CN108503510A - A kind of green natural borneol process for purification - Google Patents
A kind of green natural borneol process for purification Download PDFInfo
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- CN108503510A CN108503510A CN201810475570.4A CN201810475570A CN108503510A CN 108503510 A CN108503510 A CN 108503510A CN 201810475570 A CN201810475570 A CN 201810475570A CN 108503510 A CN108503510 A CN 108503510A
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- borneol
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- 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
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/07—Optical isomers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2602/00—Systems containing two condensed rings
- C07C2602/36—Systems containing two condensed rings the rings having more than two atoms in common
- C07C2602/42—Systems containing two condensed rings the rings having more than two atoms in common the bicyclo ring system containing seven carbon atoms
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Abstract
The present invention provides a kind of process for purification of green natural borneol.After this hair first crushes borneol camphor tree branches and leaves, use ethanol water as solvent again, after combining ultrasonic Microwave-assisted Extraction concentration remove ethyl alcohol after obtain natural borneol crude extract, then successively using supermolecule solvent clean with recrystallize to crude extract carry out purify and refined natural borneol is quantitatively obtained to natural borneol using gas chromatography.The natural borneol purity obtained through the present invention is used directly for up to 98.5% in the production of biologic medical industry and chemical product toothpaste.
Description
Technical field
The present invention relates to the extractive technique of natural borneol, specially a kind of green natural borneol process for purification.
Background technology
Natural borneol is also known as natural d-borneol, and original name " kapur " is commonly called as Borneolum, is the branches and leaves from borneol camphor tree and tree
Crystallized product through steam distillation in dry.Natural borneol has the effect of inducing resuscitation of having one's ideas straightened out, clearing away heat to and alleviating pain, for treating pyreticosis god
Dusk, convulsion are fainted and the illnesss such as the red pain of larynx numbness.Currently, natural borneol is widely used in as rare rare medicinal material and fine perfumery
Medicine, fragrance, cosmetics, chemical product ointment, in food industry.Currently, the demand of China's natural borneol constantly increases, and city
It is almost captured entirely by borneolum syntheticum on field, China's separation not high to the aggregate level of natural borneol secondary industry and traditional is pure
Change method and step is cumbersome, and yield and purity is not high, cannot achieve the efficient utilization of natural borneol resource.Such as patent CN
105837405 A《A kind of preparation method of natural borneol》Disclosed in natural borneol method be：First borneol camphor tree branches and leaves are cut off
It is distilled using distillation still afterwards, the steam condensing gas being collected into is carried out removal of impurities postcooling using oil water separator to be crystallized
Finally it is centrifugally separating to obtain the solid of natural borneol.Although the industrial production efficiency is convenient, extraction efficiency is not high, and work
Skill is cumbersome, and obtained natural borneol purity is impure, limits application of the natural borneol in medicine and chemical product industry.Cause
This, the present invention provides a kind of green natural borneol process for purification.
Invention content
There is provided a kind of green natural borneol process for purification for problems solved by the invention.The method operation letter of the present invention
It is single, it is few using organic solvent, and extraction efficiency is high, obtained natural borneol purity is high.
To solve the above problems, the present invention provides the following technical solutions：A kind of green natural borneol process for purification, feature
It is to include the following steps：
（1）After borneol camphor tree branches and leaves clean dry, using pulverizer grinding and sieving, borneol camphor tree branches and leaves powder is obtained；
（2）Take the borneol camphor tree branches and leaves powder of 1.5kg with ethanol-water mixed solvent by 1：After the mass volume ratio mixing of 5-10,
400-600W ultrasonic powers, microwave-is after ultrasound a period of time under the conditions of the microwave power of 200-300W and 20-50 DEG C, filtering,
Filtrate is collected, and by after residue continuation microwave-ultrasonic extraction 2-3 times, after merging filtrate, vacuum distillation obtains natural borneol and slightly carries
Object；
（3）600g natural borneol crude extracts are weighed, by 1：After being centrifuged after vortex 20s after the solid-to-liquid ratio addition supermolecule solvent of 1-2
After outwelling supernatant, by 1：The solid-to-liquid ratio of 3-4 is put into agitating and heating in water-bath after solvent is added, until borneol crude product is complete
Afterwards, after keeping the temperature 1 hour, standing filters solvent, and obtained crystallized product is positioned in vacuum drying chamber after drying and is obtained
The purity of borneol is measured to refined natural borneol, and using gas chromatography.
Further, step（1）Described in sieving be 60 mesh pharmacopeia sieve.
Further, step（2）Described in ethanol-water mixed solvent in ethyl alcohol percent by volume be 15-25%.
Further, step（2）Described in microwave-ultrasound time be 20-40min.
Further, step（3）Described in supermolecule solvent be tetrahydrofuran-n-octyl alcohol-water, tetrahydrofuran-just oneself
One kind in alcohol-water, tetrahydrofuran-caprylic acid-water supermolecule solvent；It is 200- to contain grain size in the supermolecule solvent
The aggregation of 600nm.
Further, step（3）Described in solvent be 120#Gasoline；The water-bath pot temperature is 40-50 DEG C.
Further, step（3）Described in time of repose be 10-12 hour, dwell temperature be 8-15 DEG C.
Further, step（3）Described in the testing conditions of gas chromatography be：DB-5 chromatographic columns (30m × 250mm
× 0.25um), hydrogen flame ionization detector (FID), detector temperature is 300 DEG C, carrier gas N2,Injector temperature is 250 DEG C,
Sample size 0.5ul, using temperature programming, column temperature is 80 DEG C, and 150 DEG C are risen to 3 DEG C/min after 2 min of heat preservation；The standing of preparation
Borneol purity is 98.5-99.2%.
It is super to use microwave-compared with traditional preparation methods for a kind of green natural borneol process for purification of the present invention
The abstraction technique of sound auxiliary, considerably improves the extraction efficiency of active ingredient, while shortening extraction time；The present invention uses
Supermolecule solvent carries out removal of impurities and uses organic solvent few, and dust removal rate is high, more environmentally protective；It is molten as recrystallizing using gasoline
Agent can remove most polar compound, substantially increase the purity of natural borneol.The present invention is easy to operate, and use is organic
Solvent is few.Obtained natural borneol utilizes its purity of vapor detection 98.5% or more, and the borneol through invention gained can be direct
In production for biological medicine and chemical product ointment.
Description of the drawings
Fig. 1 is the gas chromatogram of natural borneol prepared by the present invention, and peak 1 is natural borneol.
Specific implementation mode
A kind of green natural borneol process for purification of the present invention is done further below with reference to specific embodiment
It illustrates, to help those skilled in the art to have more complete, accurate and deep reason to the inventive concept of the present invention, technical solution
Solution.
Embodiment 1
After borneol camphor tree branches and leaves clean dry, smashes it through 60 mesh pharmacopeia using pulverizer and sieve, obtain borneol camphor tree branches and leaves powder；It takes
The borneol camphor tree branches and leaves powder of 1.5kg and 25% ethanol-water mixed solvent press 1：After 6 mass volume ratio mixing, in 400W ultrasounds
Power, under the conditions of the microwave power of 250W and 35 DEG C after microwave-ultrasound 25min, filtering collects filtrate, and residue is continued
After microwave-ultrasonic extraction 3 times, after merging filtrate, vacuum distillation obtains natural ice crude extract；600g natural borneols are weighed slightly to carry
Object, by 1：Supernatant is outwelled after being centrifuged after vortex 20s after 3 solid-to-liquid ratio addition tetrahydrofuran-caprylic acid-water supermolecule solvent
Afterwards, by 1：3 solid-to-liquid ratio is put into agitating and heating in water-bath after 120# gasoline is added, until after borneol crude product is complete, heat preservation 1 is small
Solvent is filtered after Shi Hou, 10 DEG C of standing 2h, obtained crystallized product is positioned in vacuum drying chamber after drying and is obtained
Refined natural borneol.
Embodiment 2
After borneol camphor tree branches and leaves clean dry, smashes it through 60 mesh pharmacopeia using pulverizer and sieve, obtain borneol camphor tree branches and leaves powder；It takes
The borneol camphor tree branches and leaves powder of 1.5kg and 15% ethanol-water mixed solvent press 1：It is super in 500W after 10 mass volume ratio mixing
Acoustical power, under the conditions of the microwave power of 200W and 30 DEG C after microwave-ultrasound 30min, filtrate is collected in filtering, and by residue after
After continuous microwave-ultrasonic extraction 2 times, after merging filtrate, vacuum distillation obtains natural ice crude extract；600g natural borneols are weighed slightly to carry
Object, by 1：Supernatant is outwelled after being centrifuged after vortex 20s after 2 solid-to-liquid ratio addition tetrahydrofuran-n-octyl alcohol-water supermolecule solvent
Afterwards, by 1：4 solid-to-liquid ratio is put into agitating and heating in water-bath after 120# gasoline is added, until after borneol crude product is complete, heat preservation 1 is small
Solvent is filtered after Shi Hou, 10 DEG C of standing 10h, obtained crystallized product is positioned in vacuum drying chamber after drying and is obtained
Refined natural borneol.
Embodiment 3
After borneol camphor tree branches and leaves clean dry, smashes it through 60 mesh pharmacopeia using pulverizer and sieve, obtain borneol camphor tree branches and leaves powder；It takes
The borneol camphor tree branches and leaves powder of 1.5kg and 20% ethanol-water mixed solvent press 1：After 8 mass volume ratio mixing, in 500W ultrasounds
Power, under the conditions of the microwave power of 250W and 30 DEG C after microwave-ultrasound 25min, filtering collects filtrate, and residue is continued
After microwave-ultrasonic extraction 3 times, after merging filtrate, vacuum distillation obtains natural ice crude extract；600g natural borneols are weighed slightly to carry
Object, by 1：Supernatant is outwelled after being centrifuged after vortex 20s after 3 solid-to-liquid ratio addition tetrahydrofuran-n-octyl alcohol-water supermolecule solvent
Afterwards, by 1：3 solid-to-liquid ratio is put into agitating and heating in water-bath after 120# gasoline is added, until after borneol crude product is complete, heat preservation 1 is small
Solvent is filtered after Shi Hou, 10 DEG C of standing 12h, obtained crystallized product is positioned in vacuum drying chamber after drying and is obtained
Refined natural borneol.
The detection method of natural borneol obtained by embodiment 1-3 is：DB-5 chromatographic columns (30m × 250mm × 0.25um), hydrogen
Flame ionic detector (FID), 300 DEG C, carrier gas N2,Injector temperature is 250 DEG C, sample size 0.5ul, using temperature programming,
Column temperature is 80 DEG C, and 150 DEG C are risen to 3 DEG C/min after 2 min of heat preservation；The standing borneol purity prepared through the present invention is 98.5-
99.2%.Chromatogram obtained by this method is as shown in Fig. 1, and as can be seen from the figure the purity of natural borneol is high, magazine content
It is low.
The recovery rate and purity for the natural borneol that embodiment 1-3 preparation methods obtain are as shown in table 1.
| Test event | Recovery rate（%） | Purity（%） |
| Embodiment 1 | 88 | 99.0 |
| Embodiment 2 | 85 | 98.8 |
| Embodiment 3 | 84 | 99.2 |
For the ordinary skill in the art, specific embodiment is only exemplarily described the present invention,
Obviously the present invention specific implementation is not subject to the restrictions described above, as long as use the inventive concept and technical scheme of the present invention into
The improvement of capable various unsubstantialities, or it is not improved by the present invention design and technical solution directly apply to other occasions
, within protection scope of the present invention.
Claims (8)
1. a kind of green natural borneol process for purification, it is characterised in that include the following steps：
（1）After borneol camphor tree branches and leaves clean dry, using pulverizer grinding and sieving, borneol camphor tree branches and leaves powder is obtained；
（2）Take the borneol camphor tree branches and leaves powder of 1.5kg with ethanol-water mixed solvent by 1：After the mass volume ratio mixing of 5-10,
400-600W ultrasonic powers, microwave-is after ultrasound a period of time under the conditions of the microwave power of 200-300W and 20-50 DEG C, filtering,
Filtrate is collected, and by after residue continuation microwave-ultrasonic extraction 2-3 times, after merging filtrate, vacuum distillation obtains natural borneol and slightly carries
Object；
（3）600g natural borneol crude extracts are weighed, by 1：After being centrifuged after vortex 20s after the solid-to-liquid ratio addition supermolecule solvent of 1-2
After outwelling supernatant, by 1：The solid-to-liquid ratio of 3-4 is put into agitating and heating in water-bath after solvent is added, until borneol crude product is completely molten
Xie Hou, after keeping the temperature 1 hour, standing filters solvent, and obtained crystallized product is positioned in vacuum drying chamber after drying
Refined natural borneol is obtained, and the purity of borneol is measured using gas chromatography.
2. a kind of green natural borneol process for purification according to claim 1, it is characterised in that step（1）Described in mistake
Sieve is that 60 mesh pharmacopeia are sieved.
3. a kind of green natural borneol process for purification according to claim 1, it is characterised in that step（2）Described in second
The percent by volume of ethyl alcohol is 15-25% in alcohol-water mixed solvent.
4. a kind of green natural borneol process for purification according to claim 1, it is characterised in that step（2）Described in it is micro-
The time of wave-ultrasound is 20-40min.
5. a kind of green natural borneol process for purification according to claim 1, it is characterised in that step（3）Described in it is super
Molecular solvent is tetrahydrofuran-n-octyl alcohol-water, tetrahydrofuran-n-hexyl alcohol-water, tetrahydrofuran-caprylic acid-water supermolecule solvent
In one kind；Contain the aggregation that grain size is 200-600nm in the supermolecule solvent.
6. a kind of green natural borneol process for purification according to claim 1, it is characterised in that step（3）Described in it is molten
Agent is 120#Gasoline；The water-bath pot temperature is 40-50 DEG C.
7. a kind of green natural borneol process for purification according to claim 1, it is characterised in that step（3）Described in it is quiet
It is 10-12 hours to set the time, and dwell temperature is 8-15 DEG C.
8. a kind of green natural borneol process for purification according to claim 1, it is characterised in that step（3）Described in gas
The testing conditions of phase chromatography are：DB-5 chromatographic columns (30m × 250mm × 0.25um), hydrogen flame ionization detector (FID), inspection
Survey 300 DEG C of device temperature, carrier gas N2, injector temperature is 250 DEG C, sample size 0.5ul, and using temperature programming, column temperature is 80 DEG C,
It keeps the temperature and rises to 150 DEG C with 3 DEG C/min after 2 min；The standing borneol purity of preparation is 98.5-99.2%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810475570.4A CN108503510B (en) | 2018-05-17 | 2018-05-17 | Green natural borneol refining method |
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| CN201810475570.4A CN108503510B (en) | 2018-05-17 | 2018-05-17 | Green natural borneol refining method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971545A (en) * | 2019-04-10 | 2019-07-05 | 范加家 | The high yield processing method of borneol essential oil |
| CN110003985A (en) * | 2019-04-10 | 2019-07-12 | 范加家 | A kind of combination sound wave extracting method of borneol essential oil |
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| CN103601619A (en) * | 2013-11-01 | 2014-02-26 | 宜昌万森生态科技发展有限公司 | Extraction method and extraction equipment of natural borneol |
| CN107970156A (en) * | 2017-12-16 | 2018-05-01 | 唐雪平 | A kind of preparation method of chemical product ginsenoside extract |
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2018
- 2018-05-17 CN CN201810475570.4A patent/CN108503510B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601619A (en) * | 2013-11-01 | 2014-02-26 | 宜昌万森生态科技发展有限公司 | Extraction method and extraction equipment of natural borneol |
| CN107970156A (en) * | 2017-12-16 | 2018-05-01 | 唐雪平 | A kind of preparation method of chemical product ginsenoside extract |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971545A (en) * | 2019-04-10 | 2019-07-05 | 范加家 | The high yield processing method of borneol essential oil |
| CN110003985A (en) * | 2019-04-10 | 2019-07-12 | 范加家 | A kind of combination sound wave extracting method of borneol essential oil |
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| CN108503510B (en) | 2021-08-10 |
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Address after: 343000 No. 898 beside Lushuihe Avenue, Anfu Industrial Park, Ji'an City, Jiangxi Province Patentee after: Jiangxi Zhangxiang natural borneol Co.,Ltd. Patentee after: Guangdong Kangwang Daily Chemical Co., Ltd Address before: 343200 No. 898 beside Lushuihe Avenue, Anfu county industrial park, Ji'an City, Jiangxi Province Patentee before: JIANGXI ZHANGXIANG NATURAL BORNEOL CO.,LTD. Patentee before: Guangdong Kangwang Daily Chemical Co., Ltd |