CN107382817A - A kind of inexpensive epiphysin separation method - Google Patents
A kind of inexpensive epiphysin separation method Download PDFInfo
- Publication number
- CN107382817A CN107382817A CN201710715724.8A CN201710715724A CN107382817A CN 107382817 A CN107382817 A CN 107382817A CN 201710715724 A CN201710715724 A CN 201710715724A CN 107382817 A CN107382817 A CN 107382817A
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- Prior art keywords
- epiphysin
- inexpensive
- separation method
- walnut
- decolorization
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- 238000000926 separation method Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 22
- 238000004042 decolorization Methods 0.000 claims abstract description 13
- 241000758789 Juglans Species 0.000 claims description 18
- 235000009496 Juglans regia Nutrition 0.000 claims description 18
- 235000020234 walnut Nutrition 0.000 claims description 18
- 238000002386 leaching Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 7
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 6
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- 230000008014 freezing Effects 0.000 claims description 6
- 238000007710 freezing Methods 0.000 claims description 6
- 239000003456 ion exchange resin Substances 0.000 claims description 6
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 6
- 238000001223 reverse osmosis Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 229920000742 Cotton Polymers 0.000 claims description 3
- 238000005341 cation exchange Methods 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 3
- 239000001913 cellulose Substances 0.000 claims description 3
- 238000004132 cross linking Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 238000004880 explosion Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 3
- 150000003384 small molecules Chemical class 0.000 claims description 3
- BAZVSMNPJJMILC-UHFFFAOYSA-N triadimenol Chemical compound C1=NC=NN1C(C(O)C(C)(C)C)OC1=CC=C(Cl)C=C1 BAZVSMNPJJMILC-UHFFFAOYSA-N 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000009736 wetting Methods 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 6
- 230000006378 damage Effects 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 4
- 102000004190 Enzymes Human genes 0.000 abstract description 3
- 108090000790 Enzymes Proteins 0.000 abstract description 3
- 239000011149 active material Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000009466 transformation Effects 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 6
- 230000006870 function Effects 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 description 2
- YJPIGAIKUZMOQA-UHFFFAOYSA-N Melatonin Natural products COC1=CC=C2N(C(C)=O)C=C(CCN)C2=C1 YJPIGAIKUZMOQA-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- DRLFMBDRBRZALE-UHFFFAOYSA-N melatonin Chemical compound COC1=CC=C2NC=C(CCNC(C)=O)C2=C1 DRLFMBDRBRZALE-UHFFFAOYSA-N 0.000 description 2
- 229960003987 melatonin Drugs 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- 206010052804 Drug tolerance Diseases 0.000 description 1
- 241000124008 Mammalia Species 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 208000013738 Sleep Initiation and Maintenance disease Diseases 0.000 description 1
- 208000036142 Viral infection Diseases 0.000 description 1
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000003778 catagen phase Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000026781 habituation Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 206010022437 insomnia Diseases 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 210000002752 melanocyte Anatomy 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000003248 secreting effect Effects 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
- C07D209/04—Indoles; Hydrogenated indoles
- C07D209/10—Indoles; Hydrogenated indoles with substituted hydrocarbon radicals attached to carbon atoms of the hetero ring
- C07D209/14—Radicals substituted by nitrogen atoms, not forming part of a nitro radical
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Preparation And Processing Of Foods (AREA)
Abstract
The invention discloses a kind of inexpensive epiphysin separation method, comprise the following steps：Step 1: pretreatment；Step 2: crush；Step 3: leach；Step 4: film process；Step 5: decolorization；Step 6: revolving；Step 7: dry.The inexpensive epiphysin separation method of the present invention is pure physical process by film process process, and no phase transformation, energy consumption is low, and system operates at normal temperatures, overcomes destruction of the heat to active material in enzyme preparation product.Loss of effective components is reduced, reduces BOD and COD contents in waste water.Compared with traditional filtering, concentration technology method, new technology can significantly save inorganic salts, organic solvent in technical process, reduce the production cost of product.
Description
Technical field
The present invention relates to membrane technology field, particularly a kind of inexpensive epiphysin separation method.
Background technology
Epiphysin, also known as melatonin, U.S. drawing ketone is peaceful, presses down melanocyte, melatonin, is the pine by mammal and the mankind
A kind of amine bormones caused by fruit body, a kind of cell for producing melanin can be made shinny, thus be named as epiphysin.It is present
In numerous biologies such as from algae to the mankind, contents level is with daily time change.Research shows, human body epiphysin after the middle age
Secretion start to reduce, to old age, its secretory volume Yi Weibuzhong roads.Intake supplements enough epiphysins as early as possible, can improve interior
The function of excretory system, immunity is improved, improves anti-nervous, oxidation resistant function, improve sleep, reducing human aging speed,
Slow down sexual organ catagen speed has obvious help especially for habituation insomnia etc..
The existing process production time is grown, and a large amount of virose preservative addition flocculants are with the addition of in production, and flocculation is got off
Suspended impurity and activated carbon decolorizing absorb the product of part, yield is low；It is miscellaneous that the suspension such as flocculant is removed using plate compression
Matter, production environment is very poor, and production environment is extremely difficult to food additives production requirement；Intermediate ion is produced to exchange and macroreticular resin
It is a large amount of to use, expend substantial amounts of water resource and industrial chemicals resource, while it is difficult with life that a large amount of resins, which elute poisonous waste water,
Change is handled, and heavy financial burden and environmental protection pressure are brought to enterprise.
The content of the invention
It is pure physics by film process process it is an object of the invention to provide a kind of inexpensive epiphysin separation method
Process, no phase transformation, energy consumption is low, and system operates at normal temperatures, overcomes destruction of the heat to active material in enzyme preparation product.
A kind of inexpensive epiphysin separation method, comprises the following steps：
Step 1: pretreatment：Obtained walnut is subjected to liquid nitrogen frozen processing；
Step 2: crush：Crushed after walnut after freezing is added into leaching agent；
Step 3: leach：Walnut after crushing is extracted to the required composition leached in walnut repeatedly, obtains leachate；
Step 4: film process：Obtained leachate is handled by film, removes the salinity and small-molecule substance of centre；
Step 5: decolorization：Leachate after film process is subjected to decolorization, is put into resin column, carries out decolorization；
Step 6: revolving：Leachate after decolorization is put into Rotary Evaporators and carries out revolving processing, by leaching therein
Agent evaporates, and can be continuing with；
Step 7: dry：Obtained epiphysin is put into drying box and is dried, removes the leaching agent not eliminated.
The step 2, the walnut after freezing is crushed by wet pulverizing.
The step 3, leaching agent is used as by petroleum ether, the walnut after crushing is carried out to be put into ultrasonic unit progress
Leaching process, when being delivered to by ultrasonic vibration in liquid, cavitation effect is excited, so as to produce substantial amounts of cavitation gas in a liquid
Bubble, with the generation of these cavitation bubbles and explosion, microjet will be produced, enter to be about to the great solid particle of liquid and smash, simultaneously
Due to the vibration of ultrasonic wave, solid-liquid is more fully mixed, make clasmatosis, the extraction of cell inclusion is more perfectly sound.
The step 4, concentrating and separating processing is carried out by reverse osmosis membrane, use cotton, timber of containing cellulose etc. as original
Material, acetic acid, Triafol T are made through over-churning and hydrolysis（CA、CTA）, it is reprocessed into reverse osmosis membrane.
The step 5, handled by the ion exchange resin in resin column, ion exchange resin with styrene and
Divinylbenzene is the cross-linking products of skeleton, is porous spongy along with corresponding function group such as sulfonic group or quaternary ammonium
The skeleton of construction, there are a large amount of permanent micropores inside, then imports cation exchange groups and be made, and has micropore and big mesh, soaks
The aperture of resin is up to 100~500nm.
The step 7, processing is dried by vacuum drier.
The inexpensive epiphysin separation method of the present invention has the following advantages that：
The inexpensive epiphysin separation method includes, pre-processed, crushing, leaching, film process, decolorization, revolving, drying.
Solve in the prior art, it is difficult to use biochemical treatment that a large amount of resins, which elute poisonous waste water, brings heavy economy to bear to enterprise
Load and environmental protection pressure.The inexpensive epiphysin separation method of the present invention is pure physical process by film process process, no phase transformation,
Energy consumption is low, and system operates at normal temperatures, overcomes destruction of the heat to active material in enzyme preparation product.Reduce active ingredient damage
Lose, reduce BOD and COD contents in waste water.Compared with traditional filtering, concentration technology method, new technology can significantly save technique
During inorganic salts, organic solvent, reduce the production cost of product.
Brief description of the drawings
Technical scheme in order to illustrate the embodiments of the present invention more clearly, make required in being described below to embodiment
Accompanying drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for
For those of ordinary skill in the art, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Accompanying drawing 1 is the epiphysin separation method schematic flow sheet of embodiments of the invention low cost.
Specific embodiment
Below in conjunction with the accompanying drawing 1 of the present invention, technical scheme is clearly and completely described, it is clear that institute
The embodiment of description is only part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention,
The every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, belongs to this hair
The scope of bright protection.
As shown in figure 1, a kind of inexpensive epiphysin separation method, extraction process step include：
Step 1: pretreatment：Obtained walnut is subjected to liquid nitrogen frozen processing.
Step 2: crush：Crushed after walnut after freezing is added into leaching agent；By wet pulverizing by after freezing
Walnut is crushed.
Step 3: leach：Walnut after crushing is extracted to the required composition leached in walnut repeatedly, obtains leachate；It is logical
Petroleum ether is crossed as leaching agent, the walnut after crushing is carried out to be put into ultrasonic unit progress leaching process, passes through ultrasonic vibration
When being delivered in liquid, cavitation effect is excited, so as to produce substantial amounts of cavitation bubble in a liquid, as these cavitation bubbles produce
Raw and explosion, will produce microjet, enters to be about to the great solid particle of liquid and smash, simultaneously because the vibration of ultrasonic wave, makes solid
Liquid more fully mixes, and makes clasmatosis, and the extraction of cell inclusion is more perfectly sound.
Step 4: film process：Obtained leachate is handled by film, removes the salinity and small molecule thing of centre
Matter；Concentrating and separating processing is carried out by reverse osmosis membrane, cotton, timber of containing cellulose etc. are used as raw material, through over-churning and water
Acetic acid, Triafol T is made in solution reaction（CA、CTA）, it is reprocessed into reverse osmosis membrane.
Step 5: decolorization：Leachate after film process is subjected to decolorization, is put into resin column, is decolourized
Processing；Handled by the ion exchange resin in resin column, ion exchange resin is using styrene and divinylbenzene as skeleton
Cross-linking products, be the skeleton of mandruka columnar structure along with corresponding function group such as sulfonic group or quaternary ammonium, it is internal
There are a large amount of permanent micropores, then import cation exchange groups and be made, have a micropore and big mesh, the aperture of wetting resin is up to 100
~500nm.
Step 6: revolving：Leachate after decolorization is put into Rotary Evaporators and carries out revolving processing, will be therein
Leaching agent evaporates, and can be continuing with.
Step 7: dry：Obtained epiphysin is put into drying box and is dried, removes the leaching agent not eliminated.
Processing is dried by vacuum drier.
The present invention specifically shows and described the present invention with reference to preferred embodiment, it is clear that present invention specific implementation is not
Limited by aforesaid way, as long as the various unsubstantialities for employing inventive concept and technical scheme of the present invention progress improve,
Or it is not improved the design of invention and technical scheme are directly applied into other occasions, protection scope of the present invention it
It is interior.
Claims (6)
1. a kind of inexpensive epiphysin separation method, it is characterised in that specifically comprise the following steps：
Step 1: pretreatment：Walnut is subjected to liquid nitrogen frozen processing；
Step 2: crush：Crushed after walnut after freezing is added into leaching agent；
Step 3: leach：Walnut after crushing is extracted to the required composition leached in walnut repeatedly, obtains leachate；
Step 4: film process：Obtained leachate is handled by film, removes the salinity and small-molecule substance of centre；
Step 5: decolorization：Leachate after film process is subjected to decolorization, is put into resin column, carries out decolorization；
Step 6: revolving：Leachate after decolorization is put into Rotary Evaporators and carries out revolving processing, by leaching therein
Agent evaporates, and can be continuing with；
Step 7: dry：Obtained epiphysin is put into drying box and is dried, removes the leaching agent not eliminated.
A kind of 2. inexpensive epiphysin separation method according to claims 1, it is characterised in that the step 2,
The walnut after freezing is crushed by wet pulverizing.
A kind of 3. inexpensive epiphysin separation method according to claims 1, it is characterised in that the step 3,
Leaching agent is used as by petroleum ether, the walnut after crushing is carried out to be put into ultrasonic unit progress leaching process, shaken by ultrasound
It is dynamic when being delivered in liquid, cavitation effect is excited, so as to produce substantial amounts of cavitation bubble in a liquid, with these cavitation bubbles
Generation and explosion, will produce microjet, enter to be about to the great solid particle of liquid and smash, simultaneously because the vibration of ultrasonic wave, makes
Solid-liquid more fully mixes, and makes clasmatosis, and the extraction of cell inclusion is more perfectly sound.
A kind of 4. inexpensive epiphysin separation method according to claims 1, it is characterised in that the step 4,
Concentrating and separating processing is carried out by reverse osmosis membrane, uses cotton, timber of containing cellulose etc. as raw material, it is anti-through over-churning and hydrolysis
Acetic acid, Triafol T should be made, be reprocessed into reverse osmosis membrane.
A kind of 5. inexpensive epiphysin separation method according to claims 1, it is characterised in that the step 5,
Handled by the ion exchange resin in resin column, crosslinking of the ion exchange resin using styrene and divinylbenzene as skeleton
Product, along with corresponding function group such as sulfonic group or quaternary ammonium, for the skeleton of mandruka columnar structure, inside has largely
Permanent micropore, then import cation exchange groups and be made, has a micropore and big mesh, the aperture of wetting resin up to 100~
500nm。
A kind of 6. inexpensive epiphysin separation method according to claims 1, it is characterised in that the step 7,
Processing is dried by vacuum drier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710715724.8A CN107382817A (en) | 2017-08-20 | 2017-08-20 | A kind of inexpensive epiphysin separation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710715724.8A CN107382817A (en) | 2017-08-20 | 2017-08-20 | A kind of inexpensive epiphysin separation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107382817A true CN107382817A (en) | 2017-11-24 |
Family
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| CN201710715724.8A Pending CN107382817A (en) | 2017-08-20 | 2017-08-20 | A kind of inexpensive epiphysin separation method |
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| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072479A (en) * | 2021-03-26 | 2021-07-06 | 罗田县新普生药业有限公司 | Method for extracting melatonin from melatonin crystallization mother liquor |
| CN116751149A (en) * | 2023-06-06 | 2023-09-15 | 北京逯博士行为医学科技研究院有限公司 | Preparation method of natural melatonin |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106543068A (en) * | 2016-09-24 | 2017-03-29 | 合肥信达膜科技有限公司 | A kind of melatonin separating technology |
-
2017
- 2017-08-20 CN CN201710715724.8A patent/CN107382817A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106543068A (en) * | 2016-09-24 | 2017-03-29 | 合肥信达膜科技有限公司 | A kind of melatonin separating technology |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072479A (en) * | 2021-03-26 | 2021-07-06 | 罗田县新普生药业有限公司 | Method for extracting melatonin from melatonin crystallization mother liquor |
| CN116751149A (en) * | 2023-06-06 | 2023-09-15 | 北京逯博士行为医学科技研究院有限公司 | Preparation method of natural melatonin |
| CN116751149B (en) * | 2023-06-06 | 2024-03-15 | 北京逯博士行为医学科技研究院有限公司 | Preparation method of natural melatonin |
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