description of the invention
Embodiment 1
First 5 DEG C of air are blasted device by blower fan (8), use height on device top by shower nozzle (5) Speed centrifugal spray mode decomposes alkali liquor spraying by 65 DEG C, and atomized drop is at below 0.2mm;Pass through air distribution plate (6) realize with drop Rapid contact and take away heat, realizing gas and drop at moisture separation device (4) Separating, the ratio decomposing alkali liquor fluid flow and air mass flow is 1:4000.
Drop after cooling enters under gravity under the guide functions of motor cover and kuppe (7) In crystalline portion (11), after cooling, temperature is 15 DEG C, uniform precipitation of phosphorus under the stirring action of stirring (9) Acid three sodium crystals, through discharging opening (11) discharging, measure crystallization by temperature control instrument (39) in operating process The temperature of decomposed solution in still, and decomposition alkali fluid flow and air mass flow are adjusted.
Cooling down through this device, tertiary sodium phosphate crystallization 90%, solution concentration promotes 4%.
Embodiment 2
First 28 DEG C of air are blasted device by blower fan (8), use height on device top by shower nozzle (5) Speed centrifugal spray mode decomposes alkali liquor spraying by 90 DEG C, and atomized drop is at below 0.1mm;Pass through air distribution plate (6) realize with drop Rapid contact and take away heat, realizing gas and drop at moisture separation device (4) Separating, the ratio decomposing alkali liquor fluid flow and air mass flow is 1:2500.
Drop after cooling enters under gravity under the guide functions of motor cover and kuppe (7) In crystallization kettle (11), temperature is 34 DEG C, uniformly separates out tertiary sodium phosphate brilliant under the stirring action of stirring (9) Body, through discharging opening (11) discharging, is measured in crystallization kettle by temperature control instrument (3) in operating process and decomposes The temperature of liquid, and decomposition alkali fluid flow and air mass flow are adjusted.
Cooling down through this device, tertiary sodium phosphate crystallization 87%, solution concentration promotes 3%.
Embodiment 3
First 15 DEG C of air are blasted device by blower fan (8), use height on device top by shower nozzle (5) Speed centrifugal spray mode decomposes alkali liquor spraying by 85 DEG C, and atomized drop is at below 0.1mm;Pass through air distribution plate (6) realize with drop Rapid contact and take away heat, at moisture separation device (4) by reducing air speed Degree, it is achieved gas and drop separation, the ratio decomposing alkali liquor fluid flow and air mass flow is 1:1000.
Drop after cooling enters under gravity under the guide functions of motor cover and kuppe (7) In crystallization kettle (11), temperature is 30 DEG C, uniformly separates out tertiary sodium phosphate brilliant under the stirring action of stirring (9) Body, through discharging opening (11) discharging, is measured in crystallization kettle by temperature control instrument (3) in operating process and decomposes The temperature of liquid, and decomposition alkali fluid flow and air mass flow are adjusted.
Cooling down through this device, tertiary sodium phosphate crystallization 85%, solution concentration promotes 3%.

Claims (9)

1. the device that a monazite caustic digestion liquid crystallisation by cooling separates out, it is characterised in that described device includes With lower part: storage tank (1), feed pump (2), temperature measurer (3), moisture separation device (4), Shower nozzle (5), air distribution plate (6), motor cover and kuppe (7), blower fan (8), stirring (9), Discharging opening (10) and crystalline portion (11).
The device that monazite caustic digestion liquid crystallisation by cooling the most according to claim 1 separates out, its feature exists In, described blower fan (8) and feed pump (2) use VFC, and temperature control instrument (3) can be according to crystallization The temperature feedback control blower fan intake of caustic digestion and feed pump flow after cooling in part.
The device that monazite caustic digestion liquid crystallisation by cooling the most according to claim 1 separates out, its feature exists In, described motor cover and kuppe (7) will stir electric system and the isolation of caustic digestion liquid of (9), with Time circumferential distribution have water conservancy diversion duct will decompose alkali liquor import crystalline portion (11).
The device that monazite caustic digestion liquid crystallisation by cooling the most according to claim 1 separates out, its feature exists In, described temperature measurer (3) possesses thermometric and controls blower fan (8) and feed pump (2) according to temperature The function of flow.
5. one kind utilizes the arbitrary described device of claim 1-4 to carry out the precipitation of monazite caustic digestion liquid crystallisation by cooling Technique, it is characterised in that described processing step is as follows:
1) shower nozzle by device top of the alkali liquor after monazite in storage tank (1) being decomposed with feed pump (2) (5) carrying out spray atomization, atomized drop is at below 0.3mm;
2) air is blasted described device by blower fan (8), real with drop Rapid contact by air distribution plate (6) Now take away heat, at moisture separation device (4) place by reducing air velocity, it is achieved gas and drop Separate;
3) drop after cooling enters through the guide functions of motor cover and kuppe (7) under gravity The crystalline portion (11) of described device, uniformly separates out tertiary sodium phosphate crystal under the effect of stirring (9), The tertiary sodium phosphate crystal obtained is through discharging opening (10) discharging;
4) temperature of decomposed solution in crystallization kettle is measured by temperature measurer (3), by caustic digestion fluid flow Temperature adjustment is carried out with air flow control.
The technique that monazite caustic digestion liquid crystallisation by cooling the most according to claim 5 separates out, it is characterised in that Described caustic digestion liquid feeding temperature is 60 DEG C-90 DEG C.
The technique that monazite caustic digestion liquid crystallisation by cooling the most according to claim 5 separates out, it is characterised in that Described air themperature is 5-25 DEG C.
The technique that monazite caustic digestion liquid crystallisation by cooling the most according to claim 5 separates out, it is characterised in that Enter the temperature of caustic digestion liquid in crystalline portion (11) after described cooling and be 15-35 DEG C.
The technique that monazite caustic digestion liquid crystallisation by cooling the most according to claim 5 separates out, it is characterised in that Described caustic digestion flow quantity and the ratio of air mass flow are at 1:800-1:3500.
CN201510193875.2A 2015-04-22 2015-04-22 The device of a kind of monazite caustic digestion liquid crystallisation by cooling precipitation and technique thereof Pending CN106139635A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106586992A (en) * 2016-12-10 2017-04-26 包头稀土研究院 Comprehensive fluorine and phosphorous recovery technology for liquid caustic soda decomposition of mixed rare earth concentrate
CN108057258A (en) * 2018-01-18 2018-05-22 江西金利达钾业有限责任公司 A kind of potassium nitrate spray crystallizer
CN110171808A (en) * 2019-07-09 2019-08-27 乐山师范学院 A kind of preparation facilities and preparation method thereof of pelletiod solid phosphoric acid
CN118558277A (en) * 2024-07-31 2024-08-30 江苏先卓食品科技股份有限公司 Even-heating spray crystallization device and method for isomaltulose alcohol production

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1234744A (en) * 1982-11-17 1988-04-05 William E. Rushton Spray crystallization
CN201613038U (en) * 2009-05-06 2010-10-27 余荣华 Spray crystallizer
CN102974205A (en) * 2012-12-14 2013-03-20 国电龙源电力技术工程有限责任公司 Intra-tower crystallized ammonia-process desulfurization tower
CN203525359U (en) * 2013-10-09 2014-04-09 江苏纵横浓缩干燥设备有限公司 Self-cleaning crystallization tank for evaporating crystallizer

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1234744A (en) * 1982-11-17 1988-04-05 William E. Rushton Spray crystallization
CN201613038U (en) * 2009-05-06 2010-10-27 余荣华 Spray crystallizer
CN102974205A (en) * 2012-12-14 2013-03-20 国电龙源电力技术工程有限责任公司 Intra-tower crystallized ammonia-process desulfurization tower
CN203525359U (en) * 2013-10-09 2014-04-09 江苏纵横浓缩干燥设备有限公司 Self-cleaning crystallization tank for evaporating crystallizer

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106586992A (en) * 2016-12-10 2017-04-26 包头稀土研究院 Comprehensive fluorine and phosphorous recovery technology for liquid caustic soda decomposition of mixed rare earth concentrate
CN106586992B (en) * 2016-12-10 2019-01-15 包头稀土研究院 A kind of technique of the recycling of mixed rare earth concentrates liquid alkaline Decomposition-Synthesis fluorine and phosphorus
CN108057258A (en) * 2018-01-18 2018-05-22 江西金利达钾业有限责任公司 A kind of potassium nitrate spray crystallizer
CN108057258B (en) * 2018-01-18 2023-08-18 江西金利达钾业有限责任公司 Potassium nitrate spray crystallizer
CN110171808A (en) * 2019-07-09 2019-08-27 乐山师范学院 A kind of preparation facilities and preparation method thereof of pelletiod solid phosphoric acid
CN118558277A (en) * 2024-07-31 2024-08-30 江苏先卓食品科技股份有限公司 Even-heating spray crystallization device and method for isomaltulose alcohol production

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Application publication date: 20161123