CN109896950A - A kind of system and technique of calcium gluconate continuous crystallisation - Google Patents
A kind of system and technique of calcium gluconate continuous crystallisation Download PDFInfo
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- CN109896950A CN109896950A CN201910294514.5A CN201910294514A CN109896950A CN 109896950 A CN109896950 A CN 109896950A CN 201910294514 A CN201910294514 A CN 201910294514A CN 109896950 A CN109896950 A CN 109896950A
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 107
- 229960004494 calcium gluconate Drugs 0.000 title claims abstract description 53
- 239000004227 calcium gluconate Substances 0.000 title claims abstract description 53
- 235000013927 calcium gluconate Nutrition 0.000 title claims abstract description 53
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 44
- 239000002002 slurry Substances 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 239000000047 product Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000006228 supernatant Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000009834 vaporization Methods 0.000 claims description 31
- 230000008016 vaporization Effects 0.000 claims description 31
- 239000007788 liquid Substances 0.000 claims description 15
- 238000001704 evaporation Methods 0.000 claims description 13
- 230000008020 evaporation Effects 0.000 claims description 12
- 239000007921 spray Substances 0.000 claims description 9
- 239000000498 cooling water Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000001351 cycling effect Effects 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 abstract description 20
- 239000013078 crystal Substances 0.000 abstract description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 5
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- 238000012545 processing Methods 0.000 abstract description 3
- 230000000737 periodic effect Effects 0.000 abstract 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 10
- 229960005069 calcium Drugs 0.000 description 10
- 229910052791 calcium Inorganic materials 0.000 description 10
- 239000011575 calcium Substances 0.000 description 10
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 6
- 239000008103 glucose Substances 0.000 description 6
- 238000010025 steaming Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 4
- 241000219095 Vitis Species 0.000 description 4
- 235000009754 Vitis X bourquina Nutrition 0.000 description 4
- 235000012333 Vitis X labruscana Nutrition 0.000 description 4
- 235000014787 Vitis vinifera Nutrition 0.000 description 4
- 239000000174 gluconic acid Substances 0.000 description 4
- 235000012208 gluconic acid Nutrition 0.000 description 4
- NEEHYRZPVYRGPP-IYEMJOQQSA-L calcium gluconate Chemical compound [Ca+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O NEEHYRZPVYRGPP-IYEMJOQQSA-L 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 210000002966 serum Anatomy 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 206010039509 Scab Diseases 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000011549 crystallization solution Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
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- 235000019580 granularity Nutrition 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 206010001497 Agitation Diseases 0.000 description 1
- 238000010793 Steam injection (oil industry) Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
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- 238000011084 recovery Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 108010048734 sclerotin Proteins 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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Classifications
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention relates to the systems and technique of a kind of calcium gluconate continuous crystallisation, including MVR evaporator, three-level vacuum shwoot crystallizer, vapor jet vacuum pump, mixing condenser, heat exchanger, slurry tank, centrifuge, pelletizer, drying machine, the processing step are as follows: it is 50-52% that calcium gluconate supernatant, which enters MVR evaporator to be concentrated into material concentration, enter multi-stage vacuum shwoot crystallizer later and carries out the crystallization of shwoot continuous cooling, magma after crystallization enters the isolated crystal material of centrifuge after slurry tank, enter granulator after cleaning impurity with pure water, boiled bed drying obtains calcium gluconate finished product.The present invention overcomes the shortcomings that periodic crystallisation completely, realize calcium gluconate production Crystallization Continuity, not only device structure is compact, occupied area is small, it greatly reduces energy consumption and production cost, improve working efficiency, energy conservation is in 40-50%, and crystalline particle dynamics is uniform, any surface finish, stable product quality.
Description
Technical field
The present invention relates to calcium gluconate crystallization arts, and in particular to a kind of continuous knot of calcium gluconate vacuum shwoot cooling
Crystallographic system system and technique.
Background technique
Disclosing the information of the background technology part, it is only intended to increase understanding of the overall background of the invention, without certainty
It is considered as recognizing or implying in any form that information composition has become existing skill well known to persons skilled in the art
Art.
Calcium gluconate medicine, food, in terms of have important purposes, especially in terms of medicine, grape
Calciofon facilitates the formation of sclerotin, and maintains the normal and excitability of nerves and muscles, becomes the preferred product that people replenish the calcium.
The production technology of calcium gluconate is mainly neutralized by glycoxidative gluconic acid, gluconic acid and the calcium of being made of grape as gluconic acid
Calcium finally carries out 3 parts of purification composition again.
Evaporating, concentrating and crystallizing link in subtractive process is directly related to the production cost and product quality of product, at present Portugal
Technique is stood still for crystals in the crystallization of grape Calciofon after chilling and accounts for 95% or more in calcium gluconate industry at home, there are energy consumptions
Height takes up a large area, the problems such as the degree of automation is low, labor productivity is low, and it is uneven that more important is grain size numbers, takes off
Water is difficult, has seriously affected the quality of product.
In patent CN201810245150.7, a kind of continuous cooling rapid crystallization method of calcium gluconate is disclosed, it is main
It to include dissolution, oxidation, concentration, filtering, decoloration, movement crystallization, drying and other steps, preparation side of the invention to calcium gluconate
Method is described in detail, but unintelligible to continuous cooling crystal system and process description.
In patent 201410543277.9, a kind of vacuum shwoot cooling continuous crystallisation device is disclosed, what which used
Capital equipment is that flash-pot and three-level vacuum shwoot crystallizer carry out cooling continuous crystallisation, and flash-pot needs to connect cooling system
System, surface-cooler takes up a large area, cooling efficiency is low, the system there are system complex, equipment is huge the disadvantages of.
Summary of the invention
In order to overcome the above problem, the present invention provides the system and technique of a kind of calcium gluconate continuous crystallisation, low energy consumption,
Device structure is simple, occupied area is small, investment cost is low, labor productivity is high, grain size number is uniform, and non-scaling does not scab, can
Long-term continuity production.
To realize the above-mentioned technical purpose, The technical solution adopted by the invention is as follows:
A kind of calcium gluconate continuous crystallisation vacuum shwoot crystallizer, comprising: vaporization chamber and crystallisation chamber, the vaporization chamber
Positioned at the top of crystallisation chamber, spray equipment and exhaust outlet are provided at the top of vaporization chamber；The vaporization chamber is straight-tube shape, the crystallization
Room is pyramidal structure；The crystallisation chamber is provided with interior circulation guide shell, the side wall of the crystallisation chamber be provided with multiple feed inlets and
Discharge port；The bottom of the crystallisation chamber also sets up drain, and the crystallisation chamber bottom is connected with forced circulation pump, the vaporization chamber
Top is connected with vapor jet vacuum pump.
The structure type of the crystallizer top straight tube lower cone section of the application, facilitates processing and manufacturing, and it is brilliant to can also be achieved precipitation
Efficiently separating for body particle and supernatant, eliminates settler；Meanwhile in vaporization chamber top design spray equipment, avoid
Interior wall construction phenomenon；Multiple discharge ports are arranged in the cone section of crystallizer, different positions can be selected to arrange according to different Grained Requirements
Material；It is also provided with multiple feed inlets, is provided with special exhaust, drainage arrangement, for easy to operate and security consideration.
Forced circulation pump described herein is axial-flow pump.
In order to guarantee to obtain preferable evaporation effect, in some embodiments, direct tube section and centrum section ratio are as follows: 1:1~
The angle of 3:2, cone segments and horizontal plane is 65 °~83 °, if the angle of cone segments and horizontal plane leads to crystal grain less than 65 °
Decline with the separative efficiency of supernatant, equipment yield reduces；If the angle of cone segments and horizontal plane is greater than 83 °, different granularities
Crystal be difficult to be effectively dispersed in the different parts of crystallisation chamber side wall, the partial size difference after discharge is big.
In some embodiments, solid particle and the liquid in crystallization suspension are separated from discharge port with centrifuge, Gu
Body substance obtains calcium gluconate finished product through pelletizer, drying machine；Liquid enters vacuum shwoot crystallizer vacuum by feed inlet and steams
Hair crystallization.
In some embodiments, 3 discharge ports, the glucose of collection are equally spacedly provided on the side wall of the crystallisation chamber
The partial size approximate range of sour calcium crystallization are as follows:
(1) apart from first, ground discharge port: length and diameter is respectively 70-100 and 7-10 μm；
(2) apart from second, ground discharge port: length and diameter is respectively 40-70 and 4-7 μm；
(3) apart from ground third discharge port: length and diameter is respectively 20-50 and 2-5 μm.
The application research is it is also found that: if the first discharge port is too close apart from crystallisation chamber base bleed mouth, the crystal grain easily row of being deposited in
Near port, exhaust outlet is blocked；If too far apart from crystallisation chamber bottom, the collection rate of major diameter crystal grain declines the first discharge port, knot
Brilliant efficiency reduces, and therefore, in some embodiments, the first discharge port is crystallisation chamber side wall length at a distance from crystallisation chamber bottom end
1/3~2/5.
In some embodiments, it is equipped with support tube between interior circulation guide shell and the crystallisation chamber, is steel structure, passes through
Interior circulation guide shell is fixed in crystallizing evaporator by the mode of welding.
In some embodiments, material is conveyed using transfering material pump between each vacuum shwoot crystallizer, transfering material pump is centrifugal pump.
The present invention also provides a kind of systems of calcium gluconate continuous crystallisation, comprising: on MVR evaporator, multistage are any
The vacuum shwoot crystallizer stated, the MVR evaporator, multi-stage vacuum shwoot crystallizer, slurry tank, centrifuge are sequentially connected, institute
It states centrifuge to be also connected with MVR evaporator, vapor jet vacuum pump is provided at the top of each vacuum shwoot crystallizer, it is described
Vapor jet vacuum pump is all connected with condenser.
It needs feed liquid to heat before vacuum shwoot decrease temperature crystalline and is concentrated into certain temperature and concentration, currently used hand
Section is steam heating, the advantages of evaporation and concentration using MVR evaporator:
(1) MVR energy conservation evaporation technique is current international advanced evaporation technique, and energy utilization rate is high, greatly reduces enterprise
Industry operating cost, reduces environmental pollution.
(2) device goes out and needs when starting using except external steam, and when running well, evaporator itself is not needed again
Using external steam source, cooling water and related condensing plant are not needed yet.
(3) it is compared due to providing heat source using compressor with conventional evaporator, the temperature difference is much smaller, can reach mild steaming
Hair greatlys improve product quality, reduces fouling.
(4) it is not necessarily to condenser, structure is very simple with process, full automatic working, continuously-running, securely and reliably.
(5) the evaporator material is in low temperature and do not generate foam in the state of is evaporated, and feed liquid is uniform, does not run material, no
Easy coking.
In some embodiments, the material of the MVR evaporator is transported to multi-stage vacuum shwoot crystallizer by transfering material pump.
In some embodiments, the vacuum shwoot crystallizer is divided into three-level, and first order vacuum shwoot temperature is 75~85
DEG C, relative degree of vacuum is -0.03MPa~-0.05MPa；Second level vacuum shwoot temperature be 60~75 DEG C, relative degree of vacuum be-
0.05MPa~-0.07MPa；Third level vacuum shwoot temperature be 45~60 DEG C, relative degree of vacuum be -0.07MPa~-
0.09MPa。
In some embodiments, return to cooling tower in the cooling water return water of the condenser, it is uncooled under secondary steam
It is taken away by vacuum pump.
In some embodiments, the centrifuge is also successively connected with pelletizer, ebullated bed.
The present invention also provides a kind of methods of calcium gluconate continuous crystallisation, comprising:
1) calcium gluconate supernatant be introduced into MVR evaporator be concentrated into material concentration be 50-52%, secondary steam by
Top discharge enters heat exchanger after compressor compresses and condenses, and is sucked by circulating pump, enters back into heating tube, continues cycling through；
2) MVR serum outlet is sequentially sent to three-level vacuum shwoot crystallizer by transfering material pump by pipeline；
3) calcium gluconate slurries are expelled to slurry tank from No. three vacuum shwoot crystallizers, into being centrifugated to obtain glucose
Sour calcium crystallized stock, clear liquid are back to the evaporation of MVR evaporator after heat exchanger preheats, the calcium gluconate crystallization that centrifuge is thrown away
Material enters granulator after cleaning impurity with pure water, boiled bed drying obtains calcium gluconate finished product.
In some embodiments, the pressure for the life steam that the vacuum shwoot crystallizer uses is 0.6-1.0Mpa.
The beneficial effects of the present invention are:
(1) clear liquid after shwoot crystallization is back to MVR evaporator after heat exchanger preheats, and energy-saving effect is good, comprehensive energy consumption
Low, device structure is simple, occupied area is few, does not need refrigeration system, and operating cost is low, and labor efficiency is greatly improved.
(2) structure type of crystallizer top straight tube lower cone section is, it can be achieved that precipitate crystal the effective of particle and supernatant
Separation, eliminates settler, different position discharges can be also selected according to different Grained Requirements.
(3) grain size number is uniform, by force in circulation shwoot cooling, avoid scab, plugging the problem of, can be long-term
Consecutive production.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is system flow chart of the invention, wherein 1. MVR evaporator, 2. No.1 forced circulation pump, 3. level-one vacuum
Crystallizer, 4. No.1 vapor jet vacuum pump, 5. No. two forced circulation pumps, 6. secondary vacuum crystallizer, 7. No. two steam injections
Vacuum pump, 8. No. three forced circulation pumps, 9. three-level vacuum crystallizer, 10. No. three vapor jet vacuum pumps,Slurry tank.
Fig. 2 is the structure chart of crystallization apparatus of the present invention, wherein 1. vaporization chambers, 2. crystallisation chambers, 3. spray equipments, 4. are forced
Circulating pump, 5. first row ports, 6. secondary steams, 7. feed inlets, 8. discharge ports, 9. drains, 10. guide shells, 11. supports
Bar.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used in this application have logical with the application person of an ordinary skill in the technical field
The identical meanings understood.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Uneven for current calcium gluconate crystal system grain size number as background technique is introduced, dehydration is tired
Difficulty, the problem that the device is complicated, production efficiency is low.Therefore, the present invention proposes the system and work of a kind of calcium gluconate continuous crystallisation
Skill, including MVR evaporator, three-level vacuum shwoot crystallizer, vapor jet vacuum pump, mixing condenser, heat exchanger, slurry tank,
Centrifuge, pelletizer, drying machine；It is 50- that calcium gluconate supernatant, which is introduced into MVR evaporator and is concentrated into material concentration,
52%, three concatenated vacuum shwoot crystallizers are successively continued through through transfering material pump carries out the crystallization of shwoot continuous cooling, glucose
Sour calcium slurries are expelled to slurry tank from third level vacuum shwoot crystallizer, into slurry tank after be centrifugated to obtain crystallized stock, clearly
Liquid is back to MVR evaporator.The crystallized stock that centrifuge is thrown away enters granulator, boiling after cleaning impurity with pure water
Bed is dried to obtain calcium gluconate finished product.
Connection all connection vapor jet vacuum pump, bottom connect forced circulation pump at the top of every level-one vacuum shwoot crystallizer；
It is cooling into mixing condenser after steam respectively enters every grade of vapor jet vacuum pump, cooling tower is returned in cooling water return water, not
Secondary steam under condensation is taken away by vacuum pump.
Vacuum shwoot crystallizer is circulating cooling crystallizer in forcing, comprising: vaporization chamber, crystallisation chamber, interior circulation guide shell
And forced circulation pump, bottom use forced circulation pump, and support tube is equipped between interior circulation guide shell and crystallisation chamber, lower cone section is equipped with
Multiple liquor inlet, multiple slurry outlets, bottom are equipped with drain, and the granule size of crystalline particle can be adjusted in a certain range
Section.Material is conveyed using transfering material pump between vacuum shwoot crystallizer, transfering material pump is centrifugal pump.
The vacuum degree of vacuum shwoot crystallizer is pumped by vapor jet vacuum and is maintained, and incoagulable gas is extracted out by vacuum pump is
System.First order vacuum shwoot temperature is 75~85 DEG C, and relative degree of vacuum is -0.03MPa~-0.05MPa；Second level vacuum shwoot
Temperature is 60~75 DEG C, and relative degree of vacuum is -0.05MPa~-0.07MPa；Third level vacuum shwoot temperature is 45~60 DEG C,
Relative degree of vacuum is -0.07MPa~-0.09MPa.
Crystallizer feed solution cooling is that high speed is formed in the nozzle that vapor jet vacuum pumps with raw steam (0.6-1.0Mpa)
It flows, forms high vacuum around high velocity stream, shwoot water is taken away, and crystallization solution is made to cool down.
A kind of process flow of calcium gluconate continuous crystallisation includes:
1) calcium gluconate supernatant be introduced into MVR evaporator be concentrated into material concentration be 50-52%, secondary steam by
Top discharge enters heat exchanger after compressor compresses and condenses, and is sucked by circulating pump, enters back into heating tube, continues cycling through.
2) MVR serum outlet is sequentially sent to three-level vacuum shwoot crystallizer by transfering material pump by pipeline；
3) calcium gluconate slurries are expelled to slurry tank from No. three vacuum shwoot crystallizers, into being centrifugated to obtain glucose
Sour calcium crystallized stock, clear liquid are back to the evaporation of MVR evaporator after heat exchanger preheats, the calcium gluconate crystallization that centrifuge is thrown away
Material enters granulator after cleaning impurity with pure water, boiled bed drying obtains calcium gluconate finished product.
In order to enable those skilled in the art can clearly understand technical solution of the present invention, below with reference to tool
The embodiment of body and the technical solution that the present invention will be described in detail.
Embodiment 1:
As shown in Figure 1, a kind of calcium gluconate continuous crystallizing system MVR evaporator 1., three-level vacuum shwoot crystallizer 3.,
6., 9., vapor jet vacuum pump 4., 7., 10., mixing condenser, heat exchanger, slurry tankCentrifuge, pelletizer, drying machine.
Wherein 1. 3., 6., 9., every grade of vacuum shwoot crystallizer is 3., 6., 9. for sequential connection three-level vacuum shwoot crystallizer for MVR evaporator
Lower part connect forced circulation pump 2., 5., 8., top be connected with vapor jet vacuum pump 4., 7., 10., vapor jet vacuum pump 4.,
7., 10. connect mixing condenser, 9. third level vacuum shwoot crystallizer is connected with centrifuge, centrifuge and pelletizer, drying machine
It is linked in sequence.
Wherein, the specific structure of vacuum shwoot crystallizer includes: vaporization chamber 1 and crystallisation chamber 2, and the vaporization chamber 1 is located at knot
The top of brilliant room 2 is provided with spray equipment 3 and first row port 5 at the top of vaporization chamber 1；The vaporization chamber 1 is straight-tube shape, described
Crystallisation chamber 2 is pyramidal structure；The crystallisation chamber 2 is provided with interior circulation guide shell 10, and the side wall of the crystallisation chamber 2 is provided with 3
Feed inlet 7 and a discharge port 8；The bottom of the crystallisation chamber 2 also sets up drain 9,2 bottom of crystallisation chamber and forced circulation
Pump 4 is connected, 4., 7., 10. 1 top of vaporization chamber is connected with vapor jet vacuum pump.Direct tube section and centrum section ratio are 1:1,
The angle of cone segments and horizontal plane is 79 °；First discharge port is the 2/ of 2 side wall length of crystallisation chamber at a distance from 2 bottom end of crystallisation chamber
5。
The process flow of calcium gluconate continuous crystallisation includes:
1) it is 50% that calcium gluconate supernatant, which is introduced into MVR evaporator and is 1. concentrated by evaporation to material concentration, secondary steaming
Vapour is discharged after compressor compresses by top enters heat exchanger condensation, is sucked by circulating pump, enters back into heating tube, continues cycling through.
2) 3., 6., 9. MVR serum outlet is sequentially sent to three-level vacuum shwoot crystallizer by transfering material pump by pipeline；Wherein,
4., 7., 10. the vacuum degree of vacuum shwoot crystallizer 3., 6., 9. is maintained by vapor jet vacuum pump, incoagulable gas is by vacuum pump
Extraction system.First order vacuum shwoot temperature is 75 DEG C, and relative degree of vacuum is -0.03MPa；Second level vacuum shwoot temperature is
60 DEG C, relative degree of vacuum is -0.07MPa；Third level vacuum shwoot temperature is 60 DEG C, and relative degree of vacuum is -0.08MPa.
The cooling of 2 feed liquid of crystallizer is to be pumped in nozzle 4., 7., 10. to be formed in vapor jet vacuum with raw steam (0.8Mpa)
High velocity stream forms high vacuum around high velocity stream, shwoot water is taken away, and crystallization solution is made to cool down.
3) 9. calcium gluconate slurries are expelled to slurry tank from No. three vacuum shwoot crystallizersInto being centrifugated to obtain Portugal
Grape Calciofon crystallized stock, clear liquid are back to MVR evaporator after heat exchanger preheats and 1. evaporate, the gluconic acid that centrifuge is thrown away
Calcium crystallized stock enters granulator after cleaning impurity with pure water, boiled bed drying obtains calcium gluconate finished product.
4) mother liquor of primary crystallization and recrystallization match, and recycles.
Testing result shows: the residual glucose acid calcium content not crystallized out in mother liquor is 5% hereinafter, the overall rate of recovery can
Up to 95% or more.
Average crystalline size data are obtained by using crystal size distribution (CSD) is measured microscopically, length is at 30-80 μm
Crystal in range covers 90% or more of total crystal, carries out to the data of the length and diameter more than 8000 acicular crystals
It is respectively 51.3 and 5.1 μm that statistical analysis, which can obtain average length (LS) and diameter (2rS), and grain size is crystallized compared with conventional vacuum shwoot
Device is more uniform, energy consumption reduces 40-50%.
Embodiment 2:
A kind of specific structure of calcium gluconate continuous crystallisation vacuum shwoot crystallizer includes: vaporization chamber 1 and crystallisation chamber
2, the vaporization chamber 1 is located at the top of crystallisation chamber 2, is provided with spray equipment 3 and first row port 5 at the top of vaporization chamber 1；The steaming
Hair room 1 is straight-tube shape, and the crystallisation chamber 2 is pyramidal structure；The crystallisation chamber 2 is provided with interior circulation guide shell 10, the crystallization
The side wall of room 2 is provided with multiple feed inlets 7 and discharge port 8；The bottom of the crystallisation chamber also sets up drain 9, the crystallisation chamber
2 bottoms are connected with forced circulation pump 4,4., 7., 10. 2 top of vaporization chamber is connected with vapor jet vacuum pump pump.
The operation method of above-mentioned apparatus are as follows:
Calcium gluconate supernatant is transported to multi-stage vacuum shwoot crystallizer by transfering material pump through the material of MVR evaporator 1.
3., 6., 9., material through vacuum shwoot crystallizer 3., 6., 9. feed inlet 7 enter, under the drive of bottom forced circulation pump 4 in
It is contacted in interior circulation guide shell 10 with a large amount of low-temperature circulating feed liquids, flows up and enter near 2 liquid level of crystallisation chamber together, in steam
Shwoot cooling precipitates crystal under the suction function of ejector vacuum pump 4., 7., 10., passes sequentially through the straight tube and lower cone section of crystallizer 2,
Variable grain solid falls into lower cone section different parts in infall process, is opened according to required crystalline product particle size different
Different-grain diameter crystalline product can be obtained in 8 valve of discharge port.
The structure type of the crystallizer top straight tube lower cone section of the application, facilitates processing and manufacturing, and it is brilliant to can also be achieved precipitation
Efficiently separating for body particle and supernatant, eliminates settler；Meanwhile in vaporization chamber top design spray equipment 3, avoid
Interior wall construction phenomenon；Multiple discharge ports 8 are arranged in the cone section of crystallizer, different positions can be selected to arrange according to different Grained Requirements
Material；It is also provided with multiple feed inlets 7, is provided with special exhaust, drainage arrangement, for easy to operate and security consideration.
Embodiment 3:
A kind of specific structure of calcium gluconate continuous crystallisation vacuum shwoot crystallizer includes: vaporization chamber 1 and crystallisation chamber
2, the vaporization chamber 1 is located at the top of crystallisation chamber 2, is provided with spray equipment 3 and first row port 5 at the top of vaporization chamber 1；The steaming
Hair room 1 is straight-tube shape, and the crystallisation chamber 2 is pyramidal structure；The crystallisation chamber 2 is provided with interior circulation guide shell 10, the crystallization
The side wall of room 2 is provided with multiple feed inlets 7 and discharge port 8；The bottom of the crystallisation chamber also sets up drain 9, the crystallisation chamber
2 bottoms are connected with forced circulation pump 4,4., 7., 10. 2 top of vaporization chamber is connected with vapor jet vacuum pump pump.
It is equipped with support tube 11 between the interior circulation guide shell 10 and crystallisation chamber 2, is steel structure, by welding
Interior circulation guide shell 10 is fixed in crystallizing evaporator.
In order to guarantee to obtain preferable evaporation effect, in the present embodiment, direct tube section and centrum section ratio are as follows: 1:1~3:
2, the angle of cone segments and horizontal plane is 65 °~83 °, if the angle of cone segments and horizontal plane less than 65 °, cause crystal grain with
The separative efficiency of supernatant declines, and equipment yield reduces；If the angle of cone segments and horizontal plane is greater than 83 °, different granularities
Crystal is difficult to be effectively dispersed in the different parts of crystallisation chamber side wall, and the partial size difference after discharge is big.
Embodiment 4:
A kind of specific structure of calcium gluconate continuous crystallisation vacuum shwoot crystallizer includes: vaporization chamber 1 and crystallisation chamber
2, the vaporization chamber 1 is located at the top of crystallisation chamber 2, is provided with spray equipment 3 and first row port 5 at the top of vaporization chamber 1；The steaming
Hair room 1 is straight-tube shape, and the crystallisation chamber 2 is pyramidal structure；The crystallisation chamber 2 is provided with interior circulation guide shell 10, the crystallization
The side wall of room 2 is provided with multiple feed inlets 7 and discharge port 8；The bottom of the crystallisation chamber also sets up drain 9, the crystallisation chamber
2 bottoms are connected with forced circulation pump 4,4., 7., 10. 2 top of vaporization chamber is connected with vapor jet vacuum pump pump.
Support tube 11 is equipped between the interior circulation guide shell 10 and crystallisation chamber 2.
Material is conveyed using transfering material pump between each vacuum shwoot crystallizer, transfering material pump is centrifugal pump.
In the present embodiment, 3 discharge ports, the glucose of collection are equally spacedly provided on the side wall of the crystallisation chamber 2
The partial size approximate range of sour calcium crystallization are as follows:
(1) apart from first, ground discharge port: length and diameter is respectively 70-100 and 7-10 μm；
(2) apart from second, ground discharge port: length and diameter is respectively 40-70 and 4-7 μm；
(3) apart from ground third discharge port: length and diameter is respectively 20-50 and 2-5 μm.
First discharge port is the 1/3~2/5 of 2 side wall length of crystallisation chamber at a distance from 2 bottom end of crystallisation chamber.If the first discharge port
Too close apart from 2 base bleed mouth of crystallisation chamber, crystal grain is easily deposited near exhaust outlet, blocks exhaust outlet；If the first discharge port distance
Too far, the collection rate of major diameter crystal grain declines 2 bottom of crystallisation chamber, and crystalline rate reduces.
Embodiment 5:
A kind of system of calcium gluconate continuous crystallisation, comprising: MVR evaporator 1., the vacuum shwoot knot of multi-stage embodiment 1
Brilliant device 3., 6., 9., the MVR evaporator 1., multi-stage vacuum shwoot crystallizer 3., 6., 9., slurry tankCentrifuge successively phase
Even, 1. the centrifuge is also connected with MVR evaporator, and 3., 6., 9. top is provided with steam to each vacuum shwoot crystallizer
4., 7., 10., 4., 7., 10. the vapor jet vacuum pump is all connected with condenser ejector vacuum pump.
It needs feed liquid to heat before vacuum shwoot decrease temperature crystalline and is concentrated into certain temperature and concentration, currently used hand
Section is steam heating, the advantages of 1. evaporation and concentration using MVR evaporator:
(1) MVR energy conservation evaporation technique is current international advanced evaporation technique, and energy utilization rate is high, greatly reduces enterprise
Industry operating cost, reduces environmental pollution.
(2) device goes out and needs when starting using except external steam, and when running well, evaporator itself is not needed again
Using external steam source, cooling water and related condensing plant are not needed yet.
(3) it is compared due to providing heat source using compressor with conventional evaporator, the temperature difference is much smaller, can reach mild steaming
Hair greatlys improve product quality, reduces fouling.
(4) it is not necessarily to condenser, structure is very simple with process, full automatic working, continuously-running, securely and reliably.
(5) the evaporator material is in low temperature and do not generate foam in the state of is evaporated, and feed liquid is uniform, does not run material, no
Easy coking.
Embodiment 6:
A kind of system of calcium gluconate continuous crystallisation, comprising: MVR evaporator 1., the vacuum shwoot knot of multi-stage embodiment 1
Brilliant device 3., 6., 9., the MVR evaporator 1., multi-stage vacuum shwoot crystallizer 3., 6., 9., slurry tankCentrifuge successively phase
Even, 1. the centrifuge is also connected with MVR evaporator, and 3., 6., 9. top is provided with steam to each vacuum shwoot crystallizer
4., 7., 10., 4., 7., 10. the vapor jet vacuum pump is all connected with condenser ejector vacuum pump.
3., 6., 9. the material of the MVR evaporator 1. is transported to multi-stage vacuum shwoot crystallizer by transfering material pump.
Embodiment 7:
A kind of system of calcium gluconate continuous crystallisation, comprising: MVR evaporator 1., the vacuum shwoot knot of multi-stage embodiment 1
Brilliant device 3., 6., 9., the MVR evaporator 1., multi-stage vacuum shwoot crystallizer 3., 6., 9., slurry tankCentrifuge successively phase
Even, 1. the centrifuge is also connected with MVR evaporator, and 3., 6., 9. top is provided with steam to each vacuum shwoot crystallizer
4., 7., 10., 4., 7., 10. the vapor jet vacuum pump is all connected with condenser ejector vacuum pump.
3., 6., 9. the material of the MVR evaporator 1. is transported to multi-stage vacuum shwoot crystallizer by transfering material pump.
The vacuum shwoot crystallizer 3., 6., be 9. divided into three-level, first order vacuum shwoot temperature is 75~85 DEG C, relatively
Vacuum degree is -0.03MPa~-0.05MPa；Second level vacuum shwoot temperature is 60~75 DEG C, and relative degree of vacuum is -0.05MPa
~-0.07MPa；Third level vacuum shwoot temperature is 45~60 DEG C, and relative degree of vacuum is -0.07MPa~-0.09MPa.
Embodiment 8:
A kind of system of calcium gluconate continuous crystallisation, comprising: MVR evaporator 1., the vacuum shwoot knot of multi-stage embodiment 1
Brilliant device 3., 6., 9., the MVR evaporator 1., multi-stage vacuum shwoot crystallizer 3., 6., 9., slurry tankCentrifuge successively phase
Even, 1. the centrifuge is also connected with MVR evaporator, and 3., 6., 9. top is provided with steam to each vacuum shwoot crystallizer
4., 7., 10., 4., 7., 10. the vapor jet vacuum pump is all connected with condenser ejector vacuum pump.
3., 6., 9. the material of the MVR evaporator 1. is transported to multi-stage vacuum shwoot crystallizer by transfering material pump.
The vacuum shwoot crystallizer 3., 6., be 9. divided into three-level, first order vacuum shwoot temperature is 75~85 DEG C, relatively
Vacuum degree is -0.03MPa~-0.05MPa；Second level vacuum shwoot temperature is 60~75 DEG C, and relative degree of vacuum is -0.05MPa
~-0.07MPa；Third level vacuum shwoot temperature is 45~60 DEG C, and relative degree of vacuum is -0.07MPa~-0.09MPa.
Return to cooling tower in the cooling water return water of the condenser, it is uncooled under secondary steam taken away by vacuum pump.
Embodiment 9:
A kind of system of calcium gluconate continuous crystallisation, comprising: MVR evaporator 1., the vacuum shwoot knot of multi-stage embodiment 1
Brilliant device 3., 6., 9., the MVR evaporator 1., multi-stage vacuum shwoot crystallizer 3., 6., 9., slurry tankCentrifuge successively phase
Even, 1. the centrifuge is also connected with MVR evaporator, and 3., 6., 9. top is provided with steam to each vacuum shwoot crystallizer
4., 7., 10., 4., 7., 10. the vapor jet vacuum pump is all connected with condenser ejector vacuum pump.
3., 6., 9. the material of the MVR evaporator 1. is transported to multi-stage vacuum shwoot crystallizer by transfering material pump.
The vacuum shwoot crystallizer 3., 6., be 9. divided into three-level, first order vacuum shwoot temperature is 75~85 DEG C, relatively
Vacuum degree is -0.03MPa~-0.05MPa；Second level vacuum shwoot temperature is 60~75 DEG C, and relative degree of vacuum is -0.05MPa
~-0.07MPa；Third level vacuum shwoot temperature is 45~60 DEG C, and relative degree of vacuum is -0.07MPa~-0.09MPa.
Return to cooling tower in the cooling water return water of the condenser, it is uncooled under secondary steam taken away by vacuum pump.
The centrifuge is also successively connected with pelletizer, ebullated bed.
Finally it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not limited to this hair
It is bright, although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still
It can modify to technical solution documented by previous embodiment, or part is equivalently replaced.It is all in this hair
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on should be included in protection scope of the present invention
Within.Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not to the scope of the present invention
Limitation, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not required to
Make the creative labor the various modifications or changes that can be made still within protection scope of the present invention.
Claims (10)
1. a kind of calcium gluconate continuous crystallisation vacuum shwoot crystallizer characterized by comprising vaporization chamber and crystallisation chamber,
The vaporization chamber is located at the top of crystallisation chamber, is provided with spray equipment and exhaust outlet at the top of vaporization chamber；The vaporization chamber is straight tube
Shape, the crystallisation chamber are pyramidal structure；The crystallisation chamber is provided with interior circulation guide shell, and the side wall of the crystallisation chamber is provided with more
A inlet port and outlet port；The bottom of the crystallisation chamber also sets up exhaust outlet, and the crystallisation chamber bottom is connected with forced circulation pump,
It is connected at the top of the vaporization chamber with vapor jet vacuum pump.
2. vacuum shwoot crystallizer as described in claim 1, which is characterized in that between interior circulation guide shell and the crystallisation chamber
Equipped with support tube.
3. vacuum shwoot crystallizer as described in claim 1, which is characterized in that using a turn material between each vacuum shwoot crystallizer
Pump conveying material, transfering material pump is centrifugal pump.
4. vacuum shwoot crystallizer as described in claim 1, which is characterized in that in the crystallizer, direct tube section and centrum section
Ratio is 1~3:1~2.
5. vacuum shwoot crystallizer as described in claim 1, which is characterized in that equally spacedly set on the side wall of the crystallisation chamber
It is equipped with 3 discharge ports, wherein the first discharge port is the 1/3~2/5 of crystallisation chamber side wall length at a distance from crystallisation chamber bottom end.
6. a kind of system of calcium gluconate continuous crystallisation characterized by comprising MVR evaporator, multistage claim 1-5
Described in any item vacuum shwoot crystallizers, the MVR evaporator, multi-stage vacuum shwoot crystallizer, slurry tank, centrifuge are successively
It is connected, the centrifuge is also connected with MVR evaporator, vapor jet vacuum pump is provided at the top of the vacuum shwoot crystallizer,
The vapor jet vacuum pump is connected with condenser.
7. system as claimed in claim 6, which is characterized in that the vacuum shwoot crystallizer is divided into three-level, first order vacuum
Shwoot temperature is 75~85 DEG C, and relative degree of vacuum is -0.03MPa~-0.05MPa；Second level vacuum shwoot temperature is 60~75
DEG C, relative degree of vacuum is -0.05MPa~-0.07MPa；Third level vacuum shwoot temperature be 45~60 DEG C, relative degree of vacuum be-
0.07MPa~-0.09MPa.
8. system as claimed in claim 6, which is characterized in that return to cooling tower in the cooling water return water of the condenser, not
Secondary steam under condensation is taken away by vacuum pump.
9. a kind of method of calcium gluconate continuous crystallisation characterized by comprising
1) it is 50-52% that calcium gluconate supernatant, which is introduced into MVR evaporator and is concentrated into material concentration, and secondary steam is by top
Discharge enters heat exchanger after compressor compresses and condenses, and is sucked by circulating pump, enters back into heating tube, continues cycling through；
2) MVR slurries are sequentially sent to three-level vacuum shwoot crystallizer by pipeline；
3) calcium gluconate slurries are expelled to slurry tank from No. three vacuum shwoot crystallizers, into being centrifugated to obtain calcium gluconate
Crystallized stock, clear liquid are back to the evaporation of MVR evaporator, the calcium gluconate crystallized stock that centrifuge is thrown away after heat exchanger preheats
Enter granulator after cleaning impurity with pure water, boiled bed drying obtains calcium gluconate finished product.
10. method as claimed in claim 9, which is characterized in that the pressure for the life steam that the vacuum shwoot crystallizer uses
For 0.6-1.0Mpa.
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| CN110478937A (en) * | 2019-08-21 | 2019-11-22 | 西安航天源动力工程有限公司 | A kind of crystallizer and crystal system |
| CN110559680A (en) * | 2019-07-11 | 2019-12-13 | 山东省科学院能源研究所 | Device and method for vacuum flash continuous crystallization of calcium gluconate and application of device |
| CN113184907A (en) * | 2021-05-31 | 2021-07-30 | 河钢承德钒钛新材料有限公司 | Method for purifying sodium chromate |
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