CN105159074A - Optimization method for large-scale volatile oil extraction from medicinal materials - Google Patents
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Abstract
The invention provides an optimization method for large-scale volatile oil extraction from medicinal materials. According to the optimization method, pure volatile oil is adopted as reference, and the vapor partial pressure P1 of the pure volatile oil when the pure volatile oil is mixed with water under 100 DEG C is measured, while, in an actual extraction process, a mixture in an extraction tank is a mixture composed of ground medicinal materials and water, as a result, P1 cannot actually reflect the vapor partial pressure of the volatile oil in the actual extraction process, and therefore, the medicinal materials are ground to materials of appropriate granularity, and the ground materials are mixed with water, and then, the vapor partial pressure P2 of the pure volatile oil contained in the medicinal materials under 100 DEG C is measured; P2 can reflect the vapor partial pressure of the volatile oil in the extraction tank in the actual extraction process, and thus, P2 is adopted as a valid parameter; and the P2 is introduced to subsequent steps, and therefore, parameters such as evaporated quantity of water after optimization can be obtained. With the optimization method adopted, the yielding rate of the large-scale volatile oil extraction from the medicinal materials can be greatly improved, and the curative effect of related medicines can be improved, and the efficiency of pharmaceutical companies can be increased.
Description
Technical field
The present invention relates to the extraction field of volatile oil in Chinese medicine, the optimization method of volatile oil in a kind of extensive extraction medicinal material.
Background technology
Volatile oil is a strongest active class composition in medicinal material, and country is by " pharmacopeia " and " provisions for new drugs approval " mandatory provision, and every medicinal material containing volatile oil, unless otherwise specified, all must extract volatile oil.The fact also proves, volatile oil has good curative effect really, and the ratio that the medicine containing volatile oil component on the market accounts in Chinese patent drug is many, obtains much good repercussion.
The essential oil extraction method of States Pharmacopoeia specifications is steam distillation, pharmacy corporation is all make in this way when industrial-scale extracts, mainly comprise the steps: to put into extractor by after pulverizing medicinal materials to be extracted, in extractor, put into a certain amount of water, then adopt firing equipment to heat extractor.Volatile oil component meeting stripping after heating in medicinal material, and taken away extractor by adding thermogenetic steam, input to condenser through outlet conduit and carry out condensation, obtain the oil water mixture of volatile oil and water composition.Then, this oil water mixture input oily water separating equipment is separated.
The ubiquitous problem of said extracted method be hardware device used not through Parameters Optimal Design to adapt to the extraction of different medicinal material.Specifically, in said extracted method, caliber, these parameters of condenser heat interchanging area of the amount added water in extractor, the power of firing equipment, outlet conduit all do not have the medicinal material for extracting to be optimized.Such as add the volume of amount depending on extractor of the water of extractor, instead of determine for the oleaginousness in the medicinal material that will extract, too much water not only can not increase the yield of volatile oil, also can reduce loss and the serviceable life of firing equipment on the contrary; Outlet conduit, condenser are all adopt the equipment meeting commercial production safety requirements, and are not optimized the heat interchanging area of caliber, condenser, make it adapt to specific medicinal material.Which results in large-scale production the effect extracting volatile oil unsatisfactory, the aqua aromatica of most of medicinal material can only be collected, can not receive volatile oil; Or some medicinal material can receive a small amount of oil, but oil-collecting ratio is well below laboratory yield.
Therefore, optimize Extraction Process of Volatile Oil, to improve volatile oil large-scale production yield, tool is of great significance.
In view of this, special proposition the present invention.
Summary of the invention
A kind of industrialization is the object of the present invention is to provide to extract the optimization method of volatile oil in medicinal material on a large scale, for dissimilar medicinal material, by the optimization to evaporated quantity of water, heating power, condenser heat interchanging area, these parameters of oil and water separation temperature, the recovery rate of volatile oil is improved greatly.
In order to realize above-mentioned purpose of the present invention, spy by the following technical solutions:
In extensive extraction medicinal material, an optimization method for volatile oil, comprises the steps:
(1) get volatile oil and water is mixed into first kind potpourri, measure the vapor partial pressure P of volatile oil at 100 DEG C in described first kind potpourri
1;
(2) by total oil content amount with the identical pulverizing medicinal materials of volatile oil volume in (1), add in the water of same volume and be mixed into Equations of The Second Kind potpourri, measure the volatile oil that contains in the medicinal material in described Equations of The Second Kind potpourri at the vapor partial pressure P of 100 DEG C
2;
(3) if P
2: P
1be not 0.5 ~ 1, then re-start step (2), now, before the granularity of pulverizing medicinal materials is less than once; Until P
2: P
1be 0.5 ~ 1.
(4) set up the computation model of evaporated quantity of water Z in leaching process, be specially:
p in formula
0for the saturated vapor pressure of water at 100 DEG C, C is the content of volatile oil in medicinal material, and ρ is the density of volatile oil, and m is the quality of medicinal material, and unit is followed successively by KPa, mL/g, g/mL, Kg.
In optimization method provided by the present invention, first utilize pure volatile oil as reference, measure vapor partial pressure P when it mixes with water at 100 DEG C
1.But due in actual extracting process, the potpourri in extractor be pulverize after medicinal material and water composition potpourri, therefore, P
1truly cannot reflect the vapor partial pressure of volatile oil in actual extracting process.Given this, by the granularity that pulverizing medicinal materials is extremely suitable in the present invention, after mixing with water, measure the vapor partial pressure P of volatile oil at 100 DEG C contained in medicinal material
2.P
2reflect the vapor partial pressure of volatile oil in extractor in actual extracting process, therefore, in the present invention, adopt P
2as actual parameter, substitute in subsequent step with this parameters such as drawing the evaporated quantity of water after optimization.
The computation model of the evaporated quantity of water after a kind of how calculation optimization is additionally provided in optimization method of the present invention.For different medicinal materials, calculate the evaporated quantity of water after optimization by this computation model, using this numerical value as with reference to value, in actual extracting process, water added in extractor is equal to or greater than this numerical value.
Preferably, comprise the steps: in optimization method provided by the present invention
Set up the computation model of firing equipment power K in leaching process, be specially:
in formula, 1.6 is power conversion coefficient, and t is extraction time, and unit is followed successively by Kgh/KW, h.
Preferably, comprise the steps: in optimization method provided by the present invention
Set up the computation model of the heat interchanging area S of condenser in leaching process, be specially:
in formula, 2500 is heat interchanging area reduction coefficient, Δ T
mfor the condenser thermal transfer temperature difference, unit is followed successively by W/m
2dEG C, DEG C.
Preferably, comprise the steps: in optimization method provided by the present invention
Set up the computation model of leaching process middle outlet pipe radius R, be specially:
in formula, ν is steam flow rate in pipeline, ρ
mfor the density of steam in pipeline, unit is followed successively by m/s, Kg/m
3.
Preferably, in step (1), described P
1mensuration specifically comprise the steps:
Described first kind potpourri is heated to 100 DEG C distill; Collect the water and volatile oil that distill, volume is recorded as V respectively
1 waterand V
1 oil; Described
Preferably, in step (2), described P
2mensuration specifically comprise the steps:
Described Equations of The Second Kind potpourri is heated to 100 DEG C distill; Collect the water and volatile oil that distill, volume is recorded as V respectively
2 waterand V
2 oil; Described
Preferably, described optimization method also comprises the steps:
Measure the separation time T of oil water mixture at 20-75 DEG C of 1-10mL volatile oil and 100-200mL water composition
x; Measure volatile oil and the density difference ρ of water at 20-75 DEG C
y; And according to T
xand ρ
ydetermine the optimum temperature of oil and water separation.
Preferably, described T
xmensuration specifically comprise the steps:
Get volatile oil 1 ~ 10mL, add in 100 ~ 200mL water, form oil water mixture; After oil water mixture is stirred 5 ~ 6 minutes, put into water bath device; Bath temperature is 20-75 DEG C, from low to high, measures the time required for described oil water mixture layering every 5 DEG C.
Preferably, described ρ
ymensuration specifically comprise the steps:
Get the pycnometer two of same volume, fill volatile oil by a pycnometer, in another, fill water; After two pycnometers are put into water bath heating device heating more than 5 minutes, rear taking-up is also dried outside pycnometer, weighs its quality respectively, and bath temperature is selected from 20-75 DEG C, from low to high, does once every 5 DEG C; Substitute into
m in formula
oil yrefer to the quality that the pycnometer of volatile oil is housed at a certain temperature, m
water yrefer to the quality that the pycnometer of water is housed at the same temperature, V
bottlefor the volume of pycnometer, unit is followed successively by g, g, mL.
It is further preferably, described that two pycnometers to be put into the time that water bath heating device heats be 15-20 minute.
Compared with prior art, beneficial effect of the present invention is:
Provide the optimization method that the volatile oil in medicinal material is extracted in a kind of industrialization on a large scale, for dissimilar medicinal material, by the optimization to evaporated quantity of water, heating power, condenser heat interchanging area, these parameters of oil and water separation temperature, the recovery rate of volatile oil is improved greatly.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below.
The installation drawing of Fig. 1 for using when the embodiment of the present invention carries out distillation procedure.
Embodiment
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but it will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting the scope of the invention.Unreceipted actual conditions person in embodiment, the condition of conveniently conditioned disjunction manufacturer suggestion is carried out.Agents useful for same or the unreceipted production firm person of instrument, be and can buy by commercially available the conventional products obtained.
Embodiment 1
The present embodiment provides the optimization method of the volatile oil in a kind of extensive extraction Chinese cassia tree, specifically comprises the steps:
The vapour pressure P of the volatile oil contained in Chinese cassia tree is measured according to the experimental provision in Fig. 1
1.1 is round-bottomed flask, during experiment, is put into by the first kind potpourri that volatile oil and water form and wherein heats; 2 is condenser pipe, during experiment, connects current and carries out condensation; 3 is volatile oil graduated tube; 4 is receiving bottle.
Volatile oil 2.4mL in the Chinese cassia tree of extract laboratory puts into round-bottomed flask 1 (specification of round-bottomed flask 1 is 1000mL), and the 600mL that adds water mixes, and carries out heating water bath after putting into zeolite to it, and the temperature controlling heating water bath is 100 DEG C.In still-process, when collecting 100mL moisture, record the volume of the volatile oil collected in now volatile oil graduated tube 3.Record like this three times.Calculate when evaporating 100mL moisture, the volume averaging of the volatile oil evaporated is: 0.3mL.Then, P
1=(101.74KPa × 0.30)/100=0.30522KPa.(101.74KPa is the saturated vapor pressure of water at 100 DEG C).
In Chinese cassia tree, the content measuring value of volatile oil is 1.2% (1.2% content representing volatile oil in every g Chinese cassia tree is 0.012mL), and therefore take 200g Chinese cassia tree, then the content of the volatile oil contained in the 200g Chinese cassia tree taken is 2.4mL.
200g Chinese cassia tree is pulverized, uses the comminutor that mesh size is 5mm to control grinding particle size.The device that Chinese cassia tree after pulverizing puts into Fig. 1 is distilled, measures P
2.Concrete distillating method is identical with above-mentioned determination of volatile oil method.Then, P
2=(101.74KPa × 0.21)/100=0.213654KPa.
P
2: P
1equal 0.7, be greater than 0.5, therefore, by P
2substitute in following computation model, draw the evaporated quantity of water after optimization
Embodiment 2
Based on above-described embodiment, the present invention has also done following improvement:
In actual extracting process, if 12 hours will be set to extraction time, the evaporated quantity of water Z calculated in embodiment 1 will be substituted in following computation model, draw the firing equipment power after optimization
In actual extracting process, if the heat transfer temperature difference of condenser used is 20 DEG C, the firing equipment power drawn by above-mentioned computation model substitutes in following computation model, draws the condenser heat interchanging area after optimization
then in actual extracting process, the extraction for volatile oil in Chinese cassia tree selects heat interchanging area to be 1.2m
2condenser.
Inquiry saturated vapor table (being as the criterion with pressure) can be found out, when pressure is 100KPa, vapour density is 0.5896kg/m
3, when pressure is 120KPa, vapour density is 0.6978kg/m
3.And in actual extracting process, the actual pressure of water vapour is still slightly larger than 100KPa, therefore, getting vapour density in pipeline is 0.6kg/m
3.Estimate that extraction time is 12 hours, and in pipeline, steam flow rate gets 15m/s.Data are substituted in following computation model, draws the pipe radius after optimization
Embodiment 3
On the basis of embodiment 2, the present invention has also done following improvement:
Get the volatile oil 1mL extracted in Chinese cassia tree, add in 100mL water, form oil water mixture; After oil water mixture being stirred 6 minutes, put into water bath device; Bath temperature is 20-75 DEG C, from low to high, measures the time required for described oil water mixture layering every 5 DEG C.
Get the pycnometer two of 10mL, fill volatile oil by a pycnometer, in another, fill water; After two pycnometers are put into water bath heating device heating more than 15 minutes, rear taking-up is also dried outside pycnometer, weighs its quality respectively, and bath temperature is selected from 20-75 DEG C, from low to high, does once every 5 DEG C; Substitute into
m in formula
oil yrefer to the quality that the pycnometer of volatile oil is housed at a certain temperature, m
water yrefer to the quality that the pycnometer of water is housed at the same temperature, V
bottlefor the volume of pycnometer, unit is followed successively by g, g, mL.Its testing result is as shown in table 1.
The testing result of table 1 Cortex Cinnamomi volatile oil density difference and separation time
As can be seen from separation time, the density difference of separation time and oil has very strong correlativity, and the density of volatile oil and water is more close, time required for layering longer.After casting aside the impact of density difference, temperature is higher substantially, and profit layering is easier.Therefore, in actual extracting process, select separation time little, the large corresponding temperature of density difference is the optimum temperature of oil and water separation.As can be seen from Table 1, when extracting the volatile oil in Chinese cassia tree, the optimum temperature of oil and water separation is 30 ~ 35 DEG C.
Experimental example 4
The content that can record Extracting Oil of Radix Angelica Sinensis according to the heavy oil determination method in " pharmacopeia " determination of volatile oil method is 0.4% ~ 0.6% (namely representing the volatile oil that can extract 0.004-0.006mL in every g Radix Angelicae Sinensis).
Extracting method before optimization: angelica sinensis 200kg, after coarse crushing, add in 3 cubic metres of extractors, add water 1.2 tons, exit duct diameter 133 millimeters, join horizontal tubular heat exchanger one, heat interchanging area 15 square metres, tube exchanger one, heat interchanging area 1 square metre, join oil-water separator one, heating extraction 20 hours, collects essential oil.Result can not receive volatile oil, can only receive aqua aromatica, so that this medicine can not produce listing.
Optimization method:
Volatile oil 1mL in the Radix Angelicae Sinensis extract laboratory puts into round-bottomed flask 1 (specification of round-bottomed flask 1 is 1000mL), and the 600mL that adds water mixes, and carries out heating water bath after putting into zeolite to it, and the temperature controlling heating water bath is 100 DEG C.In still-process, due to the volatile oil in Radix Angelicae Sinensis very little, not easily collecting, therefore when collecting 300mL moisture, records the volume of the volatile oil collected in now volatile oil graduated tube 3.Record like this three times, measure when evaporating 300mL moisture, the volume averaging of the volatile oil evaporated is: 0.15mL.Then,
Content because of the volatile oil in Radix Angelicae Sinensis is 0.4% ~ 0.6%, therefore takes angelica sinensis 250g, guarantees that the content of volatile oil in 250 Radix Angelicae Sinensis Tabellaes taken is 1mL.Then, 250g angelica sinensis is pulverized, use the comminutor that mesh size is 5mm to control grinding particle size.The device that Radix Angelicae Sinensis after pulverizing puts into Fig. 1 is equally distilled, measures vapour pressure P actual in medicinal material extract process
2.Concrete assay method is identical with above-mentioned determination of volatile oil method.When 300mL water is often collected in detection, the average external volume collecting volatile oil is 0.10mL.Then,
By relatively finding out, P
2: P
1be 0.67, be greater than 0.5, now, illustrate that the granularity of pulverizing medicinal materials is relatively more reasonable, can by P
2substitute in subsequent step as valid data.
Volatile oil in preextraction 200kg Radix Angelicae Sinensis.Now, Extracting Oil of Radix Angelica Sinensis containing measuring maximal value: 0.6%, i.e. 0.006mL/g.The density of the volatile oil in Radix Angelicae Sinensis is 1g/mL.Then, computation model is passed through
evaporated quantity of water can be drawn
Then in actual extracting process, the water yield added in extractor is 3640kg.
If 12 hours will be set to extraction time, then according to computation model
the firing equipment power after optimization can be drawn
In actual extracting process, if the heat transfer temperature difference of condenser used is 20 DEG C, according to computation model
the condenser heat interchanging area after optimization can be drawn
then in actual extracting process, the extraction for Extracting Oil of Radix Angelica Sinensis selects heat interchanging area to be 4m
2condenser.
Inquiry saturated vapor table (being as the criterion with pressure) can be found out, when pressure is 100KPa, vapour density is 0.5896kg/m
3, when pressure is 120KPa, vapour density is 0.6978kg/m
3.And in actual extracting process, the actual pressure of water vapour is still slightly larger than 100KPa, therefore, getting vapour density in pipeline is 0.6kg/m
3.Estimate that extraction time is 12 hours, and in pipeline, steam flow rate gets 15m/s.Data are substituted in following computation model, draws the pipe radius after optimization
Finally, optimize the optimal separation temperature that volatile oil is separated with water, specifically comprise the steps:
Get the volatile oil 1mL extracted in Radix Angelicae Sinensis, add in 100mL water, form oil water mixture; After oil water mixture being stirred 6 minutes, put into water bath device; Bath temperature is 20-75 DEG C, from low to high, measures the time required for described oil water mixture layering every 5 DEG C.
Get the pycnometer two of 10mL, fill volatile oil by a pycnometer, in another, fill water; After two pycnometers are put into water bath heating device heating more than 15 minutes, rear taking-up is also dried outside pycnometer, weighs its quality respectively, and bath temperature is selected from 20-75 DEG C, from low to high, does once every 5 DEG C; Substitute into
m in formula
oil yrefer to the quality that the pycnometer of volatile oil is housed at a certain temperature, m
water yrefer to the quality that the pycnometer of water is housed at the same temperature, V
bottlefor the volume of pycnometer, unit is followed successively by g, g, mL.Its testing result is as shown in table 2.
The testing result of table 2 Extracting Oil of Radix Angelica Sinensis density difference and separation time
As can be seen from separation time, the density difference of separation time and oil has very strong correlativity, and the density of volatile oil and water is more close, time required for layering longer.After casting aside the impact of density difference, temperature is higher substantially, and breakdown of emulsion is easier.Therefore, in actual extracting process, select separation time little, the large corresponding temperature of density difference is the optimum temperature of oil and water separation.Then as can be seen from Table 2, the optimum temperature of oil and water separation is 75 DEG C, divides light oil at this temperature, cools to 35 DEG C and is separated a heavy oil again, just can well isolate volatile oil.
Then, after above-mentioned optimization, the extraction work method after optimization is: angelica sinensis 200kg, and use mesh size is that the comminutor of 5 millimeters controls degree of grinding, and add 4 tons of water, mixing, moistens 10 ~ 14 hours.Add in 6 cubic metres of extractors, outlet inside radius is 55 millimeters, joins vertical array tubular heat interchanger one, heat interchanging area 4 square metres, after connect self-rotary oil-water separator one, connect thereafter vertical array tubular heat interchanger one again, heat interchanging area 0.5 square metre, connects thereafter filter fraction oil-water separator one again.After one-level condensation, the temperature keeping mixed liquor is 75 DEG C, after B-grade condensation, keeps mixed liquor to be 35 DEG C, extracts after 4 hours, collect the light oil in primary oil separator.After extracting 8 hours again, collect the heavy oil in every grade of oil-water separator.Merge gained essential oil, recovery rate is 0.4%.
Optimization method provided by the invention is optimized respectively the extracting method of the volatile oil in industrial extensive extraction Ligusticum wallichii, curcuma zedoary, rhizoma atractylodis, Chinese cassia tree and these medicinal materials of perilla leaf.After adopting optimization method provided by the present invention to optimize, the comparing result of its volatile oil recovery rate is as shown in table 3.
Volatile oil recovery rate comparing result before each medicinal material of table 3 is optimized and after optimizing
| Medicinal material | Volatile oil recovery rate before optimizing | Volatile oil recovery rate after optimizing |
| Ligusticum wallichii | Only aqua aromatica can be received | 0.3％ |
| Radix Angelicae Sinensis | Only aqua aromatica can be received | 0.4％ |
| Curcuma zedoary | Be less than 0.1% | Be greater than 1.5% |
| Rhizoma atractylodis | Be less than 0.1% | Be greater than 1.2% |
| Chinese cassia tree | Be less than 0.2% | Be greater than 2.0% |
| Perilla leaf | Be less than 0.2% | Be greater than 0.4% |
As can be seen from the data of experimental example 1 and table 3, the extracting method after adopting optimization method provided by the invention to optimize, the recovery rate of volatile oil all has significant raising.For Radix Angelicae Sinensis, this kind of medicinal material of Ligusticum wallichii, the extracting method before optimization only can collect aqua aromatica, and cannot receive to obtain volatile oil.After optimizing, not only can receive to obtain volatile oil, and the recovery rate of volatile oil is also considerable, in Ligustilide assay in finished dosage form, Radix Angelicae Sinensis can improve 400 times, and Ligusticum wallichii can improve 300 times.
For this kind of medicinal material of curcuma zedoary, rhizoma atractylodis, Chinese cassia tree and perilla leaf, the extracting method before optimization can receive to obtain volatile oil, but the recovery rate of volatile oil is too low.After optimizing, the recovery rate of volatile oil all has significant raising, maximumly improves more than 15 times.
Although illustrate and describe the present invention with specific embodiment, however it will be appreciated that can to make when not deviating from the spirit and scope of the present invention many other change and amendment.Therefore, this means to comprise all such changes and modifications belonged in the scope of the invention in the following claims.
Claims (10)
1. the extensive optimization method extracting volatile oil in medicinal material, is characterized in that, comprise the steps:
(1) get volatile oil and water is mixed into first kind potpourri, measure the vapor partial pressure P of volatile oil at 100 DEG C in described first kind potpourri
1;
(2) by total oil content amount with the identical pulverizing medicinal materials of volatile oil volume in (1), add in the water of same volume and be mixed into Equations of The Second Kind potpourri, measure the volatile oil that contains in the medicinal material in described Equations of The Second Kind potpourri at the vapor partial pressure P of 100 DEG C
2;
(3) if P
2: P
1be not 0.5 ~ 1, then re-start step (2), now, before the granularity of pulverizing medicinal materials is less than once; Until P
2: P
1be 0.5 ~ 1;
(4) set up the computation model of evaporated quantity of water Z in leaching process, be specially:
p in formula
0for the saturated vapor pressure of water at 100 DEG C, C is the content of volatile oil in medicinal material, and ρ is the density of volatile oil, and m is the quality of medicinal material, and unit is followed successively by KPa, mL/g, g/mL, Kg.
2. optimization method according to claim 1, is characterized in that, also comprises the steps:
Set up the computation model of firing equipment power K in leaching process, be specially:
in formula, 1.6 is power conversion coefficient, and t is extraction time, and unit is followed successively by Kgh/KW, h.
3. optimization method according to claim 1, is characterized in that, also comprises the steps:
Set up the computation model of the heat interchanging area S of condenser in leaching process, be specially:
in formula, 2500 is heat interchanging area reduction coefficient, Δ T
mfor the condenser thermal transfer temperature difference, unit is followed successively by W/m
2dEG C, DEG C.
4. optimization method according to claim 1, is characterized in that, also comprises the steps:
Set up the computation model of leaching process middle outlet pipe radius R, be specially:
in formula, ν is steam flow rate in pipeline, ρ
mfor the density of steam in pipeline, unit is followed successively by m/s, Kg/m
3.
5. optimization method according to claim 1, is characterized in that, in step (1), and described P
1mensuration specifically comprise the steps:
Described first kind potpourri is heated to 100 DEG C distill; Collect the water and volatile oil that distill, volume is recorded as V respectively
1 waterand V
1 oil; Described
6. optimization method according to claim 1, is characterized in that, in step (2), and described P
2mensuration specifically comprise the steps:
Described Equations of The Second Kind potpourri is heated to 100 DEG C distill; Collect the water and volatile oil that distill, volume is recorded as V respectively
2 waterand V
2 oil; Described
7. optimization method according to claim 1, is characterized in that, described optimization method also comprises the steps:
Measure the separation time T of oil water mixture at 20-75 DEG C of 1-10mL volatile oil and 100-200mL water composition
x; Measure volatile oil and the density difference ρ of water at 20-75 DEG C
y; And according to T
xand ρ
ydetermine the optimum temperature of oil and water separation.
8. optimization method according to claim 7, is characterized in that, described T
xmensuration specifically comprise the steps:
Get volatile oil 1 ~ 10mL, add in 100 ~ 200mL water, form oil water mixture; After oil water mixture is stirred 5 ~ 6 minutes, put into water bath device; Bath temperature is 20-75 DEG C, from low to high, measures the time required for described oil water mixture layering every 5 DEG C.
9. optimization method according to claim 7, is characterized in that, described ρ
ymensuration specifically comprise the steps:
Get the pycnometer two of same volume, fill volatile oil by a pycnometer, in another, fill water; After two pycnometers are put into water bath heating device heating more than 5 minutes, rear taking-up is also dried outside pycnometer, weighs its quality respectively, and bath temperature is selected from 20-75 DEG C, from low to high, does once every 5 DEG C; Substitute into
m in formula
oil yrefer to the quality that the pycnometer of volatile oil is housed at a certain temperature, m
water yrefer to the quality that the pycnometer of water is housed at the same temperature, V
bottlefor the volume of pycnometer, unit is followed successively by g, g, mL.
10. optimization method according to claim 9, is characterized in that, described two pycnometers to be put into the time that water bath heating device heats be 15-20 minute.
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