CN106866367A - A kind of continuous oscillation drift tube type crystallisation by cooling method of antierythrite - Google Patents
A kind of continuous oscillation drift tube type crystallisation by cooling method of antierythrite Download PDFInfo
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- CN106866367A CN106866367A CN201710247545.6A CN201710247545A CN106866367A CN 106866367 A CN106866367 A CN 106866367A CN 201710247545 A CN201710247545 A CN 201710247545A CN 106866367 A CN106866367 A CN 106866367A
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- tube
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- tube side
- extension type
- shell
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 38
- UNXHWFMMPAWVPI-UHFFFAOYSA-N Erythritol Natural products OCC(O)C(O)CO UNXHWFMMPAWVPI-UHFFFAOYSA-N 0.000 title claims abstract description 29
- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 title claims abstract description 29
- 230000010355 oscillation Effects 0.000 title claims abstract description 13
- 238000001816 cooling Methods 0.000 title claims abstract description 11
- 230000008025 crystallization Effects 0.000 claims abstract description 27
- 239000004386 Erythritol Substances 0.000 claims abstract description 13
- 229940009714 erythritol Drugs 0.000 claims abstract description 13
- 235000019414 erythritol Nutrition 0.000 claims abstract description 13
- 239000010413 mother solution Substances 0.000 claims abstract description 12
- 239000012452 mother liquor Substances 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 230000008676 import Effects 0.000 claims description 27
- 238000004891 communication Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000000498 cooling water Substances 0.000 claims description 3
- 239000012043 crude product Substances 0.000 claims description 3
- 238000006073 displacement reaction Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000004888 barrier function Effects 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract description 2
- 230000014759 maintenance of location Effects 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 230000002085 persistent effect Effects 0.000 abstract description 2
- 239000000725 suspension Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 7
- 238000002156 mixing Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- YTBSYETUWUMLBZ-UHFFFAOYSA-N D-Erythrose Natural products OCC(O)C(O)C=O YTBSYETUWUMLBZ-UHFFFAOYSA-N 0.000 description 1
- YTBSYETUWUMLBZ-IUYQGCFVSA-N D-erythrose Chemical compound OC[C@@H](O)[C@@H](O)C=O YTBSYETUWUMLBZ-IUYQGCFVSA-N 0.000 description 1
- 206010056474 Erythrosis Diseases 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 206010018473 Glycosuria Diseases 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 235000020510 functional beverage Nutrition 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000010900 secondary nucleation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0081—Use of vibrations, e.g. ultrasound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of continuous oscillation drift tube type crystallisation by cooling method of antierythrite, its technical scheme is：By in the extension type crystallizer of erythritol crystallization mother liquor feeding plural serial stage, and along the central axial setting circular baffle plate in each sleeve pipe, by circular baffle plate along the interior central axial reciprocating vibration of pipe, significantly improve the flow of fluid and microcosmic admixture of continuous extension type crystallizer near-wall, the crystal particles even suspension in crystalline mother solution can also be made, even if also can almost reach horizontal sliding flow pattern RTD (residence time destribution) at low flow rates, efficiently solve the intrinsic persistent ailment of restriction conventional tubular continuous crystalizer commercial Application, as wall easily deposits/separate out the brilliant dirt of Crystallization so as to significantly reduce heat transfer efficiency, radial temperature concentration gradient is larger caused by tube wall retention layer is thicker under low shear rate, local degree of supersaturation is higher to wait technical barrier.The present invention also has the advantages that continuous prodution, can effectively reduce antierythrite crystallization production cost.
Description
Technical field
The invention belongs to multi-sugar alcohol production technical field, and in particular to a kind of continuous oscillation drift tube type of antierythrite is cold
But method for crystallising.
Background technology
Antierythrite is a kind of natural saccharic and Functional sweetening agents, is widely used in developing health food low in calories, glycosuria
The functional food or beverage, children special-purpose of disease and the crowd such as glucose uncomfortable diseases clean the teeth articles for use etc., and market prospects are very good.
The production technology of antierythrite mainly has chemical synthesis and fermentation method, is finally both needed to using Crystallization Separation technology,
Antierythrite product could be obtained.At present, the crystallization processes of antierythrite production are mainly periodic crystallisation operation, and such as evaporation is tied
Brilliant, crystallisation by cooling and dilution crystallization.Compared to batch crystallization process, continuous crystallisation is steady state operation, with running cost it is low,
Utilization rate of equipment and installations is high, production capacity is big, high degree of automation the advantages of.And, state Behavior of Continuous Crystallization Processes product quality stabilization can
It is prevented effectively from the differences between batches phenomenon of batch crystallization process product quality.Additionally, continuous crystallisation also have procedure parameter it is easy to control,
It is more easy to realize the advantages of industry is amplified.
At present, the Continuous Cooling Crystallization equipment of main flow is broadly divided into two major classes：Mix suspending mixing discharging crystallizer
And tube type mold (MSMPR).Although MSMPR crystallizers because its simple structure, manipulate it is convenient the advantages of in current continuous knot
It is widely used in brilliant process (no matter laboratory, or commercial scale), but there is also following deficiency：Bad microcosmic mixing causes
Localised high shear region and local supersaturation are serious (secondary nucleation, crystal fracture etc.)；Contain solids on tinuous production
The conveying of material；The drawback such as non-linear of industrial amplification process.
And tube type mold is when being applied to Continuous Cooling Crystallization process, because the temperature difference is larger at heat exchange tube wall, crystal is easily in pipe
The phenomenon that wall deposition is separated out is very serious, or even the phenomenon for blocking tube type mold occurs.
The content of the invention
It is contemplated that overcoming prior art defect, it is therefore an objective to provide a kind of continuous oscillation drift tube type cooling of antierythrite
Method for crystallising, can effectively solve easily to deposit the phenomenon for separating out crystal at continuous pipe type cooler crystallizer tube wall.
To achieve the above object, the technical solution adopted by the present invention is comprised the concrete steps that：
Step one, under conditions of 10~80 DEG C and 100~500r/min of rotating speed, antierythrite crude product and water are hybridly prepared into
Concentration is the erythritol crystallization mother liquor of 50 ~ 80wt%；
Step 2, the erythritol crystallization mother liquor that will be configured in step one send into tube type mold group after filtering off solid insoluble,
The tube type mold group is made up of the extension type crystallizer of plural serial stage, and series connection series n is the natural number more than 1；The set
Tube type mold is provided with tube side import, tube side outlet, shell side import and shell-side outlet, in formation in each extension type crystallizer
There are mutually isolated tube side passage and shell side passage, described tube side passage and tube side import and tube side outlet；Described
Shell side passage is connected with shell side import with shell-side outlet；
Described sleeve pipe formula crystallizer piece damper rod of central axial setting along pipe, from damper rod near extension type crystallizer tube side
One end of import starts, and circular baffle plate is set evenly and at intervals, and damper rod passes perpendicularly through the round center of each circular baffle plate, baffle plate
Bar is connected by plunger near one end of extension type crystallizer tube side outlet with plunger displacement pump, damper rod is crystallized along bushing type
Central axial reciprocating vibration in device pipe, its frequency of oscillation is 1 ~ 10Hz, and amplitude is 1 ~ 5cm；
The diameter of the circular baffle plate is 0.3 ~ 0.8 times of extension type crystallizer tube side diameter, two neighboring on every damper rod
The spacing of circular baffle plate is 1.0 ~ 10 times of extension type crystallizer tube side diameter；
The length of described damper rod is 0.6 ~ 0.8 times of extension type crystallizer tube side length；
With the sequence of flow of crystalline mother solution as reference, in the tube type mold group of described plural serial stage, the 1st bushing type crystallization
With the tube side import of subsequent casings formula crystallizer by pipeline communication, crystalline mother solution is by the 1st bushing type knot for the tube side outlet of device
The tube side import of brilliant device is added, and is flowed continually out by the tube side outlet of last extension type crystallizer after being gradually cooled as it passes through the cooler, and is sent to
Filter, wash, dry, obtain erythritol crystal product；
With the sequence of flow of crystalline mother solution as reference, in the tube type mold group of described plural serial stage, the 1st bushing type crystallization
With the shell-side outlet of subsequent casings formula crystallizer by pipeline communication, cooling water is by last bushing type knot for the shell side import of device
The shell side import of brilliant device enters, and cools down step by step after each extension type crystallizer of series connection by the 1st shell of extension type crystallizer
Journey outlet outflow；
Last described extension type crystallizer tube side outlet temperature is 10 ~ 25 DEG C, and erythritol crystallization mother liquor is whole
Accumulative mean residence time in tube type mold group is 10 ~ 60min.
There is following good effect compared with prior art due to using above-mentioned technical proposal, the present invention：
(1) the continuous oscillation drift tube type crystallisation by cooling method of antierythrite involved in the present invention, in extension type crystallizer along pipe
The interior central axial flow of fluid for being provided with baffle plate, and extension type crystallizer tube wall surface being effectively improved by the vibration of baffle plate
With microcosmic admixture, the technical disadvantages of MSMPR crystallizers are not only effectively overcome, also efficiently solve restriction conventional tubular and connect
The intrinsic persistent ailment of continuous crystallizer commercial Application, such as wall easily deposit/separate out the brilliant dirt of Crystallization so as to significantly reduce heat transfer effect
Rate, radial temperature-concentration gradient is larger caused by tube wall retention layer is thicker under low shear rate, local degree of supersaturation is higher etc.
Technical barrier.
(2) the continuous oscillation drift tube type crystallisation by cooling method of antierythrite involved in the present invention, the vibration of baffle plate is effective
Enhance mixing, the Mass and heat transfer in double-pipe chiller so that extension type crystallizer can remain at low flow rates realize radially,
The good mixing of axial direction and the advantages of the crystal particles even suspension in crystalline mother solution can be made.Also, by baffle plate oscillation frequency
Rate can accurately regulate and control the mixing intensity in extension type crystallizer with amplitude, even if also can almost reach horizontal sliding at low flow rates
Flow pattern RTD (residence time destribution).
Brief description of the drawings
Fig. 1 is schematic diagram of the present invention.
Specific embodiment
With reference to specific embodiment, the invention will be further described, not to the limitation of its protection domain.
Embodiment 1
As shown in figure 1, the continuous oscillation drift tube type crystallisation by cooling method of antierythrite involved in the present invention, it is characterised in that
Specifically complete according to the following steps：
Step one, under conditions of 40~80 DEG C and 100~500r/min of rotating speed, by erythrose in the crystalline mother solution storage tank (1)
Alcohol crude product is hybridly prepared into the erythritol crystallization mother liquor that concentration is 50 ~ 80wt% with water；
Step 2, the erythritol crystallization mother liquor that will be configured in step one send into tubular type knot after filtering off solid insoluble with pump (2)
Brilliant device group, the tube type mold group is made up of the extension type crystallizer (3) of plural serial stage, series connection series n=4；The tubular type knot
Brilliant device group is made up of the extension type crystallizer (3) of plural serial stage, series connection series n=4；Described sleeve pipe formula crystallizer (3) is provided with pipe
Journey import (31), tube side outlet (32), shell side import (33) and shell-side outlet (34), in each extension type crystallizer (3) interior shape
Into there is mutually isolated tube side passage and shell side passage, described tube side passage is with tube side import (31) and tube side outlet (32) even
It is logical；Described shell side passage is connected with shell side import (33) with shell-side outlet (34)；
Described sleeve pipe formula crystallizer (3) piece damper rod of central axial setting along pipe, from damper rod near extension type crystallizer
(3) one end of tube side import (31) starts, and circular baffle plate is set evenly and at intervals, and damper rod passes perpendicularly through each circular baffle plate
Circle center, damper rod is connected with plunger displacement pump (4) by plunger near one end of extension type crystallizer (3) tube side outlet (32), made
Damper rod can be along central axial reciprocating vibration in extension type crystallizer pipe, and its frequency of oscillation is 1 ~ 10Hz, and amplitude is 1 ~ 5cm；
The diameter of the circular baffle plate is 0.6 times of extension type crystallizer (3) tube side diameter, two neighboring circle on every damper rod
The spacing of shape baffle plate is 5 times of extension type crystallizer (3) tube side diameter；
The length of described damper rod is 0.6 ~ 0.8 times of extension type crystallizer (3) tube side length；
With the sequence of flow of crystalline mother solution as reference, in the tube type mold group of described plural serial stage, the 1st bushing type crystallization
The tube side import (31) of tube side outlet (32) and subsequent casings formula crystallizer (3) of device (3) by pipeline communication, crystalline mother solution by
The 1st tube side import (31) of extension type crystallizer (3) is added by pump (2), is crystallized by the 4th bushing type after being gradually cooled as it passes through the cooler
Tube side outlet (32) of device (3) is flowed continually out, and is sent to filtering, washing, is dried, and obtains erythritol crystal product；
With the sequence of flow of crystalline mother solution as reference, in the tube type mold group of described plural serial stage, the 1st bushing type crystallization
By pipeline communication, cooling water is by for the shell side import (33) of device (3) and the shell-side outlet (34) of subsequent casings formula crystallizer (3)
The shell side imports (33) of 4 extension type crystallizers (3) enter, cool down step by step after each extension type crystallizer (3) of series connection by
1st shell-side outlet (34) outflow of extension type crystallizer (3).
The 4th described extension type crystallizer tube side outlet temperature is 20 DEG C, and erythritol crystallization mother liquor is entirely managed
Accumulative mean residence time in formula crystallizer group is 30 ~ 60min.
Claims (1)
1. a kind of continuous oscillation drift tube type crystallisation by cooling method of antierythrite, it is characterised in that specifically complete according to the following steps：
Step one, under conditions of 10~80 DEG C and 100~500r/min of rotating speed, antierythrite crude product and water are hybridly prepared into
Concentration is the erythritol crystallization mother liquor of 50 ~ 80wt%；
Step 2, the erythritol crystallization mother liquor that will be configured in step one send into tube type mold group after filtering off solid insoluble,
The tube type mold group is made up of the extension type crystallizer of plural serial stage, and series connection series n is the natural number more than 1；The set
Tube type mold is provided with tube side import, tube side outlet, shell side import and shell-side outlet, in formation in each extension type crystallizer
There are mutually isolated tube side passage and shell side passage, described tube side passage and tube side import and tube side outlet；Described
Shell side passage is connected with shell side import with shell-side outlet；
Described sleeve pipe formula crystallizer piece damper rod of central axial setting along pipe, from damper rod near extension type crystallizer tube side
One end of import starts, and circular baffle plate is set evenly and at intervals, and damper rod passes perpendicularly through the round center of each circular baffle plate, baffle plate
Bar is connected by plunger near one end of extension type crystallizer tube side outlet with plunger displacement pump, damper rod is crystallized along bushing type
Central axial reciprocating vibration in device pipe, its frequency of oscillation is 1 ~ 10Hz, and amplitude is 1 ~ 5cm；
The diameter of the circular baffle plate is 0.3 ~ 0.8 times of extension type crystallizer tube side diameter, two neighboring on every damper rod
The spacing of circular baffle plate is 1.0 ~ 10 times of extension type crystallizer tube side diameter；
The length of described damper rod is 0.6 ~ 0.8 times of extension type crystallizer tube side length；
With the sequence of flow of crystalline mother solution as reference, in the tube type mold group of described plural serial stage, the 1st bushing type crystallization
With the tube side import of subsequent casings formula crystallizer by pipeline communication, crystalline mother solution is by the 1st bushing type knot for the tube side outlet of device
The tube side import of brilliant device is added, and is flowed continually out by the tube side outlet of last extension type crystallizer after being gradually cooled as it passes through the cooler, and is sent to
Filter, wash, dry, obtain erythritol crystal product；
With the sequence of flow of crystalline mother solution as reference, in the tube type mold group of described plural serial stage, the 1st bushing type crystallization
With the shell-side outlet of subsequent casings formula crystallizer by pipeline communication, cooling water is by last bushing type knot for the shell side import of device
The shell side import of brilliant device enters, and cools down step by step after each extension type crystallizer of series connection by the 1st shell of extension type crystallizer
Journey outlet outflow；
Last described extension type crystallizer tube side outlet temperature is 10 ~ 25 DEG C, and erythritol crystallization mother liquor is whole
Accumulative mean residence time in tube type mold group is 10 ~ 60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710247545.6A CN106866367A (en) | 2017-04-17 | 2017-04-17 | A kind of continuous oscillation drift tube type crystallisation by cooling method of antierythrite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710247545.6A CN106866367A (en) | 2017-04-17 | 2017-04-17 | A kind of continuous oscillation drift tube type crystallisation by cooling method of antierythrite |
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| Publication Number | Publication Date |
|---|---|
| CN106866367A true CN106866367A (en) | 2017-06-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710247545.6A Pending CN106866367A (en) | 2017-04-17 | 2017-04-17 | A kind of continuous oscillation drift tube type crystallisation by cooling method of antierythrite |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109806615A (en) * | 2019-03-15 | 2019-05-28 | 武汉科技大学 | A kind of continuous bushing type method for crystallising of muitishell |
| CN112479820A (en) * | 2020-11-16 | 2021-03-12 | 江苏汉光生物工程有限公司 | Erythritol's continuous oscillation flowing film crystallization device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101312783A (en) * | 2005-11-22 | 2008-11-26 | 倪泰克解决方案有限公司 | Improved apparatus and method for temperature controlled processes |
| GB2458694A (en) * | 2008-03-28 | 2009-09-30 | Desmet Ballestra Engineering S | Crystallisation of edible oils and fats |
| CN101967114A (en) * | 2010-08-27 | 2011-02-09 | 浙江工程设计有限公司 | Continuous production method and continuous production device for synthesizing biruea |
| CN105641967A (en) * | 2016-04-01 | 2016-06-08 | 武汉科技大学 | Method for continuously crystallizing erythritol |
| CN105861570A (en) * | 2016-04-19 | 2016-08-17 | 齐鲁工业大学 | Preparation method of odorless erythritol |
-
2017
- 2017-04-17 CN CN201710247545.6A patent/CN106866367A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101312783A (en) * | 2005-11-22 | 2008-11-26 | 倪泰克解决方案有限公司 | Improved apparatus and method for temperature controlled processes |
| GB2458694A (en) * | 2008-03-28 | 2009-09-30 | Desmet Ballestra Engineering S | Crystallisation of edible oils and fats |
| CN101967114A (en) * | 2010-08-27 | 2011-02-09 | 浙江工程设计有限公司 | Continuous production method and continuous production device for synthesizing biruea |
| CN105641967A (en) * | 2016-04-01 | 2016-06-08 | 武汉科技大学 | Method for continuously crystallizing erythritol |
| CN105861570A (en) * | 2016-04-19 | 2016-08-17 | 齐鲁工业大学 | Preparation method of odorless erythritol |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109806615A (en) * | 2019-03-15 | 2019-05-28 | 武汉科技大学 | A kind of continuous bushing type method for crystallising of muitishell |
| CN112479820A (en) * | 2020-11-16 | 2021-03-12 | 江苏汉光生物工程有限公司 | Erythritol's continuous oscillation flowing film crystallization device |
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Application publication date: 20170620 |
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