CN114292702B - Method for extracting peony essential oil by using surfactant aqueous solution and solid alkali - Google Patents
Method for extracting peony essential oil by using surfactant aqueous solution and solid alkali Download PDFInfo
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Abstract
The invention belongs to the technical field of extraction of plant essential oil, and particularly discloses a method for extracting peony essential oil by using a surfactant aqueous solution and solid alkali. According to the invention, peony petals are added into an aqueous solution compounded by three surfactants for pulping, then solid alkali is added and stirred uniformly to obtain mixed slurry, and the peony essential oil is extracted by adopting a solvent reflux extraction mode, so that the prepared peony essential oil is clear and transparent, has pure fragrance, and the extraction rate of the essential oil is as high as 1.152 per mill. According to the invention, the solubilization of the essential oil in the wall breaking process is promoted, the emulsification process of the peony essential oil is enhanced, and the content of the peony essential oil dispersed in the extractant is greatly improved by utilizing the synergistic effect of the three surfactants and the solid alkali which is convenient for safe operation at room temperature; and the extraction process is simple, convenient and safe, and the material cost is low.
Description
Technical Field
The invention belongs to the technical field of extraction of plant essential oil, and particularly discloses a method for extracting peony essential oil by using a surfactant aqueous solution and solid alkali.
Background
The plant essential oils, known as volatile oils in the chemical and pharmaceutical fields, and the essential oils in the plant field. Since ancient times, through long-term medical practice, it has been found that plant essential oils have many medicinal values, such as pharmacological activities of eliminating phlegm, relieving cough, relieving asthma, dispelling wind, invigorating stomach, relieving fever, easing pain, resisting bacteria, diminishing inflammation, and the like. The peony flower contains rich flavonoid, essential oil, phenolic substances and the like, and has stronger capability of scavenging free radicals. Therefore, if the effect of the peony is fully utilized, the industrialized production of the peony essential oil can be realized, and the comprehensive utilization of the peony can be realized. The literature shows that the peony flower essential oil also contains unique functional components such as synephrine, caryophyllin, myristicin and the like, which plays an important role in improving the efficacy of the peony essential oil.
At present, the method applied to extracting the peony essential oil mainly comprises a steam distillation method and supercritical CO 2 The extraction method, solvent extraction, molecular distillation and other separation and purification means have the defects of low extraction rate, long extraction time, expensive extraction equipment and the like, so that the essential oil cannot fully exert the effect, the price of the essential oil is high, and the application range of the essential oil is limited. If the cell walls of peony petal cells can be sufficiently broken, the content of the peony petal cells can be oozed after wall breaking, and the essential oil components of the peony petal cells can be obtained. Many methods for breaking cell wall include enzymatic method, chemical method, physical method or a combination of these methods. Therefore, a method for extracting the peony essential oil, which has the advantages of high extraction rate, safety, high efficiency, low cost and wide application range, needs to be explored.
Disclosure of Invention
Aiming at the problems and the defects existing in the prior art, the invention aims to provide a method for extracting peony essential oil by utilizing a surfactant aqueous solution and solid alkali.
In order to achieve the aim of the invention, the technical scheme adopted by the invention is as follows:
the invention provides a method for extracting peony essential oil by utilizing a surfactant aqueous solution and solid alkali, which comprises the following steps:
(1) Mixing 1 part by weight of peony petals with 2.5-3 parts by weight of active water, and pulping to obtain a pulping mixture; the active water is an aqueous solution of a surfactant;
(2) Adding solid alkali into the beating mixture, supplementing water, uniformly stirring, and standing to obtain mixed slurry;
(3) Transferring the extractant and the mixed slurry prepared in the step (2) into a reflux kettle for solvent reflux extraction, collecting reflux liquid and performing post-treatment to obtain the peony essential oil.
Preferably, the surfactant is a combination of propylene glycol random polyether PPE-1500, triton X-100 and dodecyltrimethylammonium chloride; the propylene glycol random polyether PPE-1500 accounts for 65-80% of the weight of the composition, the triton X-100 accounts for 10-20% of the weight of the composition, and the dodecyl trimethyl ammonium chloride accounts for 10-20% of the weight of the composition.
Preferably, the mass percentage of the surfactant in the active water is 0.8-1.6%.
Preferably, in the step (2), the solid alkali is formed by mixing and calcining alkaline precipitates of calcium and magnesium ions and graphite powder, and the preparation method comprises the following steps: adding water into magnesium chloride and calcium chloride to prepare a solution, adding graphite powder, uniformly stirring, then dropwise adding alkali solution while stirring to adjust the pH value to 11-12 for precipitation, and filtering to separate a precipitate; washing and drying the precipitate, and then placing the precipitate in a muffle furnace to calcine for 36-48 h at 800-900 ℃ to obtain the solid alkali.
Preferably, the molar ratio of the magnesium chloride to the calcium chloride is (1.2-2.2) to 1. More preferably, the molar ratio of the magnesium chloride to the calcium chloride is (1.6-2) to 1.
Preferably, the weight ratio of the graphite powder to the calcium chloride is (3.5-4.5) to 1.
Further, when magnesium chloride and calcium chloride are added with water to prepare a solution, the addition amount of the water is 8-12 times of the weight of the calcium chloride.
Preferably, in the step (2), the solid base is used in an amount of 0.08 to 0.16 parts by weight.
Preferably, the specific operation of the solvent reflux extraction in the step (3) is as follows: stirring and heating the reflux kettle to 50-60 ℃ within 30-45 min, and preserving heat for 100-120 min; continuously stirring and heating for 30-40 min, heating to reflux temperature, and refluxing for 3-5 h; and after the reflux is finished, collecting reflux liquid, filtering, separating the liquid to obtain an organic layer, drying, and evaporating the solvent to obtain the peony essential oil.
Preferably, the extractant is a mixture of n-hexane and petroleum ether with the volume ratio of (0.1-0.15) to 1; the dosage of the extractant is as follows: every 1kg of peony petals uses 6-8L of extractant.
Preferably, in step (3), the solvent is removed, in particular by a post-treatment step comprising: filtering the collected reflux liquid, and separating the liquid to obtain an organic layer; adding anhydrous sodium sulfate or magnesium sulfate as desiccant into the organic layer, sealing and drying overnight, and removing the desiccant after drying; vacuum pumping with water pump or oil pump at below 40deg.C, vacuum degree of about 0.02-0.1 Pa, rotary evaporating, concentrating to remove extractant to obtain flos moutan essential oil.
Preferably, in the step (1), the particle size of the beating mixture is 100 mesh or less.
Preferably, the graphite powder used in the preparation of the solid base has a particle size of preferably 100 mesh or less.
More preferably, the peony petals are preferably fresh peony petals picked at 6 to 10 am and 4 to 7 pm, and half-cut is preferred. The petals are fresh and free of insect damage, and are washed by water before use, and the water is naturally drained or is dried by a low-speed rotary net drum.
More preferably, the water is deionized water.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the permeation, emulsification and solubilization effects of the compound surfactant are combined with the wall breaking effects of solid alkali and mechanical force, so that the leaching amount of the essential oil in the peony petal cells is increased, and then the peony essential oil is extracted by adopting a solvent reflux extraction mode, so that the extraction rate of the peony essential oil is improved.
(2) The invention adopts ternary compound surfactant, wherein dodecyl trimethyl ammonium chloride belongs to quaternary ammonium salt cationic surfactant, and the hydrophilic property and the strong polarity of the ternary compound surfactant can dissolve plant cell walls, destroy a network structure consisting of cellulose in plant cells and improve the exudation efficiency of essential oil substances. In addition, the dodecyl trimethyl ammonium chloride is combined with the propylene glycol random polyether PPE-1500 to have good low foaming property and emulsification effect, and the triton X-100 has good high temperature resistance and is easy to combine with a biological film to enhance the wall breaking property, so that the ternary compound surfactant can promote the release of volatile oil in plant cells in an alkaline environment, improve the extraction rate of peony essential oil, and realize the synergistic efficient, safe and controllable extraction process.
(3) The solid alkali is used in the peony essential oil extraction process, so that not only can the cell barrier be destroyed, but also the solid alkali can be adsorbed in water in a carrier mode and the essential oil is transferred, and the extraction rate of the peony essential oil is greatly improved. In the wall breaking process, on one hand, the wall is broken mechanically by beating; on the other hand, the method utilizes the characteristics of safety and easy operation of solid alkali at normal temperature and alkali enhancement under heating condition, further enhances the wall breaking effect during wall breaking, and is more beneficial to the next distillation extraction. In addition, although the traditional alkali liquor can also improve the extraction rate of the peony essential oil, the safety is far less than that of the alkali liquor. Meanwhile, the preparation process of the solid alkali is simple, the operation is easier, the advantages of small dosage and cost control are achieved, and the dosage of the subsequent extractant is reduced.
Detailed Description
The present invention will be further described in detail with reference to the following examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present application will be described in detail with reference to examples.
Example 1: preparing solid alkali with different proportions
Adding 10 times of water into magnesium chloride and calcium chloride, stirring uniformly to prepare an aqueous solution; adding graphite powder (sieving with 100 mesh sieve) and stirring; then, dropwise adding an alkaline solution (NaOH solution with the mass fraction of 10%) while stirring to adjust the pH value to 12 for precipitation, and filtering to separate a precipitate; washing the precipitate with deionized water, airing, and then placing the precipitate in a muffle furnace for calcination at 900 ℃ for 36h to obtain the solid alkali.
The amounts of magnesium chloride, calcium chloride, water and graphite powder are shown in Table 1.
TABLE 1 preparation of the amounts of the components of the solid base
| Sample numbering | Magnesium chloride (hexahydrate) | Calcium chloride | Graphite powder |
| Solid base 1 | — | 111g | 444g |
| Solid base 2 | 203g | — | 444g |
| Solid base 3 | 203g | 111g | 444g |
| Solid base 4 | 243.6g | 111g | 444g |
| Solid base 5 | 284.2g | 111g | 444g |
| Solid base 6 | 324.8g | 111g | 444g |
| Solid base 7 | 365.4g | 111g | 444g |
| Solid base 8 | 406g | 111g | 444g |
| Solid base 9 | 446.6g | 111g | 444g |
| Solid base 10 | 487.2g | 111g | 444g |
Example 2: influence of solid alkali with different proportions on extraction rate of essential oil
The peony essential oil was extracted by referring to the following procedure, and the effects of different conditions such as no alkali (blank) and different solid alkali (test) prepared in example 1 on the extraction rate of the peony essential oil were compared with those of the test examples.
The blank example extraction steps are as follows:
(1) Taking 1kg of peony petals, adding 3kg of water, mixing, and pulping to obtain a pulping mixture; standing for 3h.
(2) Transferring 8L of extractant (volume ratio of n-hexane to petroleum ether is 0.1:1) and the beating mixture into a reflux kettle for solvent reflux extraction: heating in a water bath under stirring within 45min to heat the reflux kettle to 50 ℃, and preserving heat for 120min; continuously stirring and heating for 40min, heating to reflux temperature, and refluxing for 5h; the distilled steam flows back to the reflux kettle after being condensed by a condensing system; and collecting reflux liquid after the reflux is finished, filtering, separating to obtain an organic layer, adding enough anhydrous sodium sulfate serving as a drying agent into the organic layer, sealing and drying overnight, removing the drying agent after the drying is finished, vacuumizing by a water pump or an oil pump at the temperature of below 40 ℃ to the vacuum degree of about 0.02-0.1 Pa, and removing the extracting agent by rotary evaporation to obtain the peony essential oil with the extraction rate of 0.503 per mill. The extraction rate calculation formula of the peony essential oil is as follows: the weight of the essential oil/the weight of the fresh peony flower is multiplied by 100 percent.
The extraction steps of the test example are as follows:
(1) Taking 1kg of peony petals, adding 3kg of water, mixing, and pulping to obtain a pulping mixture;
(2) Adding solid alkali into the beating mixture, uniformly stirring, and standing for 3 hours to obtain mixed slurry;
(3) Transferring 8L of extractant (the volume ratio of n-hexane to petroleum ether is 0.1:1) and the mixed slurry prepared in the step (2) into a reflux kettle, and carrying out solvent reflux extraction: heating in a water bath under stirring within 45min to heat the reflux kettle to 50 ℃, and preserving heat for 120min; continuously stirring and heating for 40min, heating to reflux temperature, and refluxing for 5h; the distilled steam enters a reflux kettle after being condensed by a condensing system and flows back to the reflux kettle; collecting reflux liquid after reflux, filtering, separating to obtain an organic layer, adding enough anhydrous sodium sulfate as a drying agent into the organic layer, sealing and drying overnight, removing the drying agent after drying, vacuumizing with a water pump or an oil pump at 40 ℃ or below, and removing the extracting agent by rotary evaporation to obtain the peony essential oil with the extraction rate shown in table 2.
TABLE 2 use of alkali in test examples 1 to 10 and extraction yield of peony essential oil
| Test number | Alkali | Alkali dosage | Essential oil extraction yield (mill) |
| Test example 1 | Solid base 1 | 100g | 0.523 |
| Test example 2 | Solid base 2 | 100g | 0.533 |
| Test example 3 | Solid base 3 | 100g | 0.546 |
| Test example 4 | Solid base 4 | 100g | 0.712 |
| Test example 5 | Solid base 5 | 100g | 0.737 |
| Test example 6 | Solid base 6 | 100g | 0.769 |
| Test example 7 | Solid base 7 | 100g | 0.816 |
| Test example 8 | Solid base 8 | 100g | 0.797 |
| Test example 9 | Solid base 9 | 100g | 0.733 |
| Test example 10 | Solid base 10 | 100g | 0.535 |
As is clear from Table 2, the use of calcium chloride or magnesium chloride alone to prepare solid base and to extract peony essential oil results in a worse extraction rate than when complex solid base is used. Moreover, the extraction rate of the peony essential oil in comparative test examples 1 to 10 can be seen that the extraction rate of the peony essential oil is obviously improved along with the improvement of the specific gravity of magnesium chloride; when the molar ratio of the magnesium chloride to the magnesium chloride reaches 1.8:1, the specific gravity of the magnesium chloride is continuously increased, the effect of improving the extraction rate is weakened, and particularly when the molar ratio reaches 2.2, the extraction rate even has a remarkable decline trend. This is probably because, in the extraction of peony essential oil, the solid alkali provides a carrier equivalent to an interface reaction in the distillation process in addition to alkalinity, and serves as a transit aid for separating essential oil, which has a significant relationship with the microscopic interface structure of the solid alkali composed of magnesium and calcium atoms. The peony essential oil has complex components, and the effect on the essential oil compound is not comprehensive by using composite solid alkali due to the single magnesium or calcium solid alkali, so that the distillation efficiency of part of essential oil molecules is lower.
Based on this, the molar ratio of magnesium chloride to calcium chloride in the present invention is preferably controlled to be (1.2 to 2.2) to 1, preferably (1.6 to 2) to 1.
Example 3: influence of surfactants with different proportions on extraction rate of essential oil
Extracting peony essential oil by referring to the following method:
(1) Taking 1kg of peony petals, adding 3kg of active water, mixing, and pulping to obtain a pulping mixture; the active water is an aqueous solution of a surfactant;
(2) Adding 100g of solid alkali 7 into the beating mixture, uniformly stirring, and standing for 3 hours to obtain mixed slurry;
(3) Transferring 8L of extractant (the volume ratio of n-hexane to petroleum ether is 0.1:1) and the mixed slurry prepared in the step (2) into a reflux kettle, and carrying out solvent reflux extraction: heating in a water bath under stirring within 45min to heat the reflux kettle to 50 ℃, and preserving heat for 120min; continuously stirring and heating for 40min, heating to reflux temperature, and refluxing for 5h; condensing the distilled steam by a condensing system, flowing back to a reflux kettle, collecting reflux liquid after the reflux is finished, filtering, separating to obtain an organic layer, adding a sufficient amount of anhydrous sodium sulfate as a drying agent into the organic layer, sealing and drying overnight, removing the drying agent after the drying is finished, vacuumizing by a water pump or an oil pump at the temperature below 40 ℃ to the vacuum degree of about 0.02-0.1 Pa, and removing the extracting agent by rotary evaporation to obtain the peony essential oil, wherein the extraction rate is shown in table 3.
Different surfactants were formulated according to table 3 and tested according to the procedure described above, with test designations in order: examples 3-1 to 3-9, the effect of different surfactants on the extraction yield of essential oils was compared. In examples 3-1 to 3-9, the total concentration of the surfactant in the active water was 1.3% (mass percentage).
TABLE 3 Effect of surfactant ratios on essential oil extraction yield
| Numbering device | Propylene glycol random polyether PPE-1500 | Triton X-100 | Dodecyl trimethyl ammonium chloride | Essential oil extraction yield (mill) |
| Example 3-1 | 100％ | — | — | 0.632 |
| Example 3-2 | — | 100％ | — | 0.615 |
| Examples 3 to 3 | — | — | 100％ | 0.606 |
| Examples 3 to 4 | 80％ | 10％ | 10％ | 0.869 |
| Examples 3 to 5 | 75％ | 10％ | 15％ | 0.892 |
| Examples 3 to 6 | 70％ | 15％ | 15％ | 0.912 |
| Examples 3 to 7 | 65％ | 20％ | 15％ | 0.886 |
| Examples 3 to 8 | 65％ | 15％ | 20％ | 0.837 |
| Examples 3 to 9 | 71％ | 17％ | 12％ | 0.937 |
As can be seen from table 3, when the active water is prepared by using the surfactant with a single component, the extraction rate of the essential oil is not high as that of the compound surfactant, and the extraction rate is lower when the active water is prepared by using the dodecyl trimethyl ammonium chloride alone than when the other two surfactants are used alone. This is because dodecyl trimethyl ammonium chloride has hydrophilicity and strong polarity, and has the strongest action of dissolving plant cell walls among three surfactant components, and can destroy the cell fiber network structure; however, since the surfactant itself is an ionic surfactant, an increased amount of the surfactant will produce a large amount of "foam" which will adversely affect distillation. Therefore, the extraction rate of the peony essential oil is reduced by using the dodecyl trimethyl ammonium chloride alone, but the amplitude is not large. The propylene glycol random polyether PPE-1500 has good low-foam performance, the triton X-100 has good high-temperature resistance and is easy to combine with a biological film, and when the three surfactants are combined, the hydrophilicity, polarity, low-foam performance, high-temperature resistance and biological infiltration performance can reach an equilibrium state suitable for distilling peony flowers, so that a higher extraction rate of essential oil is obtained.
Example 4: influence of the mass percentage of the surfactant in the active water on the extraction rate of the essential oil
Extracting peony essential oil by referring to the following method:
(1) Taking 1kg of peony petals, adding 3kg of active water, mixing, and pulping to obtain a pulping mixture; as shown in Table 4, the influence of the concentration of the active water on the extraction rate of the peony essential oil is examined by setting the active water with different concentrations, and in the embodiment, the surfactant in the active water is prepared by 71% of propylene glycol random polyether PPE-1500, 17% of triton X-100 and 12% of dodecyl trimethyl ammonium chloride;
(2) Adding 100g of solid alkali 7 into the beating mixture, uniformly stirring, and standing for 3 hours to obtain mixed slurry;
(3) Transferring 8L of extractant (the volume ratio of n-hexane to petroleum ether is 0.1:1) and the mixed slurry prepared in the step (2) into a reflux kettle, and carrying out solvent reflux extraction: heating in a water bath under stirring within 45min to heat the reflux kettle to 50 ℃, and preserving heat for 120min; continuously stirring and heating for 40min, heating to reflux temperature, and refluxing for 5h; condensing the distilled steam by a condensing system, flowing back to a reflux kettle, collecting reflux liquid after the reflux is finished, filtering, separating to obtain an organic layer, adding a sufficient amount of anhydrous sodium sulfate as a drying agent into the organic layer, sealing and drying overnight, removing the drying agent after the drying is finished, vacuumizing by a water pump or an oil pump at the temperature below 40 ℃ to the vacuum degree of about 0.02-0.1 Pa, and removing the extracting agent by rotary evaporation to obtain the peony essential oil, wherein the extraction rate is shown in table 4.
TABLE 4 influence of the surfactant mass% in active Water on the extraction yield of essential oils
| Numbering device | The mass percent of the surfactant in the active water (%) | Essential oil extraction yield (mill) |
| Example 4-1 | 0.4 | 0.733 |
| Example 4-2 | 0.6 | 0.741 |
| Examples 4 to 3 | 0.8 | 0.923 |
| Examples 4 to 4 | 1.0 | 0.986 |
| Examples 4 to 5 | 1.2 | 0.972 |
| Examples 4 to 6 | 1.4 | 0.921 |
| Examples 4 to 7 | 1.6 | 0.902 |
| Examples 4 to 8 | 1.8 | 0.755 |
As shown in table 4, the extraction rate of the peony essential oil shows a tendency of increasing and then decreasing with increasing mass percentage of the surfactant, because the activity of the surfactant is enhanced with increasing addition amount of the surfactant, but a large amount of the surfactant generates more foam during pulping, which affects the next step of separation and extraction.
Example 5: influence of the amount of solid alkali on the extraction yield of essential oil
Extracting peony essential oil according to the following method:
(1) Taking 1kg of peony petals, adding 3kg of active water, mixing, and pulping to obtain a pulping mixture; the mass percentage of the surfactant in the active water is 1%, and the surfactant is prepared from 71% of propylene glycol random polyether PPE-1500, 17% of triton X-100 and 12% of dodecyl trimethyl ammonium chloride.
(2) Solid alkali 7 (specific addition amounts and corresponding example numbers are shown in table 5) with different weights is added into the beating mixture, and the mixture is stirred uniformly and then is left to stand for 3 hours, so that mixed slurry is obtained.
(3) Transferring 8L of extractant (the volume ratio of n-hexane to petroleum ether is 0.1:1) and the mixed slurry prepared in the step (2) into a reflux kettle, and carrying out solvent reflux extraction: heating in a water bath under stirring within 45min to heat the reflux kettle to 50 ℃, and preserving heat for 120min; continuously stirring and heating for 40min, heating to reflux temperature, and refluxing for 5h; condensing the distilled steam by a condensing system, flowing back to a reflux kettle, collecting reflux liquid after the reflux is finished, filtering, separating to obtain an organic layer, adding a sufficient amount of anhydrous sodium sulfate as a drying agent into the organic layer, sealing and drying overnight, removing the drying agent after the drying is finished, vacuumizing by a water pump or an oil pump at the temperature below 40 ℃ to the vacuum degree of about 0.02-0.1 Pa, and removing the extracting agent by rotary evaporation to obtain the peony essential oil, wherein the extraction rate is shown in table 5.
TABLE 5 influence of solid alkali dosage on extraction yield of essential oil
| Numbering device | Alkali dosage | Essential oil extraction yield (mill) |
| Example 5-1 | 50g | 0.703 |
| Example 5-2 | 60g | 0.811 |
| Examples 5 to 3 | 70g | 0.833 |
| Examples 5 to 4 | 80g | 0.955 |
| Examples 5 to 5 | 90g | 0.977 |
| Examples 5 to 6 | 100g | 0.986 |
| Examples 5 to 7 | 120g | 1.152 |
| Examples 5 to 8 | 140g | 1.115 |
| Examples 5 to 9 | 160g | 0.956 |
| Examples 5 to 10 | 220g | 0.801 |
As can be seen from table 5, the extraction rate of the essential oil tends to increase and decrease with the increase of the amount of the solid alkali, because the amount of the solid alkali is too small, which is difficult to promote the extraction rate of the essential oil, whereas the high-concentration alkaline environment is unfavorable for the extraction of the essential oil and causes unnecessary waste of raw materials. Test examples 5-4, 5-5, 5-6, 5-7, 5-8 and test example 5-9 have better effects, and the dosage of the solid alkali is preferably controlled to be 0.08-0.16 times of the weight of the peony petals.
Example 6
A method for extracting flos moutan essential oil by using surfactant aqueous solution and solid alkali comprises the steps of:
(1) Preparing peony petals: the petals of the fresh peony flower picked at the beginning of 6-10 am and at the end of 4-7 pm are selected, half-opened is good, the petals are fresh and free from insect damage, and the petals are washed with water before use, and the water is naturally drained or is spin-dried by a low-speed rotary net drum.
(2) Preparing solid alkali:
203g of magnesium chloride and 55.5g of calcium chloride are taken, water with the weight being 8 times that of the calcium chloride is added, and the mixture is stirred uniformly to prepare an aqueous solution; 222g of graphite powder (sieving with a 100-mesh sieve) is added and stirred uniformly; then, dropwise adding an alkaline solution (NaOH solution with the mass fraction of 10%) while stirring to adjust the pH value to 11 for precipitation, and filtering to separate a precipitate; washing the precipitate with deionized water, airing, and then placing the precipitate in a muffle furnace for calcination at 800 ℃ for 48 hours to obtain the solid alkali.
Then extracting according to the following steps:
(1) Taking 1kg of peony petals, adding 3kg of active water, mixing, pulping to obtain a pulping mixture, and sieving with a 100-mesh sieve. The active water is an aqueous solution of a surfactant, the mass percentage of the surfactant is 1%, the water is deionized water, and the surfactant is prepared from 71% of propylene glycol random polyether PPE-1500, 17% of triton X-100 and 12% of dodecyl trimethyl ammonium chloride.
(2) 150g of solid alkali is added into the beating mixture, and the mixture is stirred uniformly and then is kept stand for 3 hours to obtain mixed slurry.
(3) Transferring 6L of extractant (the volume ratio of n-hexane to petroleum ether is 0.1:1) and the mixed slurry prepared in the step (2) into a reflux kettle, and starting solvent reflux extraction: heating in a water bath under stirring within 30min, heating the reflux kettle to 60 ℃, and preserving heat for 120min; continuously stirring and heating for 30min, heating to reflux temperature, and refluxing for 4h; condensing the distilled steam by a condensing system, then flowing back to a reflux kettle, collecting reflux liquid after the reflux is finished, filtering, separating to obtain an organic layer, adding a sufficient amount of anhydrous sodium sulfate as a drying agent into the organic layer, sealing and drying overnight, removing the drying agent after the drying is finished, vacuumizing by a water pump or an oil pump at the temperature below 40 ℃ to the vacuum degree of about 0.02-0.1 Pa, and removing the extracting agent by rotary evaporation to obtain the peony essential oil with the extraction rate of 1.103 per mill.
Example 7
A method for extracting flos moutan essential oil by using surfactant aqueous solution and solid alkali comprises the steps of:
(1) Preparing peony petals: the petals of the fresh peony flower picked at the beginning of 6-10 am and at the end of 4-7 pm are selected, half-opened is good, the petals are fresh and free from insect damage, and the petals are washed with water before use, and the water is naturally drained or is spin-dried by a low-speed rotary net drum.
(2) Preparing solid alkali:
adding 223.3g of magnesium chloride and 55.5g of calcium chloride into 12 times of water, uniformly stirring, and preparing into an aqueous solution; 222g of graphite powder (sieving with a 200-mesh sieve) is added and stirred uniformly; then, dropwise adding an alkaline solution (NaOH solution with the mass fraction of 10%) while stirring to adjust the pH value to 11 for precipitation, and filtering to separate a precipitate; washing the precipitate by deionized water, airing, and then placing the precipitate in a muffle furnace for calcination at 900 ℃ for 36h to obtain the solid alkali.
Then extracting according to the following steps:
(1) Taking 1kg of peony petals, adding 3kg of active water, mixing, pulping to obtain a pulping mixture, and sieving with a 200-mesh sieve. The active water is an aqueous solution of a surfactant, the mass percentage of the surfactant is 1%, the water is deionized water, and the surfactant is prepared from 71% of propylene glycol random polyether PPE-1500, 17% of triton X-100 and 12% of dodecyl trimethyl ammonium chloride.
(2) 110g of solid alkali is added into the beating mixture, and the mixture is stirred uniformly and then is kept stand for 5 hours to obtain mixed slurry.
(3) Transferring 7L of extractant (the volume ratio of n-hexane to petroleum ether is 0.15:1) and the mixed slurry prepared in the step (2) into a reflux kettle, and starting solvent reflux extraction: heating in a water bath under stirring within 40min, heating the reflux kettle to 55 ℃, and preserving heat for 110min; continuously stirring and heating for 35min, heating to reflux temperature, and refluxing for 3h; condensing the distilled steam by a condensing system, flowing back to a reflux kettle, collecting reflux liquid after the reflux is finished, filtering, separating to obtain an organic layer, adding a sufficient amount of anhydrous sodium sulfate as a drying agent into the organic layer, sealing and drying overnight, removing the drying agent after the drying is finished, vacuumizing by a water pump or an oil pump at the temperature below 40 ℃ to the vacuum degree of about 0.02-0.1 Pa, and removing the extracting agent by rotary evaporation to obtain the peony essential oil with the extraction rate of 0.997 per mill.
Example 8
A method for extracting flos moutan essential oil by using surfactant aqueous solution and solid alkali comprises the steps of:
(1) Preparing peony petals: the petals of the fresh peony flower picked at the beginning of 6-10 am and at the end of 4-7 pm are selected, half-opened is good, the petals are fresh and free from insect damage, and the petals are washed with water before use, and the water is naturally drained or is spin-dried by a low-speed rotary net drum.
(2) Preparing solid alkali:
adding 182.7g of magnesium chloride and 55.5g of calcium chloride into 12 times of water, uniformly stirring, and preparing into an aqueous solution; 222g of graphite powder (sieving with a 100-mesh sieve) is added and stirred uniformly; then, dropwise adding an alkaline solution (NaOH solution with the mass fraction of 10%) while stirring to adjust the pH value to 12 for precipitation, and filtering to separate a precipitate; washing the precipitate by deionized water, airing, and then placing the precipitate in a muffle furnace for calcining at 900 ℃ for 48 hours to obtain the solid alkali.
Then extracting according to the following steps:
(1) Taking 1kg of peony petals, adding 2.5kg of active water, mixing, pulping to obtain a pulping mixture, and sieving with a 100-mesh sieve. The active water is an aqueous solution of a surfactant, the mass percentage of the surfactant is 1%, the water is deionized water, and the surfactant is prepared from 71% of propylene glycol random polyether PPE-1500, 17% of triton X-100 and 12% of dodecyl trimethyl ammonium chloride.
(2) 130g of solid alkali is added into the beating mixture, and the mixture is stirred uniformly and then is kept stand for 5 hours to obtain mixed slurry.
(3) Transferring 8L of extractant (the volume ratio of n-hexane to petroleum ether is 0.15:1) and the mixed slurry prepared in the step (2) into a reflux kettle, and starting solvent reflux extraction: heating in a water bath under stirring within 45min, heating the reflux kettle to 55 ℃, and preserving heat for 100min; continuously stirring and heating for 35min, heating to reflux temperature, and refluxing for 5h; condensing the distilled steam by a condensing system, then flowing back to a reflux kettle, collecting reflux liquid after the reflux is finished, filtering, separating to obtain an organic layer, adding a sufficient amount of anhydrous sodium sulfate as a drying agent into the organic layer, sealing and drying overnight, removing the drying agent after the drying is finished, vacuumizing by a water pump or an oil pump at the temperature below 40 ℃, and removing an extracting agent by blowing nitrogen to obtain the peony essential oil with the extraction rate of 1.137 per mill.
In conclusion, the invention effectively overcomes the defects in the prior art and has high industrial utilization value. The above-described embodiments are provided to illustrate the gist of the present invention, but are not intended to limit the scope of the present invention. It will be understood by those skilled in the art that various modifications and equivalent substitutions may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (7)
1. The method for extracting the peony essential oil by using the aqueous solution of the surfactant and the solid alkali is characterized by comprising the following steps of:
(1) Mixing 1 part by weight of peony petals with 2.5-3 parts by weight of active water, and pulping to obtain a pulping mixture; the active water is an aqueous solution of a surfactant;
(2) Adding solid alkali into the beating mixture, stirring uniformly, and standing to obtain mixed slurry;
(3) Transferring the extractant and the mixed slurry prepared in the step (2) into a reflux kettle for solvent reflux extraction, collecting reflux liquid and performing post-treatment to obtain peony essential oil;
the mass percentage of the surfactant in the active water is 0.8-1.6%; the surfactant is a composition of propylene glycol random polyether PPE-1500, triton X-100 and dodecyl trimethyl ammonium chloride; the propylene glycol random polyether PPE-1500 accounts for 65-80% of the weight of the composition, the triton X-100 accounts for 10-20% of the weight of the composition, and the dodecyl trimethyl ammonium chloride accounts for 10-20% of the weight of the composition;
the solid alkali in the step (2) is formed by mixing and calcining alkaline precipitates of calcium and magnesium ions and graphite powder, and the preparation method comprises the following steps: adding water into magnesium chloride and calcium chloride to prepare a solution, adding graphite powder, uniformly stirring, then dropwise adding alkali solution while stirring to adjust the pH value to 11-12 for precipitation, and filtering to separate a precipitate; washing and drying the precipitate, and then placing the precipitate in a muffle furnace to calcine the precipitate at 800-900 ℃ for 36-48 h to obtain the solid alkali.
2. The method for extracting peony essential oil by using a surfactant aqueous solution and solid alkali according to claim 1, wherein the molar ratio of magnesium chloride to calcium chloride is (1.2-2.2) to 1.
3. The method for extracting peony essential oil by using a surfactant aqueous solution and solid alkali according to claim 2, wherein the weight ratio of the graphite powder to the calcium chloride is (3.5-4.5) to 1.
4. The method for extracting peony essential oil by using a surfactant aqueous solution and solid alkali as claimed in claim 3, wherein when the magnesium chloride and the calcium chloride are added with water to prepare the solution, the addition amount of the water is 8-12 times of the weight of the calcium chloride.
5. The method for extracting essential oil of peony flower using aqueous solution of surfactant and solid base as claimed in any one of claims 1 to 4, wherein in the step (2), the solid base is used in an amount of 0.08 to 0.16 weight part.
6. The method for extracting peony essential oil by using a surfactant aqueous solution and solid alkali according to claim 1, wherein the specific operation of performing the solvent reflux extraction in the step (3) is as follows: stirring and heating the reflux kettle to 50-60 ℃ within 30-45 min, and preserving heat for 100-120 min; continuously stirring and heating for 30-40 min, heating to reflux temperature, and refluxing for 3-5 h; and (5) collecting reflux liquid after the reflux is finished, filtering, separating liquid, collecting an organic layer, drying, and evaporating the solvent to obtain the peony essential oil.
7. The method for extracting peony essential oil by using a surfactant aqueous solution and solid alkali according to claim 6, wherein the extractant is a mixture of n-hexane and petroleum ether in a volume ratio of (0.1-0.15) to 1; the dosage of the extractant is as follows: every 1kg of peony petals is used with 6-8L extractant.
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