CN106349015B - A kind of method that multistage condenses, recycles distillation extraction high-purity natural borneol - Google Patents
A kind of method that multistage condenses, recycles distillation extraction high-purity natural borneol Download PDFInfo
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- CN106349015B CN106349015B CN201610618732.6A CN201610618732A CN106349015B CN 106349015 B CN106349015 B CN 106349015B CN 201610618732 A CN201610618732 A CN 201610618732A CN 106349015 B CN106349015 B CN 106349015B
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- borneol
- multistage
- natural 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
- 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
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
Abstract
The present invention relates to a kind of methods for extracting high-purity natural borneol as raw material using borneol camphor tree or Blumea balsamifera, borneol camphor tree or the crushing of Blumea balsamifera branches and leaves are placed in distillation still first, according to 1:Water or distillate is added in the solid-liquid ratio of 3-7 and residue filter liquid impregnates 12-48h at 15-50 DEG C, then heating distillation still carries out distilling with water, mixed vapour is input in 3 sections of folded plate condensers and is condensed, product is obtained in second segment, the distillate and filtrate that first segment and third section obtain can be used for next group borneol camphor tree or Blumea balsamifera branches and leaves impregnate distillation, and filter residue can be used for countryside planting.The method of the present invention not only shortens technical process and improves the purity of product, but also reduce the generation of waste water and pollutant by detaching natural borneol and byproduct segmentation condensation with sublimating.Using borneol camphor tree as made from raw material without natural borneol product yield >=1.1%, purity >=95% that extract and crystallize again, natural borneol product purity >=85% produced as raw material using Blumea balsamifera.
Description
Technical field
The present invention relates to a kind of condensation of multistage, the methods for recycling distillation extraction high-purity natural borneol, belong to chemistry and life
Object pharmaceutical technology field.
Background technology
Borneol is divided into L-Borneol, d-Bomeol, left-handed isoborneol, dextrorotation isoborneol, racemic borneol by its optical activity.
By sources, it is divided into natural borneol and borneolum syntheticum, natural borneol is divided into natural L-Borneol and natural d-borneol.Natural dextrorotation
Borneol (D-borneol) original name " kapur ", also known as natural borneol, are commonly called as Borneolum, are the branches from borneol camphor tree, cinnamomum camphora and Borneolum tree
The crystallized product extracted through steam distillation in leaf, trunk.Natural L-Borneol is also known as L-Borneol, is from Blumea balsamifera
The extracted crystallization being processed into the fresh leaf of (B.balsamifera (L.) DC.).Natural borneol has inducing resuscitation of having one's ideas straightened out, clear
The effect of heat analgesic is a kind of rare rare medicinal material and advanced perfume (or spice) for treating pyreticosis coma, the illnesss such as convulsion is fainted, the red pain of larynx numbness
Material.In addition, natural borneol is widely used in the fields such as medicine, fragrance, cosmetics, food industry.
The production method of borneol is mainly extracted including the use of steam distillation from plant, chemical synthesis and biology are closed
At 3 kinds of methods such as method.Latter two method can all generate harmful isoborneol in the synthesis process due to technical reason,
And the d-Bomeol and L-Borneol of high-purity can not be obtained.Thus utilize steam distillation from plant (such as borneol camphor tree, Ai Na
Perfume (or spice) etc.) in extraction be still current production high-purity natural borneol unique method.Currently, the extraction of natural borneol is steamed from local method
It evaporates refinement to distill to modern industrialization, basic principle and production process variation are little, rely primarily on the experience that the older generation leaves, lack
As reference, to the production of natural borneol, there is also mistaken ideas, and there are low production efficiency, product purity are low for the research of systematic science
Problem.Therefore high-purity natural borneol preparation need deeper into research, the industrialized production of natural borneol is prepared with realization.
The plant extract technique of natural borneol is all made of traditional one organic solvent extracting process of steam distillation at present, should
The method generally existing operation cycle is long, water consumption is big, pollution is larger, yield is relatively low, product purity is low and the difficult drawbacks such as purify.
Invention content
It is an object of the invention to overcome the above problem present in existing natural borneol preparation process, one kind is provided with dragon
Brain camphor tree or Blumea balsamifera are the method that raw material directly extracts high-purity natural borneol, and product natural borneol not only can be improved in this method
Yield and purity, and highly shortened technological process and extraction time compared to traditional handicraft or subsequent purification obtains
The natural borneol product for obtaining higher purity provides facility, it is often more important that has significantly cut down yield and the row of organic pollution
High-volume.Technical scheme is as follows：
A kind of method that multistage condenses, recycles distillation extraction high-purity natural borneol, it is characterised in that include the following steps：
A by borneol camphor tree or Blumea balsamifera branches and leaves crushing be placed in distillation still, be added water, distillate, one kind in residue filter liquid or its
Combination is impregnated；B heats distillation still and carries out distilling with water；The mixed vapour that distillation still is overflowed is input to multistage condenser by c
In condensed, respectively obtain product natural borneol, distillate and residue.
In said program, borneol camphor tree branches and leaves dry product or the mass ratio of Blumea balsamifera fresh leaf and liquid are 1 in step a:3-7, material
Liquid soaking time is 12-48h, and soaking temperature is 10-50 DEG C.
In said program, first liquid in distillation still is heated to boiling in step b, then proceedes to heating 25-85min and carry out
Distilling with water.
In said program, multistage condenser described in step c is specially 3 sections, and steam condenses to obtain in first segment and third section
Distillate and being collected into distillates in liquid bath, sublimates to obtain product natural borneol in second segment.
In said program, first segment condenser temperature is controlled at 90-100 DEG C.
In said program, second segment condenser temperature is controlled at 60-90 DEG C.
In said program, third section condenser temperature is controlled in room temperature.
According to said program, the multistage condenser is 3 sections of folded plate condensers, and cooling medium is cooling water.
According to said program, the distillate in step a is applied mechanically to be distillated from what multistage condenser first segment and third section were discharged
Liquid, residue filter liquid are applied mechanically from distillation still and filter gained raffinate, and it is 10-100 times to apply mechanically number.
Compared with traditional extraction process, the invention has the advantages that：
(1) traditional distillation-organic solvent extraction extraction process has been abandoned, using process control, by product (natural dragon
Brain) it carries out segmentation condensation with byproduct (water and other volatile oil substances) and detaches with sublimating, technical process is shortened, is improved
The purity of product reduces the generation of waste water and pollutant.
(2) distillation still raffinate and distillate are applied to next distilling with water extraction process, further reduce natural dragon
Brain product loses while improving product yield, drastically reduces the discharge of high-concentration waste water.
(3) the method for the present invention is produced using the natural borneol without extracting and crystallizing again that borneol camphor tree branches and leaves dry product is produced as raw material
Product yield >=1.1% (in terms of dry product), purity >=95%.Using Blumea balsamifera fresh leaf as raw material produce without extracting and crystallizing again
Natural borneol product yield >=1.1% (in terms of dry product), purity >=85%.
Description of the drawings
Fig. 1 is the process flow chart of the present invention；
Fig. 2 is the device of the invention schematic diagram；
Fig. 3 is natural borneol GC-MS total ion chromatograms prepared by the embodiment of the present invention 1.
Wherein, 1 is distillation still, and 101 be batching hole, and 102 be mud hole, and 103 be heating steam entrance, and 103 ' steam for heat supply
The liquid outlet of vapour cooling liquid, first, second and third grade of condensation segment of the respectively multistage folded plate condenser of 2-1,2-2,2-3,201,
201 ' be respectively the cooling water import and export of the first condensation segment, and 202,202 ' be respectively the cooling water import and export of the second condensation segment,
203,203 ' be third condensation segment cooling water import and export, 204 for emptying exhaust tube.
Specific implementation mode
To make those of ordinary skill in the art fully understand technical scheme of the present invention and advantageous effect, below in conjunction with specific
Embodiment and attached drawing are further described.
A method of it extracting high-purity natural borneol using borneol camphor tree or Blumea balsamifera as raw material, technological process and is made
Equipment is as shown in Figs. 1-2.The technical principle of the present invention is as follows：In borneol camphor tree branches and leaves or Blumea balsamifera fresh leaf distilling with water process
In, natural borneol, vapor and volatility oils steam together.Wherein vapor and other ethereal oil substance dew points compared with
Height, (90-100 DEG C) collection reuse of condensation in first segment condenser；And target product natural borneol have easily distil/sublimate
Characteristic, and it sublimates a little relatively low, therefore sublimates to the cold precipitation in second segment condenser (60-90 DEG C), to realize and grease
Separation, also avoid the interference of other impurities from polluting；The steam not condensed in time is that distillate is received in the liquefaction of third condensation segment
Collect reuse.In addition, the distillate for condensing collection in first and third section of condenser still contains a small amount of natural borneol ingredient, by it
It is operated with distilling with water of the iterative cycles set for next batch together with vinasse, avoids natural borneol ingredients from lossing, improve
Its yield.Distillation still filtering gained filter residue, which is sent to borneol camphor tree or Blumea balsamifera planting site, makees green manure.Certain number (the 10- of recycled
100 times) after distillation still raffinate periodically discharge on a small quantity, and the distillate of the certain number (10-100 times) of recycled periodically carries out
The processing of borneol oil extract.
Embodiment 1
High-purity natural borneol is extracted in industrialized unit as shown in Figure 2 according to technological process as shown in Figure 1.It is first
To be by batching hole (101) input volume after 100kg borneol camphor tree branches and leaves dry products crushing (equivalent particle size about 0.5~2mm or so) first
In the distillation still 1 of 1000L, according still further to 1:5 solid-liquid ratio injects tap water, soak at room temperature 48h.Then in a manner of steam-heated
(heating steam enters pipeline by 103, by 103 ' outflows in the form of liquid cooled water) carries out distilling with water to distillation still and operates.
The mixed vapour distilled enters in multistage folded plate condenser, adjusts separately the flow of cooling water in condensers at different levels, and first
At 100~90 DEG C, 202 temperature of the second condensation segment is controlled at 90~80 DEG C the control of 201 temperature of condensation segment, make volatile oil substance and
The mixture of water is condensed on 201 folded plate of condensation segment, natural d-borneol in condensation segment 202 condense folded plate on be precipitated, not by and
The steam of Shi Lengning is further cooled to room temperature in condensation segment 203, and on-condensible gas is discharged through exhaust tube 204.
Wherein, it is equipped with successively below condensation segment 2-1,2-2 and 2-3 and receives bucket, collect distillate and natural dextrorotation dragon respectively
Brain product.After distillation still boiling begins to warm up 35 minutes, stop heating distillation, after system cooling, balling-up is condensing
Product about 1.115kg on section 2-2 folded plates.
After extraction process, the solid-liquid mixing residue in distillation still is discharged, raffinate about 200kg, filter residue collection are obtained after filtering
In send to planting site.Distillate in filtrate and 2-1 and 2-3 is applied in next distillation procedure.
Natural d-borneol product yield >=1.1% of the present embodiment production, purity >=95%, quality gas-chromatography point
The results are shown in Figure 3 for analysis, and Fig. 3 can confirm that main peak retention time is 12.917min, and corresponding substance is that target product is naturally right
Revolve borneol.
Embodiment 2
It is put into the distillation still 1 that volume is 2000L, is added by batching hole (101) after 200kg borneol camphor tree branches and leaves dry products are crushed
Residual (filter) liquid and distillate for entering last batch, supplementing a certain amount of clear water makes solid-liquid ratio be 1 ︰ 6, impregnates 36h at 40 DEG C.It connects
It and carries out distilling with water operation in a manner of steam-heated.The mixed vapour distilled enters in multistage folded plate condenser, point
Do not adjust the flow of cooling water in condensers at different levels, the control of 201 temperature of the first condensation segment is at 100~90 DEG C, the second condensation segment 202
Temperature is controlled at 90~70 DEG C, and the mixture of volatile oil substance and water is made to be condensed on 201 folded plate of condensation segment, natural dextrorotation dragon
Brain is condensed in condensation segment 202 and is precipitated on folded plate, and the steam not condensed in time is further cooled to room temperature in condensation segment 203, no
Solidifying gas is discharged through exhaust tube 204.Distillate and natural d-borneol product are collected respectively.
It is begun to warm up after forty minutes from distillation still boiling, stops heating distillation, wait for that system cools down, balling-up is in condensation segment
Product about 2.406kg on 2-2 folded plates.After extraction process, the residue in distillation still is discharged, filtrate is obtained about after filtering
460kg, filter residue concentration are sent to planting site.Distillate in filtrate and 2-1 and 2-3 is applied to next distillation procedure.This implementation
Example gained natural d-borneol product yield >=1.2%, purity >=95%.
Embodiment 3
It is put into the distillation still 1 that volume is 1000L, is added by batching hole (101) after 100kg Blumea balsamifera grass fresh leafs are crushed
Residual (filter) liquid and distillate of last batch, supplementing a certain amount of clear water makes solid-liquid ratio be 1 ︰ 4, impregnates 12h at 40 DEG C.Then
Distilling with water operation is carried out in a manner of steam-heated.The mixed vapour distilled enters in multistage folded plate condenser, respectively
The flow of cooling water in condensers at different levels is adjusted, for the control of 201 temperature of the first condensation segment at 100~90 DEG C, the second condensation segment 202 is warm
Degree control makes the mixture of volatile oil substance and water be condensed on 201 folded plate of condensation segment, natural L-Borneol at 90~75 DEG C
It condenses in condensation segment 202 and is precipitated on folded plate, the steam not condensed in time is further cooled to room temperature in condensation segment 203, does not coagulate
Gas is discharged through exhaust tube 204.Distillate and natural L-Borneol product are collected respectively.
It is begun to warm up after forty minutes from distillation still boiling, stops heating distillation, wait for that system cools down, balling-up is in condensation segment
Product about 1.162kg on 2-2 folded plates.After extraction process, the residue in distillation still is discharged, filtrate is obtained about after filtering
240kg, filter residue concentration are sent to planting site.Distillate in filtrate and 2-1 and 2-3 is applied to next distillation procedure.This implementation
Natural L-Borneol product yield >=1.1% of example gained, purity >=85%.
Embodiment 4
It is 10m that borneol camphor tree branches and leaves dry product 1000kg, which puts into volume, after crushed3In steeping tank, the steaming applied mechanically is added thereto
Kettle filtering raffinate and distillate are evaporated, supplementing a certain amount of clear water makes solid-liquid ratio be 1 ︰ 5, in intermittent stirring and 45 DEG C of temperature conditions
Under, it is spare after impregnating for 24 hours.Under agitation, it is the distillation still 1 of 1000L by 600kg mixtures force feed in steeping tank to volume
In, distilling with water operation is carried out in a manner of steam-heated, the mixed vapour distilled enters in multistage folded plate condenser, point
Do not adjust the flow of cooling water in condensers at different levels, the control of 201 temperature of the first condensation segment is at 100~90 DEG C, the second condensation segment 202
Temperature is controlled at 90~80 DEG C, and the mixture of volatile oil substance and water is made to be condensed on 201 folded plate of condensation segment, natural dextrorotation dragon
Brain is condensed in condensation segment 202 and is precipitated on folded plate, and the steam not condensed in time is further cooled to room temperature in condensation segment 203, no
Solidifying gas is discharged through exhaust tube 204.
After distillation still boiling begins to warm up 35 minutes, stop heating distillation, waits for that system cools down, balling-up is in condensation segment
Product about 1.203kg on 2-2 folded plates.After extraction process, the solid-liquid mixing raffinate in distillation still is discharged, is obtained after filtering residual
Liquid about 200kg, filter residue concentration are sent to planting site.Distillate in filtrate and 2-1 and 2-3 is applied to next distillation procedure.Institute
Obtain natural d-borneol product yield >=1.2%, purity >=95%.
Claims (8)
1. a kind of method of multistage condensation, cycle distillation extraction high-purity natural borneol, it is characterised in that include the following steps：
Borneol camphor tree or the crushing of Blumea balsamifera branches and leaves are placed in distillation still by a, and one kind in water, distillate, residue filter liquid is added
Or combinations thereof impregnated；
B heats distillation still and carries out distilling with water；
The mixed vapour that distillation still is overflowed is input in multistage condenser and condenses by c, respectively obtains product natural borneol, evaporates
Go out liquid and residue；
Wherein, multistage condenser described in step c is specially 3 sections, and steam condenses to obtain distillate and quilt in first segment and third section
It is collected into and distillates in liquid bath, sublimate to obtain product natural borneol in second segment.
2. the method for multistage condensation as described in claim 1, cycle distillation extraction high-purity natural borneol, it is characterised in that：
Borneol camphor tree branches and leaves dry product or the mass ratio of Blumea balsamifera fresh leaf and liquid are 1 in step a:3-7, feed liquid soaking time are 12-48h,
Soaking temperature is 10-50 DEG C.
3. the method for multistage condensation as described in claim 1, cycle distillation extraction high-purity natural borneol, it is characterised in that：
First liquid in distillation still is heated to boiling in step b, then proceedes to heating 25-85min and carry out distilling with water.
4. the method for multistage condensation as described in claim 1, cycle distillation extraction high-purity natural borneol, it is characterised in that：
First segment condenser temperature is controlled at 90-100 DEG C.
5. the method for multistage condensation as described in claim 1, cycle distillation extraction high-purity natural borneol, it is characterised in that：
Second segment condenser temperature is controlled at 60-90 DEG C.
6. the method for multistage condensation as described in claim 1, cycle distillation extraction high-purity natural borneol, it is characterised in that：
Third section condenser temperature is controlled in room temperature.
7. the method for multistage condensation as claimed in any one of claims 1 to 6, cycle distillation extraction high-purity natural borneol, special
Sign is：The multistage condenser is 3 sections of folded plate condensers, and cooling medium is cooling water.
8. the method for multistage condensation as claimed in any one of claims 1 to 6, cycle distillation extraction high-purity natural borneol, special
Sign is：Distillate in step a applies mechanically the distillate from multistage condenser first segment and the discharge of third section, residue filter liquid set
Gained raffinate is filtered with from distillation still, it is 10-100 times to apply mechanically number.
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| CN201610618732.6A CN106349015B (en) | 2016-08-01 | 2016-08-01 | A kind of method that multistage condenses, recycles distillation extraction high-purity natural borneol |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108484358A (en) * | 2018-04-27 | 2018-09-04 | 泉州市泉美生物科技有限公司 | A method of extracting natural d-borneol from camphor tree branches and leaves |
| CN110257174A (en) * | 2019-06-12 | 2019-09-20 | 湖南省林业科学院 | For the essential oil containing brain condensing unit and contain the Distallation systm of the condensing unit |
| CN111205169B (en) * | 2019-10-25 | 2022-11-29 | 绍兴文理学院元培学院 | Refining process of natural borneol |
| CN111635295A (en) * | 2020-06-08 | 2020-09-08 | 储和英 | Processing method of borneol filling material for mask health-care layer |
| CN115708786A (en) * | 2022-11-19 | 2023-02-24 | 贵州省罗甸县全兴药业开发有限责任公司 | Preparation method and application of blumea balsamifera and borneol water and bacteriostatic agent |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102423331A (en) * | 2011-12-06 | 2012-04-25 | 江口县苗药生物科技有限公司 | Method and equipment for preparing borneol flakes |
| 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 |
| CN104693008A (en) * | 2015-03-16 | 2015-06-10 | 江苏金叶子生物科技有限公司 | Method for coarsely extracting natural borneol from cinnamomum camphora |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102423331A (en) * | 2011-12-06 | 2012-04-25 | 江口县苗药生物科技有限公司 | Method and equipment for preparing borneol flakes |
| 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 |
| CN104693008A (en) * | 2015-03-16 | 2015-06-10 | 江苏金叶子生物科技有限公司 | Method for coarsely extracting natural borneol from cinnamomum camphora |
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