CN106831337A - A kind of method of the continuous dissolved membrane crystallization of antierythrite - Google Patents
A kind of method of the continuous dissolved membrane crystallization of antierythrite Download PDFInfo
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- CN106831337A CN106831337A CN201710247553.0A CN201710247553A CN106831337A CN 106831337 A CN106831337 A CN 106831337A CN 201710247553 A CN201710247553 A CN 201710247553A CN 106831337 A CN106831337 A CN 106831337A
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- Prior art keywords
- dissolved
- membrane
- antierythrite
- dissolved agent
- crystallization
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- 239000012528 membrane Substances 0.000 title claims abstract description 61
- UNXHWFMMPAWVPI-UHFFFAOYSA-N Erythritol Natural products OCC(O)C(O)CO UNXHWFMMPAWVPI-UHFFFAOYSA-N 0.000 title claims abstract description 39
- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 title claims abstract description 39
- 238000002425 crystallisation Methods 0.000 title claims abstract description 30
- 230000008025 crystallization Effects 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 50
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000004821 distillation Methods 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 14
- 230000008020 evaporation Effects 0.000 claims abstract description 13
- 239000010413 mother solution Substances 0.000 claims abstract description 13
- 239000004386 Erythritol Substances 0.000 claims abstract description 11
- 229940009714 erythritol Drugs 0.000 claims abstract description 11
- 235000019414 erythritol Nutrition 0.000 claims abstract description 11
- 239000002699 waste material Substances 0.000 claims abstract description 10
- 230000008929 regeneration Effects 0.000 claims abstract description 8
- 238000011069 regeneration method Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000012452 mother liquor Substances 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 230000008676 import Effects 0.000 claims description 13
- 239000012530 fluid Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000012043 crude product Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 abstract description 5
- 239000012895 dilution Substances 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 206010054949 Metaplasia Diseases 0.000 abstract description 2
- 230000015689 metaplastic ossification Effects 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000004134 energy conservation Methods 0.000 abstract 1
- 230000002209 hydrophobic effect Effects 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 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
- 241001515806 Stictis Species 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 230000004907 flux 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
- 238000009776 industrial production Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000010900 secondary nucleation Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000003765 sweetening agent Substances 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
-
- 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
-
- 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
Abstract
The present invention relates to a kind of method of the continuous dissolved membrane crystallization of antierythrite.Its technical scheme is：Erythritol crystallization mother liquor is sent into hydrophobic hollow tubular membrane component tube side passage, dissolved agent is added from membrane module shell side passage, dissolved agent is entered into crystalline mother solution by evaporation alcohol permselective membrane, make crystalline mother solution gradually supersaturated and separate out crystal, leave the magma filtering of membrane module tube side passage, washing and be drying to obtain erythritol crystal product, and the liquid of filtrate, washings and membrane module shell side outflow sends into atmospheric distillation tower together, the regeneration dissolved agent feeding membrane module shell side channel cycle of rectifying column tower top is used.The Total continuity metaplasia that the present invention realizes antierythrite dilution crystallization process is produced, effectively prevent the part supersaturation high and excessive nucleation existed when dissolved agent is directly added into crystalline mother solution, and dissolved agent can reclaim to realize recycling, have the advantages that to reduce production cost, reduce " three wastes " discharge, energy-conservation.
Description
Technical field
The invention belongs to multi-sugar alcohol production technical field, and in particular to a kind of side of the continuous dissolved membrane crystallization of antierythrite
Method.
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.
Antierythrite industrial production mainly uses fermentation method, is first concentrated by evaporation after the purified treatment of zymotic fluid, then cool down knot
The prepared erythritol crystal of crystalline substance.Because zymotic fluid mesoerythrit concentration is relatively low, operation temperature is higher when atmospheric evaporation is concentrated, water
Point evaporation capacity is larger, and energy consumption is higher；Though and use decompression or multiple-effect evaporation can be energy-saving, but equipment and technique can be increased
Complexity.
Zhang Chuntao etc. (CN 102992957A) discloses the dilution crystallization method of antierythrite, by antierythrite
Continuous stream solubilization analysis agent in saturated solution, and combine dissolved agent speed change feed-batch process and add crystal seed control crystallization, produce 30 ~ 60
The crystal of mesh or 40 ~ 80 mesh accounts for the erythritol crystal product of more than 90wt%.Although antierythrite dilution crystallization disclosed above
The method is said in method (CN 102992957A) more traditional antierythrite evaporative crystallization energy consumption low many, but stricti jurise
It is intermittently operated, and when dissolved agent is added directly into crystalline mother solution, it is very big in dissolved agent addition point part degree of supersaturation,
Secondary nucleation phenomenon is serious.Additionally, dissolved agent does not have in antierythrite dilution crystallization method (CN 102992957A) disclosed above
There is realization to reclaim circulation, dissolved agent consumption is larger.
Continuous crystallisation is the new focus of modern industry crystallization WeiLai Technology competition and industry protection, can not only improve product
Quality (elimination differences between batches), also has the advantages that to reduce production cost, reduces " three wastes " discharge and energy-saving, and its is important
Property and meaning are self-evident.
The content of the invention
It is contemplated that overcoming prior art defect, it is therefore an objective to provide a kind of side of the continuous dissolved membrane crystallization of antierythrite
Method.
To achieve the above object, the technical solution adopted by the present invention is comprised the concrete steps that：
Step one, under conditions of 25 ~ 40 DEG C and rotating speed are 200~500r/min, by the antierythrite crude product of 35 ~ 45wt% and
The water mixing of 55 ~ 65wt%, dissolving, are configured to erythritol crystallization mother liquor；
Step 2, the erythritol crystallization mother liquor that will be configured in step one send into the tube side import of hollow tubular membrane component, will walk
The regeneration dissolved agent of gained mixes with pure dissolved agent in rapid three, and its temperature control is then fed at 25 ~ 40 DEG C by heat exchanger
The shell side import of hollow tubular membrane component, dissolved agent progresses into the tube side of membrane module by evaporation alcohol permselective membrane,
Make crystalline mother solution gradually supersaturated and separate out crystal, separate out the magma after crystal by the continuous row of hollow tubular membrane component tube side outlet
Go out, the filtering of feeding filter, washing obtain erythritol crystal product after filtration cakes torrefaction, and filtrate, cleaning solution and leave film
The liquid of component shell-side outlet sends into mixing in blender together, obtains dissolved agent waste liquid；
Step 3, the distillate with atmospheric distillation tower tower reactor that the dissolved agent waste liquid of gained in step 2 is first exchange heat, and are re-fed into often
Pressure rectifying column, the namely regenerated dissolved agent of overhead of atmospheric distillation tower；
Tubular membrane in described hollow tubular membrane component is evaporation alcohol permselective membrane.
Described dissolved agent is the one kind in ethanol, propyl alcohol, isopropanol.
Dissolved agent concentration is 90 ~ 100wt% in the regeneration dissolved agent that described atmospheric distillation column overhead is distillated.
The fluid flow of the shell side import of described hollow tubular membrane component is the tube side import of hollow tubular membrane component
0.5 ~ 5 times of fluid flow.
Described filter is Full-automatic filter formula centrifuge, and charging, separation of solid and liquid, washing, discharging, discharge opeing are all automatic
It is continuously finished.
There is following good effect compared with prior art due to using above-mentioned technical proposal, the present invention：
(1) method of the continuous dissolved membrane crystallization of antierythrite involved in the present invention, realizes antierythrite dilution crystallization process
Total continuity metaplasia produce, and dissolved agent can reclaim with realize recycle, with reduce production cost, reduce " three wastes " row
The advantage put.
(2) method of the continuous dissolved membrane crystallization of antierythrite involved in the present invention, dissolved agent is preferential by infiltration evaporation
Alcohol permselective membrane is added in crystalline mother solution, and the permeation flux of general evaporation alcohol permselective membrane is about 0.1 ~ 0.5kg/m2H,
The fenestra on film surface is evenly distributed so that the dissolved agent addition that the present invention is protected is highly uniform, effectively prevent directly molten
Part supersaturation high and excessive nucleation that analysis agent exists when being added in crystalline mother solution so that the granularity of crystalline product
It is evenly distributed, average grain diameter is larger.
(3) method of the continuous dissolved membrane crystallization of antierythrite involved in the present invention, the magma solid-liquid by membrane module
Filtrate and cleaning solution feeding atmospheric distillation tower after separation reclaims dissolved agent, realizes the regeneration cycle of dissolved agent, and can root
According to the dissolved agent that the loss supplement of dissolved agent in produce reality is fresh, additionally, filtrate and cleaning solution are before rectifying column is entered,
Preheated using the used heat at rectifying tower bottom, can effectively be saved the energy consumption of rectifying column, therefore the present invention also has energy-saving and emission-reduction
Advantage.
Brief description of the drawings
Fig. 1 is schematic flow sheet 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
A kind of method of the continuous dissolved membrane crystallization of antierythrite, as shown in figure 1, specifically including crystalline mother solution tank (1), membrane module
(2), atmospheric distillation tower (3), filter (5), blender (6), heat exchanger (7), heat exchanger (8), dissolved agent storage tank (9),
Blender (10), between the crystalline mother solution tank (1) and membrane module (2) tube side import, dissolved agent storage tank (9) and blender (10)
Between, between atmospheric distillation tower (3) tower top and blender (10), atmospheric distillation tower (3) bottom of towe and heat exchanger (8) shell side inlet
Between, between filter (5) and blender (6), between blender (6) and heat exchanger (8) tube-side inlet respectively by set
Have pump (4) pipeline connect, between the blender (10) and heat exchanger (7) tube-side inlet, heat exchanger (7) tube side export
Between membrane module (2) shell side inlet, between membrane module (2) shell-side outlet and blender (6), membrane module (2) tube side outlet with
Between filter (5), the outlet of the tube side of heat exchanger (8) is connected by pipeline respectively between atmospheric distillation tower (3).
Specific implementation step of the invention is as follows：
Step one, under conditions of 25 ~ 40 DEG C and rotating speed are 200~500r/min, by 35 ~ 45wt% in crystalline mother solution tank (1)
Antierythrite crude product and 55 ~ 65wt% water mixing, dissolving, be configured to erythritol crystallization mother liquor；
Step 2, the erythritol crystallization mother liquor that will be configured in step one send into the tube side import of hollow tubular membrane component (2)；Will
The agent of regeneration dissolved and the pure dissolved agent of gained are sent into blender (10) and are mixed in step 3, by heat exchanger (7) by its temperature control
System is then fed into the shell side import of hollow tubular membrane component (2) at 25 ~ 40 DEG C, and dissolved agent passes through evaporation alcohol permselective membrane
The tube side of membrane module (2) is progressed into, is made crystalline mother solution gradually supersaturated and is separated out crystal, the magma after precipitation crystal is in
The empty continuous discharge of tubular membrane component (2) tube side outlet, feeding filter (5) filtering, washing obtain antierythrite after filtration cakes torrefaction
Crystal product, and filtrate, cleaning solution and leave the liquid of membrane module shell-side outlet and send into mixing in blender (6) together, obtain
To dissolved agent waste liquid；
Step 3, the distillate with atmospheric distillation tower (3) tower reactor that the dissolved agent waste liquid of gained in step 2 is first exchange heat, and are re-fed into
Atmospheric distillation tower (3), the namely regenerated dissolved agent of overhead of atmospheric distillation tower (3)；
Tubular membrane in described hollow tubular membrane component (2) is evaporation alcohol permselective membrane.
Described dissolved agent is ethanol.
Dissolved agent concentration is 90 ~ 95wt% in the regeneration dissolved agent that described atmospheric distillation tower (3) tower top is distillated.
The fluid flow of described hollow tubular membrane component (2) shell side import is hollow tubular membrane component (2) tube side import
0.5 ~ 5 times of fluid flow.
Described filter (5) is Full-automatic filter formula centrifuge, and charging, separation of solid and liquid, washing, discharging, discharge opeing are all
Automatically continuously complete.
The crystalline mother solution tank (1) is controllable temperature, the jacket reactor with stirring.
The heat exchanger (8) is tubular heat exchanger.
Claims (5)
1. the method for the continuous dissolved membrane crystallization of a kind of antierythrite, it is characterised in that specifically complete according to the following steps：
Step one, under conditions of 25 ~ 40 DEG C and rotating speed are 200~500r/min, by the antierythrite crude product of 35 ~ 45wt% and
The water mixing of 55 ~ 65wt%, dissolving, are configured to erythritol crystallization mother liquor；
Step 2, the erythritol crystallization mother liquor that will be configured in step one send into the tube side import of hollow tubular membrane component, will walk
The regeneration dissolved agent of gained mixes with pure dissolved agent in rapid three, and its temperature control is then fed at 25 ~ 40 DEG C by heat exchanger
The shell side import of hollow tubular membrane component, the dissolved agent in membrane module shell side passage is gradually entered by evaporation alcohol permselective membrane
Enter the tube side passage to membrane module, make the crystalline mother solution in tube side gradually supersaturated and separate out crystal, separate out the magma after crystal
By the continuous discharge of hollow tubular membrane component tube side outlet, the filtering of feeding filter, washing obtain antierythrite brilliant after filtration cakes torrefaction
Body product, and filtrate, cleaning solution and leave the liquid of membrane module shell-side outlet and send into mixing in blender together, obtain dissolved
Agent waste liquid；
Step 3, the distillate with atmospheric distillation tower tower reactor that the dissolved agent waste liquid of gained in step 2 is first exchange heat, after preheating
Dissolved agent waste liquid is re-fed into atmospheric distillation tower and reclaims dissolved agent, the namely regenerated dissolved agent of overhead of atmospheric distillation tower；
Tubular membrane in described hollow tubular membrane component is evaporation alcohol permselective membrane.
2. the method for the continuous dissolved membrane crystallization of antierythrite according to claim 1, it is characterised in that described dissolved agent
It is the one kind in ethanol, propyl alcohol, isopropanol.
3. the method for the continuous dissolved membrane crystallization of antierythrite according to claim 1, it is characterised in that described normal pressure essence
Dissolved agent concentration is 90 ~ 100wt% in evaporating the regeneration dissolved agent that column overhead is distillated.
4. the method for the continuous dissolved membrane crystallization of antierythrite according to claim 1, it is characterised in that described hollow tube
The fluid flow of the shell side import of formula membrane module is 0.5 ~ 5 times of the fluid flow of the tube side import of hollow tubular membrane component.
5. the method for the continuous dissolved membrane crystallization of antierythrite according to claim 1, it is characterised in that described filter
It is Full-automatic filter formula centrifuge, charging, separation of solid and liquid, washing, discharging, discharge opeing are all automatically continuously to complete.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710247553.0A CN106831337A (en) | 2017-04-17 | 2017-04-17 | A kind of method of the continuous dissolved membrane crystallization of antierythrite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710247553.0A CN106831337A (en) | 2017-04-17 | 2017-04-17 | A kind of method of the continuous dissolved membrane crystallization of antierythrite |
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| Publication Number | Publication Date |
|---|---|
| CN106831337A true CN106831337A (en) | 2017-06-13 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710247553.0A Pending CN106831337A (en) | 2017-04-17 | 2017-04-17 | A kind of method of the continuous dissolved membrane crystallization of antierythrite |
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| CN (1) | CN106831337A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912475A (en) * | 2020-07-08 | 2022-01-11 | 山东福洋生物科技股份有限公司 | Preparation method of erythritol crystals |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992957A (en) * | 2012-12-13 | 2013-03-27 | 武汉科技大学 | Solvent-out crystallization method of erythritol |
| CN103709008A (en) * | 2013-12-18 | 2014-04-09 | 武汉科技大学 | Method for separating and purifying erythritol by membrane crystallization |
| CN103709007A (en) * | 2013-12-18 | 2014-04-09 | 武汉科技大学 | Cooling coupling solvent-out crystallization refinement method of erythritol |
| CN105641967A (en) * | 2016-04-01 | 2016-06-08 | 武汉科技大学 | Method for continuously crystallizing erythritol |
| CN106178583A (en) * | 2016-09-20 | 2016-12-07 | 武汉科技大学 | The feedback of crystal product granularity during a kind of dilution crystallization |
-
2017
- 2017-04-17 CN CN201710247553.0A patent/CN106831337A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992957A (en) * | 2012-12-13 | 2013-03-27 | 武汉科技大学 | Solvent-out crystallization method of erythritol |
| CN103709008A (en) * | 2013-12-18 | 2014-04-09 | 武汉科技大学 | Method for separating and purifying erythritol by membrane crystallization |
| CN103709007A (en) * | 2013-12-18 | 2014-04-09 | 武汉科技大学 | Cooling coupling solvent-out crystallization refinement method of erythritol |
| CN105641967A (en) * | 2016-04-01 | 2016-06-08 | 武汉科技大学 | Method for continuously crystallizing erythritol |
| CN106178583A (en) * | 2016-09-20 | 2016-12-07 | 武汉科技大学 | The feedback of crystal product granularity during a kind of dilution crystallization |
Non-Patent Citations (1)
| Title |
|---|
| 欧雪娇;张春桃;李雪伟;王海蓉;: "膜结晶技术的研究进展" * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912475A (en) * | 2020-07-08 | 2022-01-11 | 山东福洋生物科技股份有限公司 | Preparation method of erythritol crystals |
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Application publication date: 20170613 |