CN108557894A - A kind of manganese sulfate solution crystallization apparatus and method - Google Patents

A kind of manganese sulfate solution crystallization apparatus and method Download PDF

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Publication number
CN108557894A
CN108557894A CN201810089909.7A CN201810089909A CN108557894A CN 108557894 A CN108557894 A CN 108557894A CN 201810089909 A CN201810089909 A CN 201810089909A CN 108557894 A CN108557894 A CN 108557894A
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China
Prior art keywords
manganese sulfate
pump
drying machine
solution
filtrate
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Pending
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CN201810089909.7A
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Chinese (zh)
Inventor
曾锡华
杜修权
彭小红
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Jiangsu Mike Chemical Machinery Co Ltd
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Jiangsu Mike Chemical Machinery Co Ltd
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Priority to CN201810089909.7A priority Critical patent/CN108557894A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00Compounds of manganese
    • C01G45/10Sulfates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0018Evaporation of components of the mixture to be separated
    • B01D9/0031Evaporation of components of the mixture to be separated by heating
    • 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

Abstract

The invention discloses a kind of manganese sulfate solution crystallization apparatus and methods, belong to solution crystallization art, the temperature raising pressure-raising in manganese sulfate crystallization process, reduce the solubility of manganese sulfate, a large amount of manganese sulfate crystal can be precipitated, and need not repeat to crystallize, and reduce crystallization energy consumption.According to the characteristic of manganese sulfate solution, the solubility of manganese sulfate solution is reduced with the raising of temperature, it is 0.25MPa in pressure, temperature is under 138 DEG C of working conditions, the solubility of manganese sulfate in water is 4.2%, a large amount of manganese sulfate can in crystalline form be separated out from solution, using crystallizing evaporator and filtering drying machine with the use of the crystallization for completing manganese sulfate solution, manganese sulfate concentration in the filtrate in filtering drying machine lower part filtrate area is only 4.2%, subsequent processing is sent to by filtrate pump discharge pipe under the promotion of filtrate pump, crystallizing evaporator need not be sent back to again to continue to evaporate moisture content, so manganese sulfate solution high temperature crystallization method is a kind of very energy-efficient crystallization processes technology.

Description

A kind of manganese sulfate solution crystallization apparatus and method
Technical field
The invention belongs to solution crystallization art more particularly to a kind of manganese sulfate solution crystallization apparatus and methods.
Background technology
The crystallization of manganese sulfate solution is crystallized under the working condition of normal pressure in hydrometallurgy industry, but normal pressure The solubility of lower manganese sulfate in water is larger, and about 22.3%, so the crystallization of manganese sulfate solution under normal pressure need to evaporate solution Supersaturated solution is concentrated to crystallize by manganese sulfate, then by containing the magma that manganese sulfate crystallizes be sent from scheming carry out separation must sulphur Sour manganese crystalline product, but the filtrate of centrifuge is a kind of saturated solution, wherein a concentration of the 22.3% of manganese sulfate, it is seen that manganese sulfate Content is very high, and manganese sulfate therein, which is separated, must send back to filtrate progress repeated evaporation condensing crystallizing in crystallizer, But it needs to consume a large amount of heating steam during repeated evaporation condensing crystallizing, so the crystal energy of manganese sulfate solution under normal pressure Consumption is very high.
Invention content
The present invention provides a kind of manganese sulfate solution crystallization apparatus and method, the temperature raising pressure-raising in manganese sulfate crystallization process, The solubility of manganese sulfate is reduced, a large amount of manganese sulfate crystal can be precipitated, and need not repeat to crystallize, and reduce crystallization energy consumption.
To realize that the object above present invention adopts the following technical scheme that:
A kind of manganese sulfate solution crystallization apparatus, including 7 top of crystallizing evaporator connect temperature control valve (TCV) 8, temperature control valve (TCV) connection Indirect steam outlet 9,7 side lower end of crystallizing evaporator are connect by forced circulation pump inlet tube 2 with forced circulation pump 3, by force Pump inlet pipe 2 processed connects solution inlet port pipe close to one end of forced circulation pump 3, and 7 side upper end of crystallizing evaporator is by adding Hot device outlet 6 is connect with heater 5, and 5 other end of heater is connect by forced circulation pump discharge pipe 4 with forced circulation pump 3, 5 side of heater connection heating steam inlet tube mouth 10,5 lower end side of heater is connected cold by heater condensed water outlet spout 11 Condensate tank 12,12 bottom end of condensate water pot connect condensed water outlet spout 13, and the bottom end of crystallizing evaporator 7 passes through magma pump inlet pipe 14 It is connect with magma pump 15, magma pump 15 is connect by magma pump discharge pipe 16 with 17 top side of filtering drying machine, filtration drying The 17 top other side of machine is equipped with compressed air inlet pipe 22, and 17 side of filtering drying machine is equipped with dumping pit 21, filtering drying machine 17 Interior to be equipped with filter element 18, connection filtering layer crystallizes dumping glassware 19 and extends to self-filtering portion among 17 top of filtering drying machine 18 top of part, filtering layer, which crystallizes, connects motor 20 on dumping glassware 19,17 bottom end of filtering drying machine passes through filtrate pump inlet tube 23 Filtrate pump 24 is connected, filtrate pump 24 is equipped with filtrate pump outlet spout 25.
A kind of manganese sulfate solution method for crystallising, including:Manganese sulfate solution is sent to forced circulation pump inlet tube by inlet tube 1 In 2, solution is sent to by forced circulation pump discharge pipe 4 together under the promotion of forced circulation pump 3 and in crystallizing evaporator 7 In 5 tube side of heater, heating steam is sent to by heating steam inlet pipe 10 in 5 shell side of heater, in 5 tube side of heater Solution carries out strong heat exchange during flowing up with the heating steam in shell side, and solution is heated and gradually carried Temperature, while the pressure in crystallizing evaporator 7 steps up, the solubility of solution manganese sulfate during pressure-raising temperature raising can be dropped by Zhejiang It is crystallized down to being precipitated to hypersaturated state, when solution pressure reaches 0.25MPa, and temperature is 138 DEG C, manganese sulfate is molten in solution Xie Du is 4.2%, and a large amount of manganese sulfate can in crystalline form be separated out from solution, due to gravity effect it can sink collection to steam 7 lower part of crystallizer is sent out, the clear liquid on 7 top of crystallizing evaporator continues to tie in heater 5 and evaporation together with the solution come is supplemented in It is recycled in brilliant device 7, feed liquid constantly has manganese sulfate to crystallize out to sink to 7 lower part of crystallizing evaporator during cycle, evaporation production The conditioned valve 8 of raw indirect steam and indirect steam outlet 9 are discharged, and discharge rate will be with the temperature in crystallizing evaporator 7 Interlocking ensures that the temperature in crystallizing evaporator 7 is 138 DEG C, and the condensed water that heater 5 generates passes through heater condensation-water drain Pipe 11 is sent to condensate water pot 12, then is sent out by condensating water outlet tube 13, and the manganese sulfate crystallization of 7 lower part of crystallizing evaporator increases to When a certain amount of, manganese sulfate magma is sent in magma pump 15 by magma pump inlet pipe 14, under the promotion of magma pump 15 It is sent in filtering drying machine 17 by magma pump discharge pipe 16, filtering drying machine 17 is divided into two regions, mistake by filter element 18 Filter 18 upper area of component is magma filter cake area, and it is 0.25MPa to control its pressure, and 18 lower area of filter element is filtrate area, It is an atmospheric area, stops charging when the magma that 18 top magma filter cake area of filter element is sent into is to certain volume, with Compressed air is sent to by compressed air inlet pipe 22 in the top magma filter cake area of filtering drying machine 17 afterwards, manganese sulfate magma Under the double action of gravity and pressure difference, the saturated solution in manganese sulfate magma enters filtering drying machine 17 through filter element 18 The filtrate area of lower part, manganese sulfate crystallizes the magma filter cake area that can be trapped within 18 top of filter element, in order to ensure manganese sulfate knot The permeability of brilliant filter cake, filtering layer crystallization dumping glassware 19 constantly run under the driving of motor 20 and stir manganese sulfate knot up and down Brilliant filter cake, the attachment saturated solution basic filtering in making manganese sulfate crystallize finally may be used to the filtrate area of 17 lower part of filtering drying machine Dry manganese sulfate crystallization is taken out from dumping pit 21, the manganese sulfate concentration in the filtrate in 17 lower part filtrate area of filtering drying machine is only 4.2%, filtrate pump 24 is sent to by filtrate pump inlet tube 23, is sent to by filtrate pump discharge pipe 25 under the promotion of filtrate pump 24 Subsequent processing.
Beneficial effects of the present invention:The present invention provides a kind of manganese sulfate solution crystallization apparatus and methods, in crystallization process Solution in middle heater tube side carries out strong heat exchange during flowing up with the heating steam in shell side, and solution obtains To heating and gradually temperature raising, while the pressure in crystallizing evaporator steps up, solution manganese sulfate during pressure-raising temperature raising Solubility, which can continuously decrease, reaches hypersaturated state precipitation crystallization, molten when solution pressure reaches 0.25MPa, and temperature is 138 DEG C The solubility of manganese sulfate is 4.2% in liquid, and a large amount of manganese sulfate can in crystalline form be separated out from solution;Filtering layer crystallizes dumping Glassware constantly runs and stirs manganese sulfate crystalli-zation cake up and down under motor drive, the attachment saturation in making manganese sulfate crystallize Solution basic filtering can take out dry manganese sulfate crystallization from dumping pit, also ensure sulphur to the filtrate area of filtering drying machine lower part The permeability of sour manganese crystalli-zation cake, the manganese sulfate concentration in the filtrate in filtering drying machine lower part filtrate area is only 4.2%, passes through filter Liquid pump inlet tube is sent to filtrate pump, and subsequent processing is sent to by filtrate pump discharge pipe under the promotion of filtrate pump, without sending back to again Crystallizing evaporator continues to evaporate moisture content, so manganese sulfate solution crystallization processes of the present invention are a kind of very energy-efficient crystallization processes.
Description of the drawings
Fig. 1 is manganese sulfate solution crystallization apparatus figure of the present invention, wherein:1 is manganese sulfate solution inlet tube, and 2 be forced circulation Pump inlet pipe, 3 be forced circulation pump, and 4 be forced circulation pump discharge pipe, and 5 be heater, and 6 be heater outlet pipe, and 7 be evaporation Crystallizer, 8 be temperature control valve (TCV), and 9 be indirect steam outlet, and 10 go out for heating steam inlet pipe, 11 for heater condensed water Mouth pipe, 12 be condensate water pot, and 13 be condensating water outlet tube, and 14 be magma pump inlet pipe, and 15 pump for magma, and 16 be magma pump discharge Pipe, 17 be filtering drying machine, and 18 be filter element, and 19 crystallize dumping glassware for filtering layer, and 20 be motor, and 21 be dumping pit, 22 It is filtrate pump inlet tube for compressed air inlet pipe, 23,24 be filtrate pump, and 25 be filtrate pump discharge pipe.
Specific implementation mode
Manganese sulfate solution is sent to by manganese sulfate solution inlet tube 1 in forced circulation pump inlet tube 2, in forced circulation pump 3 Promotion under with solution in crystallizing evaporator 7 together be sent in 5 tube side of heater by forced circulation pump discharge pipe 4, heat Steam is sent to by heating steam inlet pipe 10 in 5 shell side of heater, and the solution in 5 tube side of heater is during flowing up Strong heat exchange is carried out with the heating steam in shell side, solution obtains heating and gradually temperature raising, while in crystallizing evaporator 7 Pressure steps up, and the solubility of solution manganese sulfate during pressure-raising temperature raising can be reduced by Zhejiang reaches hypersaturated state precipitation knot Crystalline substance, when solution pressure reaches 0.25MPa, and temperature is 138 DEG C, the solubility of manganese sulfate is 4.2% in solution, a large amount of sulfuric acid Manganese can in crystalline form be separated out from solution, due to gravity effect it can sink collection arrive 7 lower part of crystallizing evaporator, evaporative crystallization Continue to recycle in heater 5 and crystallizing evaporator 7 together with the clear liquid on 7 top of device and the solution being supplemented in, feed liquid is recycling During constantly there is manganese sulfate to crystallize out to sink to 7 lower part of crystallizing evaporator, the indirect steam for evaporating generation is conditioned Valve 8 and indirect steam outlet 9 are discharged, and discharge rate is interlocked with the temperature in crystallizing evaporator 7, ensure in crystallizing evaporator 7 Temperature is 138 DEG C, and the condensed water that heater 5 generates is sent to condensate water pot 12 by heater condensating water outlet tube 11, then passes through Condensating water outlet tube 13 is sent out.
The manganese sulfate crystallization of 7 lower part of crystallizing evaporator is when increasing to a certain amount of, by magma pump inlet pipe 14 by sulphur Sour manganese magma is sent in magma pump 15, and filtering drying machine 17 is sent to by magma pump discharge pipe 16 under the promotion of magma pump 15 Interior, filtering drying machine 17 is divided into two regions by filter element 18, and 18 upper area of filter element is magma filter cake area, controls it Pressure is 0.25MPa, and 18 lower area of filter element is filtrate area, it is an atmospheric area, when 18 top magma of filter element Compressed air is then sent to by the magma that filter cake area is sent into charging is stopped when certain volume by compressed air inlet pipe 22 In the top magma filter cake area of filtering drying machine 17, manganese sulfate magma is under the double action of gravity and pressure difference, manganese sulfate magma In saturated solution enter the filtrate area of filtering drying machine 17 lower part through filter element 18, manganese sulfate crystallization can be trapped within The magma filter cake area for filtering 18 top of component, in order to ensure that the permeability of manganese sulfate crystalli-zation cake, filtering layer crystallize dumping glassware 19 and exist Motor 20 constantly runs and stirs manganese sulfate crystalli-zation cake up and down under driving, the attachment saturated solution in making manganese sulfate crystallize Basic filtering finally takes out dry manganese sulfate crystallization, filtration drying to the filtrate area of 17 lower part of filtering drying machine from dumping pit 21 Manganese sulfate concentration in the filtrate in 17 lower part filtrate area of machine is only 4.2%, and filtrate pump 24 is sent to by filtrate pump inlet tube 23, Subsequent processing is sent to by filtrate pump discharge pipe 25 under the promotion of filtrate pump 24.
The above is only a preferred embodiment of the present invention, it should be pointed out that for those skilled in the art For, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications should also regard For protection scope of the present invention.

Claims (4)

1. a kind of manganese sulfate solution crystallization apparatus, which is characterized in that connect temperature control valve (TCV) including crystallizing evaporator (7) top (8), temperature control valve (TCV) connection indirect steam outlet (9), crystallizing evaporator (7) side lower end passes through forced circulation pump inlet tube (2) it is connect with forced circulation pump (3), forced circulation pump inlet tube (2) connects solution inlet port close to one end of forced circulation pump (3) Pipe, crystallizing evaporator (7) side upper end are connect by heater outlet pipe (6) with heater (5), and heater (5) other end is logical It crosses pressure circulating-pump outlet pipe (4) to connect with forced circulation pump (3), heater (5) side connection heating steam inlet tube mouth (10), Heater (5) lower end side connects condensate water pot (12), condensate water pot (12) bottom end by heater condensed water outlet spout (11) Condensed water outlet spout (13) is connected, the bottom end of crystallizing evaporator (7) is connect by magma pump inlet pipe (14) with magma pump (15), Magma pump (15) is connect by magma pump discharge pipe (16) with filtering drying machine (17) top side, filtering drying machine (17) top The other side is equipped with compressed air inlet pipe (22), and filtering drying machine (17) side is equipped with dumping pit (21), filtering drying machine (17) Interior to be equipped with filter element (18), connection filtering layer crystallizes dumping glassware (19) and extends to inside among filtering drying machine (17) top Above filter element (18), filtering layer crystallizes connection motor (20) on dumping glassware (19), and filtering drying machine (17) bottom end passes through Filtrate pump inlet tube (23) connects filtrate pump (24), and filtrate pump (24) is equipped with filtrate pump outlet spout (25).
2. manganese sulfate solution crystallization apparatus according to claim 1, which is characterized in that filter house in filtering drying machine (17) Part (18) upper area pressure is 0.25MPa, and lower area is normal pressure.
3. a kind of working method of manganese sulfate solution crystallization apparatus as described in claim 1 and 2.
4. the working method of manganese sulfate solution crystallization apparatus according to claim 3, which is characterized in that the operating pressure For 0.25MPa, the operating temperature is 138 DEG C.
CN201810089909.7A 2018-01-30 2018-01-30 A kind of manganese sulfate solution crystallization apparatus and method Pending CN108557894A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109052482A (en) * 2018-11-02 2018-12-21 湖南广义节能装备有限公司 It is a kind of for solving the problems, such as the tiny device and method of manganese sulfate class material crystal
CN109453538A (en) * 2018-11-23 2019-03-12 衡阳市晋宏精细化工有限公司 The crystallization making apparatus of the rapid drying and moulding of energy
CN110548310A (en) * 2019-09-10 2019-12-10 贵州大龙汇成新材料有限公司 manganese sulfate solution purification treatment equipment
CN113663356A (en) * 2021-08-23 2021-11-19 广西埃索凯新材料科技有限公司 Crystallization impurity removal monitoring system applied to manganese sulfate production

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CN101239730A (en) * 2008-01-30 2008-08-13 江西赣锋锂业股份有限公司 Method and device for producing crystal anhydrous lithium chloride
CN203315784U (en) * 2013-01-18 2013-12-04 内乡县乌克生物化学制品有限公司 Scraper crystallization separator
CN105883926A (en) * 2014-10-27 2016-08-24 北京春景辉节能环保科技有限公司 Evaporative crystallization apparatus for manganese sulfate monohydrate
CN207957789U (en) * 2018-01-30 2018-10-12 江苏迈克化工机械有限公司 A kind of manganese sulfate solution crystallization apparatus

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001091874A1 (en) * 2000-05-29 2001-12-06 Basf Aktiengesellschaft Device for producing crystals
US20030180202A1 (en) * 2000-05-29 2003-09-25 Ellen Peter Mark Device for producing crystals
CN101239730A (en) * 2008-01-30 2008-08-13 江西赣锋锂业股份有限公司 Method and device for producing crystal anhydrous lithium chloride
CN203315784U (en) * 2013-01-18 2013-12-04 内乡县乌克生物化学制品有限公司 Scraper crystallization separator
CN105883926A (en) * 2014-10-27 2016-08-24 北京春景辉节能环保科技有限公司 Evaporative crystallization apparatus for manganese sulfate monohydrate
CN207957789U (en) * 2018-01-30 2018-10-12 江苏迈克化工机械有限公司 A kind of manganese sulfate solution crystallization apparatus

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109052482A (en) * 2018-11-02 2018-12-21 湖南广义节能装备有限公司 It is a kind of for solving the problems, such as the tiny device and method of manganese sulfate class material crystal
CN109453538A (en) * 2018-11-23 2019-03-12 衡阳市晋宏精细化工有限公司 The crystallization making apparatus of the rapid drying and moulding of energy
CN110548310A (en) * 2019-09-10 2019-12-10 贵州大龙汇成新材料有限公司 manganese sulfate solution purification treatment equipment
CN113663356A (en) * 2021-08-23 2021-11-19 广西埃索凯新材料科技有限公司 Crystallization impurity removal monitoring system applied to manganese sulfate production

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