CN109293671A - A kind of purification process of Cineole - Google Patents
A kind of purification process of Cineole Download PDFInfo
- Publication number
- CN109293671A CN109293671A CN201811023603.8A CN201811023603A CN109293671A CN 109293671 A CN109293671 A CN 109293671A CN 201811023603 A CN201811023603 A CN 201811023603A CN 109293671 A CN109293671 A CN 109293671A
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- CN
- China
- Prior art keywords
- cineole
- purification process
- valve
- eucalyptus oil
- temperature
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/08—Bridged systems
Abstract
The present invention provides a kind of purification process of Cineole, step is to be centrifuged first by eucalyptus oil freezing and crystallizing, then after crystal obtained by preceding step is crushed, and obtains thick Cineole and mother liquor, thick Cineole obtained by step before last rectifying.Method provided by the present invention, simple process, period is shorter, yield is higher, and cost is relatively low, solves in the prior art, from folium eucalypti oil refining Cineole, there are process complexity, product purity is low, the small problem of output, is suitable for industrialized production, provided method through the invention, gained Cineole purity is greater than 99.9%, using method provided by the present invention, can according to need, further rectifying mother liquid obtained in purification process is obtained into eucalyptus oil and camphor oil white, whole process of purification is generated without waste, environmental-friendly, and raw material availability is high.
Description
Technical field
The invention belongs to eucalyptus oil separating and purifying technology fields, and in particular to a kind of purification process of Cineole.
Background technique
Cineole is widely used in pharmaceuticals industry due to its special aromatic odor and good sterilization, disinfecting power, main
It is used for toothpaste, tooth powder, talcum powder, medicated soap, chewing gum and cough drop etc..
In the prior art, mainly have from the method for folium eucalypti oil refining Cineole: chemical reaction method, special extract rectification method, silica gel
Chromatography, fused junction crystallization and freeze crystallization.Chemical reaction method the problem is that: need secondary separation process, process ratio
More complex, and exist in technical process and be harmful to the human body substance, when separation, is not thorough, and will affect the quality of Cineole；It is special
Rectification method the problem is that: folium eucalypti cellulose content obtained can only achieve 99%, be unable to satisfy market to the need of high-purity Cineole
It wants；Silica gel chromatography the problem is that: treating capacity is small, be not suitable for industrialization large-scale production；It is asked existing for fused junction crystallization
Topic is: the Cineole purity being prepared is low, and output is small, and operating process is cumbersome；Freeze crystallization the problem is that: it is raw
The production period is longer, and can only obtain the Cineole that content is 99%.
To sum up, it in order to obtain the Cineole of higher degree from eucalyptus oil, still needs to develop a kind of new method.
Summary of the invention
To solve in the prior art, from folium eucalypti oil refining Cineole there are process complexity, product purity is low, and output is small
Problem, the object of the present invention is to provide a kind of purification process of Cineole.
To achieve the above object, the invention adopts the following technical scheme:
A kind of purification process of Cineole, step include:
(1) by eucalyptus oil freezing and crystallizing；
(2) it is centrifuged after crushing crystal obtained by step (1), obtains thick Cineole and mother liquor；
(3) thick Cineole obtained by rectification step (2).
Preferably, in step (1) described eucalyptus oil, the mass percentage of Cineole is greater than 80%.
Preferably, the time of step (1) described freezing is 48h, and temperature is -15~-25 DEG C.
Preferably, the time of step (2) described centrifugation is 30~45min.
Preferably, step (3) described rectifying evaporated before including, in evaporate and after evaporate.
It is further preferred that the bottom temperature evaporated before described is 70~85 DEG C, tower top temperature is 65~75 DEG C.
It is further preferred that the bottom temperature evaporated in described is 80~90 DEG C, tower top temperature is 70~75 DEG C.
It is further preferred that the bottom temperature evaporated after described is 90~120 DEG C, tower top temperature is 73~100 DEG C.
Method provided by the present invention removes mother liquor using the congealing point difference of each composition, is centrifuged to obtain thick folium eucalypti
After element, through distilling the Cineole for obtaining content and being greater than 99.5%.
In method provided by the present invention, the eucalyptus oil for being first 80% by content respectively enters refrigerator knot after Weighing
In brilliant food tray, refrigerator and the refrigeration crystallization of cool brine valve are opened.The crystal come out after chilled crystallization is centrifugated out after crushed
Thick Cineole and mother liquor, thick Cineole melt barrelling and are deployed into finished product after sending to rectifying column processing, and mother liquor is sent to rectifying section point
The low eucalyptus oil of different content is deployed into after evaporating.Crystalline solid is into before centrifuge, it is necessary to which being ground into fine granularity, equilibrium is put into again
In centrifugal basket.
When rectifying mother liquor, vacuum system and pipeline valve have first been checked, opened carbonated drink ejector vacuum pump (water ring grade), surely
When reciprocal of duty cycle is greater than -0.06MPa, raw material is sucked into rectifying tower reactor, cooling water valve is opened and then opens steam heating, slowly increase
Big steam pressure, and adjust reflux ratio, carries out rectifying, rectification step is dehydration, go out before evaporate, in evaporate, after evaporate.
When rectifying Cineole, vacuum system and pipeline valve have first been checked, open water stream injection pump or water ring pump, it is quantitative to suck
Thick Cineole is to rectifying tower reactor.Open water circulating pump, heating, distillation.It is first dehydrated, then rapid steaming goes out product to ensure product matter
Amount.
Beneficial effects of the present invention
1, method provided by the present invention, simple process, the period is shorter, and yield is higher, and cost is relatively low, solves existing skill
In art, from folium eucalypti oil refining Cineole there are process complexity, product purity is low, the small problem of output, is suitable for industrial metaplasia
It produces；
2, provided method, gained Cineole purity are greater than 99.9% through the invention；
3, it using method provided by the present invention, can according to need, by further rectifying mother liquid obtained in purification process
Eucalyptus oil and camphor oil white are obtained, whole process of purification is generated without waste, and environmental-friendly, raw material availability is high.
Detailed description of the invention
Fig. 1 is the process flow chart of Cineole purification process.
Specific embodiment
The following is specific embodiments of the present invention, and is described with reference to the drawings and further retouches to technical solution of the present invention work
It states, however, the present invention is not limited to these examples.
Embodiment 1
A kind of purification process of Cineole, process is as shown in Figure 1, step includes:
(1) by eucalyptus oil freezing and crystallizing；
(2) it is centrifuged after crushing crystal obtained by step (1), obtains thick Cineole and mother liquor；
(3) thick Cineole obtained by rectification step (2).
In step (1) described eucalyptus oil, the mass percentage of Cineole is greater than 80%.
The time of step (1) described freezing is 48h, and temperature is -15 DEG C.
The time of step (2) described centrifugation is 30min.
Step (3) described rectifying evaporates before including, in evaporate and after evaporate, wherein the preceding bottom temperature evaporated is 70 DEG C, tower top temperature
It is 65 DEG C；In the bottom temperature that evaporates be 80 DEG C, tower top temperature is 70 DEG C；The bottom temperature evaporated afterwards is 90 DEG C, tower top temperature 73
℃。
The equipment that can be selected is as shown in table 1.
The list of devices that table 1 can be selected
Before purification, whether need to confirming the cleaning of used tower reactor, whether the equipment such as vacuum pump are normal.
Notice boiler room send the steam main valve slowly opened after vapour on gas-distributing cylinder, and observe steam pressure gauge pressure whether
It meets the requirements.Cleaning, the inspection of foreign substance of filter device etc. of tower reactor feed inlet used perform relative recording.
Before charging, for outsourcing raw material, it should which the detection data neck according to Pin Kong department confirms batch, quantity to workshop
Heating in sucking kettle after errorless.
The feeding manner of rectifying column is divided into vacuum intake and oil pump inputs two kinds of methods.
Wherein, when vacuum intake, close the valve that is communicated with the atmosphere in rectifying tower system: i.e. the baiting valve of receiver bottom with
Blow valve, the sampling valve on the blow valve (material sucking valve) and capillary regulating valve and system of tower reactor.Simultaneously by its in system
Remaining valve is placed in open state, the vacuum degree according to required by different product, selects different vacuum pumps, and press vacuum pump phase
Safety regulation for operations is closed, vacuum pump is opened, to system forvacuum, when the pressure indicator of vacuum meter in tower reactor reaches -0.06Mpa
When, suction can be started, after suction, material inlet valve is closed, start to warm up carry out distillation operation.
When oil pump inputs, tower reactor bottom discharge valve and capillary regulating valve are closed, closes receiver bottom discharge valve, is opened
Receiver vent valve and tower reactor inlet valve vent valve (material sucking valve) open the sampling valve in pipe-line system.Simultaneously by its in system
Remaining valve is placed in open state, is operated by oil pump operating instruction, and required material is input in rectifying tower reactor, charging knot
Shu Hou closes product pump charging/discharging valve, stops product pump, turn off other valves being connected in tower reactor outlet valve and system with atmosphere
Door can start to vacuumize heating progress distillation operation.
When distillation operation, reflux ratio controller is adjusted, reflux ratio is in and returns state entirely, adjust the unlatching of capillary valve
Degree makes to form a boiling center in kettle, but it is excessive to must be noted that capillary valve cannot be opened, in order to avoid cause under vacuum degree
Drop sets bottom temperature value, according to the technique working condition of different product, sets the temperature control of bottom temperature display control instrument
Value slowly opens the steam valve of gas-distributing cylinder, supplies gas to equipment, material ramp case in kettle is often observed, such as heating rate mistake
In slow, temperature controlling value should be suitably adjusted, as bottom temperature rises, there will be material to distillate, at this point, paying attention in observation visor
There are dripless or liquid stream.Occur if any drop, then adjusts reflux ratio and be adjusted to infinite reflux, and kept for 30~40 minutes, infinite reflux knot
Shu Hou adjusts reflux ratio to appropriate value.Note: the different fractions of different product have different reflux ratios, according to tower top temperature
Variation distillates the quantity of material and the data of process sampling measurement, in time and switches in fraction to different receivers, in receiver
Material drain after, should be in time by receiver forvacuum.The forvacuum of receiver should open forepump, when vacuum degree reaches
, can be spare by the receiver input coefficient after it is required that, just receiver can't be connected without forvacuum with system, be destroyed in tower
It balances, in distillation process, pays attention to adjusting tower reactor heating temperature in time according to different fractions.Material in kettle should be often observed simultaneously
Liquid level should close corresponding heating coil valve if liquid level is lower than heating coil in kettle in time.
When parking, steam valve on steam off gas-distributing cylinder should will be on gas-distributing cylinder when not having other equipment vapour such as
Main valve is closed, and boiler room stopping is notified to send vapour, is closed tower reactor bottom coil and is heated steam valve, and opens the chassis being attached thereto
Pipe cooling water valve keeps salvage stores fast cooling in kettle cooling, in kettle after material cooling, inlet valve can be closed, by vacuum
After disengaging valve on surge tank is closed, stop vacuum pump, slowly blow valve in open system, slowly deflates into tower, makes sure to keep in mind not
It can deflate too fast, in order to avoid causing fire incident, open tower reactor bottom discharge valve, the salvage stores (leftover bits and pieces) in kettle is put to old packet
In barrelling, baiting valve is closed.
It should be noted that item have: in operating process, often pay attention to observation temperature, pressure and the variation for distillating speed, and
Record in time in operating process and relevant issues, should record and be illustrated in operating instruction, various different products, difference
In fraction either metal bucket packaging or input basin, there need to be obvious mark, and measure and record in time, after distillation, and
When carry out mass balance, and recorded, during distillation procedure, heating steam valve should be first shut off in case of cut off the water, having a power failure,
Stop heating, in operating process, all original records strictly according to the facts, must be filled in conscientiously.Minute book keeps clean and tidy, must not arbitrarily apply
Change, if modified because filling out mistake, rewriting should be crossed out, and sign modification people's name, time, distillation tower reactor feed inlet filter device into
Coherence check must be carried out before material, unpicked and washed after charging and cleared up foreign matter impurity etc. and to form writing record standby
It looks into, distills the cleaning and replacement of tower reactor feed pipe, oil foot discharging hose, the raw material with kind does not have to cleaning, uses when replacing kind
Edible alcohol (ethyl alcohol) is cleaned and is dried, and hose is not replaced generally at bottom discharge oil foot, and emission is that oil foot is (discarded
Object).
Embodiment 2
A kind of purification process of Cineole, step include:
(1) by eucalyptus oil freezing and crystallizing；
(2) it is centrifuged after crushing crystal obtained by step (1), obtains thick Cineole and mother liquor；
(3) thick Cineole obtained by rectification step (2).
In step (1) described eucalyptus oil, the mass percentage of Cineole is greater than 80%.
The time of step (1) described freezing is 48h, and temperature is -25 DEG C.
The time of step (2) described centrifugation is 45min.
Step (3) described rectifying evaporates before including, in evaporate and after evaporate, wherein the preceding bottom temperature evaporated is 85 DEG C, tower top temperature
It is 75 DEG C；In the bottom temperature that evaporates be 90 DEG C, tower top temperature is 75 DEG C；The bottom temperature evaporated afterwards is 120 DEG C, and tower top temperature is
100℃。
Embodiment 3
A kind of purification process of Cineole, step include:
(1) by eucalyptus oil freezing and crystallizing；
(2) it is centrifuged after crushing crystal obtained by step (1), obtains thick Cineole and mother liquor；
(3) thick Cineole obtained by rectification step (2).
In step (1) described eucalyptus oil, the mass percentage of Cineole is greater than 80%.
The time of step (1) described freezing is 48h, and temperature is -20 DEG C.
The time of step (2) described centrifugation is 35min.
Step (3) described rectifying evaporates before including, in evaporate and after evaporate, wherein the preceding bottom temperature evaporated is 75 DEG C, tower top temperature
It is 70 DEG C；In the bottom temperature that evaporates be 85 DEG C, tower top temperature is 72 DEG C；The bottom temperature evaporated afterwards is 105 DEG C, tower top temperature 85
℃。
Detect example
By the eucalyptus oil of Cineole mass percentage 80%, using the method for Examples 1 to 3, purifying obtains three kinds of eucalyptus
Foline, number are respectively A, B and C, test its physicochemical property, are as a result listed in table 2.
The physicochemical property testing result of 2 Cineole of table
Claims (8)
1. a kind of purification process of Cineole, which is characterized in that step includes:
(1) by eucalyptus oil freezing and crystallizing；
(2) it is centrifuged after crushing crystal obtained by step (1), obtains thick Cineole and mother liquor；
(3) thick Cineole obtained by rectification step (2).
2. the purification process of Cineole according to claim 1, which is characterized in that in step (1) described eucalyptus oil, folium eucalypti
The mass percentage of element is greater than 80%.
3. the purification process of Cineole according to claim 1, which is characterized in that the time of step (1) described freezing is
48h, temperature are -15~-25 DEG C.
4. the purification process of Cineole according to claim 1, which is characterized in that the time of step (2) described centrifugation is
30~45min.
5. the purification process of Cineole according to claim 1, which is characterized in that step (3) described rectifying evaporates before including,
In evaporate and after evaporate.
6. the purification process of Cineole according to claim 5, which is characterized in that the bottom temperature evaporated before described be 70~
85 DEG C, tower top temperature is 65~75 DEG C.
7. the purification process of Cineole according to claim 5, which is characterized in that the bottom temperature evaporated in described be 80~
90 DEG C, tower top temperature is 70~75 DEG C.
8. the purification process of Cineole according to claim 5, which is characterized in that the bottom temperature evaporated after described be 90~
120 DEG C, tower top temperature is 73~100 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811023603.8A CN109293671A (en) | 2018-09-04 | 2018-09-04 | A kind of purification process of Cineole |
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| CN201811023603.8A CN109293671A (en) | 2018-09-04 | 2018-09-04 | A kind of purification process of Cineole |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110066285A (en) * | 2019-04-29 | 2019-07-30 | 江西思派思香料化工有限公司 | A kind of preparation method of Cineole |
| CN111676093A (en) * | 2020-06-15 | 2020-09-18 | 江西思派思香料化工有限公司 | Copper pipe cooling method eucalyptus oil purification process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110066285A (en) * | 2019-04-29 | 2019-07-30 | 江西思派思香料化工有限公司 | A kind of preparation method of Cineole |
| CN111676093A (en) * | 2020-06-15 | 2020-09-18 | 江西思派思香料化工有限公司 | Copper pipe cooling method eucalyptus oil purification process |
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Application publication date: 20190201 |