CN107617228A - A kind of low-temperature evaporation crystallization apparatus for being used to prepare magnesium sulfate crystals and the method for crystallising based on the device - Google Patents
A kind of low-temperature evaporation crystallization apparatus for being used to prepare magnesium sulfate crystals and the method for crystallising based on the device Download PDFInfo
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- CN107617228A CN107617228A CN201710959639.6A CN201710959639A CN107617228A CN 107617228 A CN107617228 A CN 107617228A CN 201710959639 A CN201710959639 A CN 201710959639A CN 107617228 A CN107617228 A CN 107617228A
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- magnesium sulfate
- cell body
- evaporation
- evaporator tank
- crystallising
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Abstract
The invention discloses a kind of low-temperature evaporation crystallization apparatus for being used to prepare magnesium sulfate crystals and the method for crystallising based on the device, described device include the parts such as fixed mount, one section of evaporator tank, dual circulation groove, heater, sealing device, air-introduced machine, densitometer, spray equipment, feed tube, drain pipe.The method for crystallising is by regulating and controlling temperature and solution density, while by multi-stage evaporation separation of solid and liquid, removal of impurities, is concentrated, crystallized, obtain high-purity sulfuric acid magnesium crystal product.Treatment fluid source of the present invention is wide, and the leaching waste liquid available for containing magnesium sulfate is handled, it can also be used to the preparation of pure magnesium sulfate.This device can also be used in other middle low-temperature evaporation crystallization treatment techniques.
Description
Technical field
The invention belongs to low-temperature evaporation crystallization technique field, waste water low-temperature evaporation process field can equally use, specifically
Ground, the present invention relates to a kind of low-temperature evaporation crystallization apparatus for preparing magnesium sulfate crystals and the method for crystallising based on the device.
Background technology
With the production development of society, the demand of magnesium sulfate is huge, and there is many deficiencies for the preparation of traditional magnesium sulfate
Part is urgently to be resolved hurrily.The production generally use sulfuric acid process of traditional magnesium sulfate crystals, crystal, condensation used are produced using crystallisation by cooling
Device contains the more coiled pipes of weight and cooling jacket, during by (80 DEG C) coolings of high temperature, not only needs a large amount of condensed waters, and crystallized product is easy to stick
Wall.The method of another kind production magnesium sulfate crystals is to add crystal seed in saturation Adlerika, make magnesium sulfate in solution from
By crystallizing, but the crystal grain that the technique obtains is uneven, and subsequent treatment complex procedures.
The shortcomings that for current magnesium sulfate preparation method, patent《A kind of method of magnesium sulfate continuous crystallisation》(Publication No.
CN104058429A), a kind of method of continuous production magnesium sulfate crystallization is disclosed, the cooling of this method second level uses chilled water
Cooling, though effectively increasing the yield of magnesium sulfate, the production of chilled water makes flow more complicated, and energy consumption is higher.Patent《It is empty
Air cooling crystallizing tower》(Publication No. CN201543264U), a kind of cooling crystallization tower using air as medium is disclosed, without cold
But water and steam, energy consumption is low, but the crystallizing tower needs Recycling Mother Solution and drying system, and technological process is long and efficiency is low.
The content of the invention
It is an object of the invention to overcome some shortcomings of traditional magnesium sulfate preparation method, a kind of energy-conservation, efficiently system are proposed
The apparatus and method of standby magnesium sulfate crystallization.
In order to achieve the above object, the present invention adopts the following technical scheme that：
A kind of low-temperature evaporation crystallization apparatus for being used to prepare magnesium sulfate crystals, described device include：Fixed mount 1, several
One section of evaporator tank, several dual circulation grooves, feed tube 3, sealing device 4, drain pipe 5, air-introduced machine 7, heater 8, spray
Device 9, densitometer 11；One section of evaporator tank and dual circulation groove are vertically stacked on fixed mount 1, one section of evaporator tank and two sections of steamings
Sending out groove includes evaporation cell body 2；Evaporation cell body 2 includes top cylinder and bottom cone-shaped bottom land；
In the top layout sealing device 4 of evaporation cell body 2, hole is left in centre, and the hole is used to set one or more air inducing
Machine 7, outside air inducing, make to form certain negative pressure in groove, while agitation treatment liquid, accelerate moisture evaporation；In evaporation cell body 2
Portion is respectively provided with heater for the heating to treatment fluid；
Spray equipment 9 is also set up at the top of evaporation cell body 2, the spray equipment 9 connects with feed tube 3, in evaporator tank
The bottom land of body 2 sets drain pipe 5；
Thermal detector 10 and densitometer 11 are additionally provided with evaporation cell body 2.
Preferably, the material of the fixed mount is according to the size of evaporator tank, from steel construction or concrete structure.
Preferably, the top cylinder of the evaporation cell body 2 is cylinder or multiedge cylinder；Bottom cone-shaped bottom land is circular cone
Body or polygonal pyramid body；The inclination angle of one section of evaporator tank bottom land is 15~30 °, and the inclination angle of dual circulation groove bottom land is 45~50 °.
Preferably, the heater is controllable temperature heater, and its temperature control is partially disposed in groove in treatment fluid, heating part
It is divided into heating tape 8, is arranged in each evaporator tank in a ring close to the position of inwall certain distance (such as apart from evaporator tank inwall 5-
10cm)。
The size of air-introduced machine of the present invention is related to the internal diameter of evaporator tank, the internal diameter ratio of usual air-introduced machine diameter and evaporator tank
1：3 or so.
The present invention is additionally provided with control valve 6 on drain pipe, controls the size of flow.
Present invention also offers based on the above-mentioned crystallization side for being used to prepare the low-temperature evaporation crystallization apparatus of magnesium sulfate crystals
Method, the method for crystallising comprise the following steps：
1) treatment fluid is pumped into one section of evaporator tank, being concentrated into density at 0~45 DEG C reaches 1.23~1.25g/cm3,
Obtain suspension；
2) solid-liquid separation step 1) in gained suspension, obtain liquid phase；
3) gained liquid phase in step 2) is pumped into interior evaporative crystallization to the density at 35~65 DEG C of dual circulation groove to reach
1.33~1.38g/cm3, obtain suspension；
4) solid-liquid separation step 3) in gained suspension, obtain solid phase, dry the solid phase, obtain magnesium sulfate crystals.
In the present invention, the mass concentration of magnesium sulfate is not less than 30% in the treatment fluid, and the mass concentration of sodium ion is
5%~10%, calcium, iron ion mass concentration are not more than 25%, and pH value is 5.5~6.5, and magnesite powder, sulfuric acid can be used to adjust.
Separation of solid and liquid described in step 2), gained solid-phase calcium, the impurity of iron ion；Separation of solid and liquid described in step 4),
Gained liquid phase foreign ion containing sodium ion.
Heretofore described fixed mount is used to fix all evaporator tanks being vertically stacked, and being vertically stacked effectively to be reduced
Occupation area of equipment, and need to be spaced certain altitude between each cell body, make moisture orientation, accelerate evaporation, and later maintenance work to need
Will.
Heretofore described fixed mount is additionally operable to other devices such as the fixed feed tube being connected with cell body, drain pipe.This
One section of evaporator tank described in invention is used for the concentration and evaporation stage for the treatment of fluid, removes the impurity such as molysite, calcium salt；Described two sections
Evaporator tank is used for the impurity such as the crystallization and evaporation stage for the treatment of fluid, magnesium sulfate crystals needed for precipitation, sodium ion and stayed in the solution.
Heretofore described densitometer each arrangement one in each evaporator tank；Described spray equipment is in each evaporation
On groove, spray equipment is connected with feed tube；Described feed tube is arranged in the top edge of evaporator tank, is connected with spray equipment；Institute
The drain pipe stated is arranged in the bottommost at each evaporator tank cone tank bottom.
Magnesium ion, sulfate ion may originate from ore leachate in heretofore described treatment fluid, and magnesium sulfate containing waste water is also
Can.
When evaporation is carried out in step 1) in the present invention, treatment fluid is persistently sprayed to keep liquid level constant；When step 1)
When liquid level and density reach preset value in middle evaporator tank, suspension is exported and carries out separation of solid and liquid, take clear liquid to next
The evaporation in stage；Gained solid phase is calcic, the impurity of iron plasma.
When evaporation is carried out in step 3) in the present invention, treatment fluid is persistently sprayed to keep liquid level constant；When step 3)
When liquid level and density reach preset value in middle evaporator tank, suspension is exported and carries out separation of solid and liquid, filter residue is sulfuric acid
Magnesium crystal；Gained liquid phase is i.e. containing foreign ions such as sodium ions.
Compared with prior art, the present invention has following characteristics：Treatment fluid source is wide, the leaching waste liquid available for containing magnesium sulfate
Processing, it can also be used to the preparation of pure magnesium sulfate.This device can also be used in other middle low-temperature evaporation crystallization treatment techniques.
Brief description of the drawings
Fig. 1 is the structural representation of low-temperature evaporation crystallization apparatus of the present invention；
Fig. 2 is the top view of one section of evaporator tank；
Fig. 3 is the flow chart of method for crystallising of the present invention.
Reference：1st, fixed mount；2nd, cell body is evaporated；3rd, feed tube；4th, sealing device；5th, drain pipe；6th, control valve；
7th, air-introduced machine；8th, heating tape；9th, spray equipment；10th, thermal detector；11st, densitometer.
Embodiment
With the drawings and specific embodiments, the present invention is further detailed explanation below.
As depicted in figs. 1 and 2, a kind of low-temperature evaporation crystallization apparatus for being used to prepare magnesium sulfate crystals, described device include：
Fixed mount 1, several section of evaporator tank, several dual circulation grooves；Several section of evaporator tank and several dual circulation grooves
It is vertically stacked on fixed mount 1；
One section of evaporator tank and dual circulation groove include evaporation cell body 2；Evaporation cell body 2 includes top cylinder and bottom cone
Shape bottom land；
In the top layout sealing device 4 of evaporation cell body 2, hole is left in centre, and the hole is used to set one or more air inducing
Machine 7, heater is respectively provided with for the heating to treatment fluid in the inside of evaporation cell body 2；
Spray equipment 9 is also set up at the top of evaporation cell body 2, the spray equipment 9 connects with feed tube 3, in evaporator tank
The bottom land of body 2 sets drain pipe 5；
Thermal detector 10 and densitometer 11 are additionally provided with evaporation cell body 2.
The top cylinder of the evaporation cell body 2 is cylinder or multiedge cylinder；Bottom cone-shaped bottom land is cone or more
Pyramid.
The heater is controllable temperature heater, and its temperature control is partially disposed in groove in treatment fluid, and heating part is to add
The torrid zone 8, the position of evaporator tank inwall certain distance is disposed adjacent in a ring.
The present invention is additionally provided with control valve 6 on drain pipe, controls the size of flow.
The heater is controllable temperature heater, and its temperature control is partially disposed in groove in treatment fluid, and heating part is to add
The torrid zone, the position of evaporator tank inwall certain distance is disposed adjacent in a ring.
One section of evaporator tank feed tube is connected with treatment fluid accumulator tank, and treatment fluid is pumped into one section of evaporator tank through feed tube, warp
It is concentrated by evaporation and obtains suspension.
One section of evaporator tank drain pipe is connected with equipment for separating liquid from solid, in one section of evaporator tank gained suspension through separation of solid and liquid,
Liquid phase is pumped into treatment fluid accumulator tank, and solid phase is that impurity transports salvage stores to.
Dual circulation groove feed tube is connected with treatment fluid accumulator tank, and treatment fluid is pumped into dual circulation groove through feed tube, warp
Evaporative crystallization obtains suspension.
Dual circulation groove drain pipe is connected with equipment for separating liquid from solid, in dual circulation groove gained suspension through separation of solid and liquid,
Liquid phase is pumped into tail washings groove, and solid phase is magnesium sulfate crystallization.
Magnesium sulfate crystallization can be sent to drying device, and the magnesium sulfate crystals of the different crystallizations water can be obtained through drying.
Steel construction or concrete structure can be selected according to the size of evaporator tank in the material of fixed mount.
The inwall of evaporator tank requires certain smoothness, especially dual circulation groove, prevents occurring in evaporation and crystal process
Bonding phenomenon.
The size of air-introduced machine is related to the internal diameter of evaporator tank, and the internal diameter ratio of usual air-introduced machine diameter and evaporator tank is 1：3
Left and right.
Thermal detector is usually placed in evaporator tank centered position, ensures the accuracy of thermometric.
The specific embodiment of the present invention is the following is, it is used only as illustrating rather than limitation for the application.
Embodiment 1
Certain chemical plant produces seven water and magnesium sulfate, sulfuric acid is added in magnesite, magnesium sulfate leachate uses low-temperature evaporation
The mode of crystallization.
One section of evaporation is carried out under the conditions of 30 DEG C, and fluid density is steamed to 1.24 or so；Dual circulation is entered under the conditions of 60 DEG C
OK, fluid density is steamed to 1.35 or so, produces magnesium sulfate crystallization.Epsom salt sample quality analyze data such as following table：
| Project | Magnesium sulfate is (with MgSO4·7H2O is counted) w% >= |
| High-class product | 99.5 |
| Certified products | 95.0 |
| Sample | 99.6 |
Embodiment 2
Certain lateritic nickel ore mine, a large amount of sulfate wastewaters, wherein sulphur are produced using " acidleach-vulcanization sink nickel " process engineering
Sour content of magnesium accounts for the 80% of total sulfate amount, because it contains substantial amounts of magnesium ion and other metal ions, so can not be direct
Discharge, it is necessary to handle it, on the one hand can effectively utilize the magnesium resource in waste water, on the other hand can improve again red
Native nickel ore resource comprehensive utilization ratio.
Using this device, one section of evaporation is carried out under the conditions of 40 DEG C, and fluid density is steamed to 1.24 or so, and pH value control exists
6.0 or so, remove iron ion, calcium ion and other impurities ion；Dual circulation is carried out under the conditions of 60 DEG C, fluid density steam to
1.35 or so, produce magnesium sulfate crystallization.Epsom salt sample quality analyze data such as following table：
| Project | MgSO4·7H2O≥ | Iron (Fe)≤ | Chloride≤ | Water-insoluble |
| Grade A | 98.0 | 0.005 | 0.30 | 0.10 |
| Certified products | 95.0 | 0.01 | 0.50 | 0.15 |
| Sample | 98.67 | 0.003 | 0.46 | 0.08 |
Embodiment 3
The waste water in certain chemical plant contains trace element ion in a large amount of magnesium sulfate, and potassium, calcium, silicon, boron, iron, zinc etc., this
A little elements can improve soil, can effectively facilitate plant growth.Therefore liquid waste processing, recovery wherein beneficial element, not only may be used
To prevent the pollution of the environment, can also increase economic efficiency.
PH is brought to 6.0 during wastewater treatment, and one section of evaporation is carried out at normal temperatures, and fluid density is steamed to 1.24 or so；Two sections
Evaporation is carried out under the conditions of 40 DEG C or so, and fluid density is steamed to 1.35 or so, produces sulphate of potash magnesia crystallization.Last drying process can
Magnesium sulfate potash fertilizer is obtained, parameter is as follows：
Potassium oxide (K2O) >=22%；
Magnesium (MG) >=6%；
Sulphur (S) >=16%；
Moisture≤2%.
It should be noted last that the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted.Although ginseng
The present invention is described in detail according to embodiment, it will be apparent to an ordinarily skilled person in the art that the technical side to the present invention
Case is modified or equivalent substitution, and without departure from the spirit and scope of technical solution of the present invention, it all should cover in the present invention
Right among.
Claims (5)
1. a kind of low-temperature evaporation crystallization apparatus for being used to prepare magnesium sulfate crystals, it is characterised in that described device includes：Fixed mount
(1), several section of evaporator tank, several dual circulation grooves, feed tube (3), sealing device (4), drain pipe (5), air-introduced machine
(7), heater (8), spray equipment (9), densitometer (11)；
One section of evaporator tank and dual circulation groove are vertically stacked on fixed mount (1), and one section of evaporator tank and dual circulation groove wrap
Include evaporation cell body (2)；Evaporation cell body (2) includes top cylinder and bottom cone-shaped bottom land；
In the top layout sealing device (4) of evaporation cell body (2), hole is left in centre, and the hole is used to set one or more air inducing
Machine (7), heater is respectively provided with the inside of evaporation cell body (2) for the heating to treatment fluid；
Spray equipment (9) is also set up at the top of evaporation cell body (2), the spray equipment (9) connects with feed tube (3), steamed
The bottom land for sending out cell body (2) sets drain pipe (5)；
Thermal detector (10) and densitometer (11) are additionally provided with evaporation cell body (2).
2. the low-temperature evaporation crystallization apparatus according to claim 1 for being used to prepare magnesium sulfate crystals, it is characterised in that described
Heater is controllable temperature heater, and its temperature control is partially disposed in groove in treatment fluid, and heating part is heating tape (8), in ring
Shape is disposed adjacent to the position of evaporator tank inwall certain distance.
It is 3. described based on the method for crystallising for being used to prepare the low-temperature evaporation crystallization apparatus of magnesium sulfate crystals described in claim 1
Method for crystallising comprises the following steps：
1) treatment fluid is pumped into one section of evaporator tank, being concentrated into density at 0~45 DEG C reaches 1.23~1.25g/cm3, hanged
Turbid；
2) solid-liquid separation step 1) in gained suspension, obtain liquid phase；
3) by gained liquid phase in step 2) be pumped into dual circulation groove evaporative crystallization to the density at 35~65 DEG C reach 1.33~
1.38g/cm3, obtain suspension；
4) solid-liquid separation step 3) in gained suspension, obtain solid phase, dry the solid phase, obtain magnesium sulfate crystals.
4. method for crystallising according to claim 3, it is characterised in that the mass concentration degree of magnesium sulfate is not in the treatment fluid
Less than 30%, the mass concentration of sodium ion is 5%~10%, and calcium, iron ion mass concentration are not more than 25%, pH value is 5.5~
6.5。
5. method for crystallising according to claim 3, it is characterised in that separation of solid and liquid described in step 2), gained solid phase contain
The impurity of calcium, iron ion；Separation of solid and liquid described in step 4), gained liquid phase foreign ion containing sodium ion.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710959639.6A CN107617228B (en) | 2017-10-16 | 2017-10-16 | Low-temperature evaporation crystallization device for preparing magnesium sulfate crystals and crystallization method based on device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710959639.6A CN107617228B (en) | 2017-10-16 | 2017-10-16 | Low-temperature evaporation crystallization device for preparing magnesium sulfate crystals and crystallization method based on device |
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| CN107617228A true CN107617228A (en) | 2018-01-23 |
| CN107617228B CN107617228B (en) | 2019-12-17 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109045744A (en) * | 2018-08-30 | 2018-12-21 | 山东亚邦化工科技有限公司 | The method and apparatus for preparing acesulfame potassium crystallization of continuous-stable |
| CN109078359A (en) * | 2018-08-30 | 2018-12-25 | 山东亚邦化工科技有限公司 | A kind of technique and device for acesulfame potassium sulfonation hydrolysis liquid continuous extration |
| CN112429754A (en) * | 2020-11-15 | 2021-03-02 | 盘锦泓实环保科技有限公司 | Large-particle magnesium sulfate cooling crystallization method and system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2154734Y (en) * | 1993-03-09 | 1994-02-02 | 何晓东 | 3-effect vacuum concentration evaporator |
| CN206027121U (en) * | 2016-08-31 | 2017-03-22 | 西北民族大学 | Novel tea polyphenol evaporative concentration device |
-
2017
- 2017-10-16 CN CN201710959639.6A patent/CN107617228B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2154734Y (en) * | 1993-03-09 | 1994-02-02 | 何晓东 | 3-effect vacuum concentration evaporator |
| CN206027121U (en) * | 2016-08-31 | 2017-03-22 | 西北民族大学 | Novel tea polyphenol evaporative concentration device |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109045744A (en) * | 2018-08-30 | 2018-12-21 | 山东亚邦化工科技有限公司 | The method and apparatus for preparing acesulfame potassium crystallization of continuous-stable |
| CN109078359A (en) * | 2018-08-30 | 2018-12-25 | 山东亚邦化工科技有限公司 | A kind of technique and device for acesulfame potassium sulfonation hydrolysis liquid continuous extration |
| CN109078359B (en) * | 2018-08-30 | 2020-11-06 | 山东亚邦化工科技有限公司 | Process and device for continuous extraction of acesulfame potassium sulfonated hydrolysate |
| CN109045744B (en) * | 2018-08-30 | 2021-04-27 | 山东亚邦化工科技有限公司 | Method and device for continuously and stably preparing acesulfame potassium crystals |
| CN112429754A (en) * | 2020-11-15 | 2021-03-02 | 盘锦泓实环保科技有限公司 | Large-particle magnesium sulfate cooling crystallization method and system |
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