CN110551012B - Process for extracting paeonol from moutan bark by steam distillation method - Google Patents

Process for extracting paeonol from moutan bark by steam distillation method Download PDF

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CN110551012B
CN110551012B CN201910900133.7A CN201910900133A CN110551012B CN 110551012 B CN110551012 B CN 110551012B CN 201910900133 A CN201910900133 A CN 201910900133A CN 110551012 B CN110551012 B CN 110551012B
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paeonol
oil
water
steam distillation
crystal
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CN110551012A (en
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亓云吉
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Shandong Huawutang Biotechnology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78Separation; Purification; Stabilisation; Use of additives
    • C07C45/81Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78Separation; Purification; Stabilisation; Use of additives
    • C07C45/81Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C45/82Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation

Abstract

The invention relates to a process for extracting paeonol from moutan bark by a steam distillation method, which comprises the following steps: d1 preparing cortex moutan powder, D2 extracting by steam distillation, D3 separating oil from water, collecting the volatile oil containing paeonol, collecting paeonol crystal A: and D2, separating the distillate in the step D2 into volatile oil containing paeonol and aromatic water containing paeonol, cooling the volatile oil to separate out brown yellow large paeonol crystal A, cooling the aromatic water D4, collecting paeonol crystal B, and purifying the paeonol crystal D5. The solvent is added with sodium chloride and hydrochloric acid, so that paeonol can be quickly evaporated out, the pipeline wall of equipment is prevented from being blocked, the paeonol is extracted from the distillate by stages, the yield of the paeonol is improved, the supernatant obtained after multiple extractions is recycled, water is saved, the equipment maintenance is facilitated, and the service life of the equipment is prolonged.

Description

Process for extracting paeonol from moutan bark by steam distillation method
Technical Field
The invention relates to the technical field of paeonol extraction, and particularly relates to a process for extracting paeonol from moutan bark by a steam distillation method.
Background
Paeonol is an effective component extracted from dried root bark of Paeonia suffruticosa Andr. Paeonol is white or yellowish needle crystal with luster, and colorless needle crystal (ethanol). Cortex moutan is dried root bark of Paeonia suffruticosa Andr. Produced in Anhui, Shandong, etc. Digging root in autumn, removing fine root, peeling root bark, and sun drying. The main ingredients of the medicine comprise paeonol, paeoniflorin, paeonol glycoside, paeonol neoside, benzoylpaeoniflorin, volatile oil, etc. Wherein the paeonol content is the highest and is a content determination index component specified in Chinese pharmacopoeia. Modern researches prove that the paeonol has the effects of calming, hypnotizing, resisting bacteria, diminishing inflammation, resisting oxidation, reducing blood pressure and the like, and in the aspect of daily use chemicals, the paeonol can inhibit the generation of intracellular O2-free radicals, whiten the skin, reduce and discolor pigments deposited in the skin, and remove blood stasis and spots; also has antiinflammatory, repercussive, analgesic, antiallergic, and antiviral effects. Has good therapeutic and health promoting effects on mottle, myalgia, skin pruritus, psoriasis, herpes zoster, and eczema, and also has good effects in toothpaste, collutory, dentifrice, and toothache liquid. Cortex moutan is a common Chinese medicinal material, and many varieties of cortex moutan in pharmaceutical factories need to extract paeonol. The paeonol extraction process is a steam distillation method at present, because the paeonol can be dissolved in hot water, the distilled aromatic water is cooled by frozen water, and the paeonol is collected by a filtration method after crystal form growth for about three to four days. At present, most of the processes for large-scale production of the medicine enterprises are the same. The process is mature, and the obtained paeonol has good crystal form and high quality. However, for mass production by an enterprise, there are the following problems: after steam distillation, the temperature of water vapor is reduced after the water vapor passes through a condenser, the cortex moutan volatile oil is condensed into fine oil droplets which are not discharged along with aromatic water, the cortex moutan volatile oil contains more paeonol, the settlement is rapid, fine grains are easily formed and attached to the wall and the bottom, the cortex moutan volatile oil cannot be taken out, the downtime maintenance cost is high, and the service life of equipment pipelines is short; the distilled aromatic water contains volatile oil and paeonol crystals with higher concentration, in the production process, a plurality of paeonol crystals can be adsorbed in the pipeline of the equipment, the pipeline is almost blocked, the yield of the paeonol is influenced, in addition, although the solubility of the paeonol in cold water is low, the amount of the aromatic water is large, the paeonol is not dissolved, the paeonol cannot be effectively recovered, the water consumption is large, and the water resource is wasted.
Disclosure of Invention
In order to overcome the defects, the invention aims to provide a process for extracting paeonol from moutan bark by a steam distillation method.
The technical scheme adopted by the invention for solving the technical problem is as follows: a process for extracting paeonol from cortex moutan by steam distillation comprises the following steps:
d1 preparation of moutan bark powder: selecting clean and disease-free dry moutan bark, crushing, and sieving by a sieve of 80-100 meshes;
d2 steam distillation extraction: adding cortex moutan powder into a steam distillation extractor, adding 8-10 times of solvent (sodium chloride, hydrochloric acid, and ethanol water solution containing 8-12 wt% of sodium chloride, 8-10 wt% of wtHCl, and 5-10 wt% of ethanol), soaking at room temperature for 1-2 hr, heating to boil, performing steam distillation, and collecting distillate;
d3 oil-water separation, collecting volatile oil containing paeonol, collecting paeonol crystal A: d2, separating the distillate from the oil-water separator to obtain volatile oil containing paeonol and aromatic water containing paeonol, and cooling the volatile oil to separate out brown yellow bulk paeonol crystal A;
d4 cooling the aromatic water, and collecting paeonol crystal B: d, oscillating the aromatic water obtained in the step D3 at the temperature of 2-10 ℃ for crystallization for 1-2h, then standing for crystallization for 12h, and filtering to obtain a supernatant and an acicular paeonol crystal B;
d5 purifying paeonol crystal: mixing the paeonol crystal A and the paeonol crystal B, mixing with 7-8 times of 60-70% ethanol, heating to 70-80 deg.C, stirring for dissolving, freezing at 2-10 deg.C for crystallizing, filtering, and air drying to obtain pure paeonol product.
Specifically, the method also comprises secondary distillation, wherein the secondary distillate is recovered: recovering the supernatant to Soxhlet extractor for secondary distillation, connecting the liquid outlet pipe of the secondary distillate with the liquid inlet of the oil-water separator, recovering paeonol in the secondary distillate, and determining that the separated supernatant still contains paeonol.
Specifically, the oil-water separation process is set to be two stages, the distillate is extracted from a steam distillation extraction device to a first-stage oil-water separator, the temperature of the first-stage oil-water separation is 60-70 ℃, oil-water separation is carried out at high temperature, volatile oil A containing paeonol is collected, aromatic water after the first-stage oil-water separation is left in the second-stage oil-water separator, the temperature of the second-stage oil-water separation is 50-60 ℃, volatile oil B containing paeonol is collected, aromatic water after the second-stage oil-water separation is collected, the volatile oil A containing paeonol and the volatile oil B containing paeonol are combined into volatile oil containing paeonol, the melting point of the paeonol is 49-51 ℃, the collected paeonol volatile oil is subjected to melting point experiment, the paeonol is still in a liquid state at 40-48 ℃, and a brownish yellow blocky solid can be rapidly formed when stimulation is given to oscillation, seed crystal and the like, and the mixture is dense and has certain hardness, the paeonol content is about 99 percent by measurement.
Specifically, the oil-water separator adopts a high-temperature demulsification oil-water separator, adopts double-stage heating demulsification and gravity separation, changes the electric field of fine oil droplets through high temperature (60-70 ℃), reduces mutual repulsion, enables the fine oil droplets to be more easily collided with each other to combine into large oil droplets, is beneficial to gravity separation, removes the separated oil stains on the top by tracking an oil film layer through an ingenious floater, and can effectively separate the oil droplets suspended in the middle of tank liquid.
Specifically, when the volume of the supernatant generated in D4 was 2/3 of the volume of the liquid in the steam distillation extractor, the supernatant was directly added as a solvent to the steam distillation extractor for recycling.
The invention has the following beneficial effects: according to the invention, sodium chloride and hydrochloric acid are added into the solvent, so that paeonol can be quickly evaporated out, and the production efficiency is accelerated; ethanol is added into the solvent, the ethanol is volatile, in the initial stage of distillation, the ethanol in the solvent is in the initial distillate, the solubility of the volatile oil in the ethanol is high, and the high-concentration paeonol volatile oil in the initial distillate can be prevented from being adsorbed on the pipeline wall of the equipment; extracting paeonol from the distillate by stages, wherein the paeonol content in the volatile oil is high, the paeonol is easy to crystallize, the yield is high and accounts for about 70 percent of the total paeonol, and the paeonol can be prevented from being adsorbed in equipment to block equipment pipelines; the paeonol content in the aromatic water after oil-water separation is low, crystallization in equipment pipelines is not easy, cooling is gradually carried out in the preparation process, the using amount of frozen water is reduced, about 25% of paeonol is recovered, supernatant of the crystallized aromatic water can be subjected to secondary distillation, the residual 5% of paeonol is extracted, the yield of the paeonol is improved, the supernatant obtained after repeated extraction is recycled, water is saved, equipment maintenance is facilitated, and the service life of the equipment is prolonged.
Detailed Description
The present invention will now be described in further detail.
Example 1
A process for extracting paeonol from cortex moutan by steam distillation comprises the following steps:
d1 preparation of moutan bark powder: selecting clean and disease-free dry moutan bark, crushing, and sieving by a sieve of 80-100 meshes;
d2 steam distillation extraction: adding 1000g of tree peony bark powder into a steam distillation extractor, adding 8 times of solvent which contains 8 wt% of sodium chloride, 10 wt% of WtHCl and 5 wt% of ethanol, soaking at normal temperature for 1h, heating to boil, performing steam distillation, and collecting distillate after distillation;
d3 oil-water separation, collecting volatile oil containing paeonol, collecting paeonol crystal A: d2, enabling the distillate to pass through an oil-water separator, wherein the oil-water separation process is carried out in two stages, the distillate is from a steam distillation extraction device to a first-stage oil-water separator, the temperature of the first-stage oil-water separation is 60-70 ℃, oil-water separation is carried out at high temperature, volatile oil A containing paeonol is collected, aromatic water after the first-stage oil-water separation is left in a second-stage oil-water separator, the temperature of the second-stage oil-water separation is 50-60 ℃, volatile oil B containing paeonol is collected, aromatic water after the second-stage oil-water separation is collected, the volatile oil A containing the paeonol and the volatile oil B are combined into volatile oil containing the paeonol, the volatile oil containing the paeonol and the aromatic water containing the paeonol are separated, the volatile oil is cooled to separate brown yellow large blocks of paeonol crystal A, and the volatile oil is dried and weighed to be 8.69 g;
d4 cooling the aromatic water, and collecting paeonol crystal B: oscillating the aromatic water obtained in the step D3 at the temperature of 2-10 ℃ for crystallization for 1h, standing for crystallization for 12h, filtering to obtain a supernatant and a needle crystal paeonol crystal B, drying, and weighing 3.87 g;
d5 purifying paeonol crystal: mixing the paeonol crystal A and the paeonol crystal B, mixing with 7 times of 60% ethanol, heating to 80 deg.C, stirring for dissolving, freezing at 2-10 deg.C for crystallizing, filtering, and air drying to obtain pure paeonol product 11.53 g.
Specifically, the method also comprises secondary distillation, wherein the secondary distillate is recovered: recovering the supernatant to Soxhlet extractor for secondary distillation, connecting the liquid outlet pipe of the secondary distillate with the liquid inlet of the oil-water separator, recovering paeonol in the secondary distillate, and determining that the separated supernatant still contains paeonol.
Specifically, the oil-water separator adopts a high-temperature demulsification oil-water separator.
Specifically, after the secondary distillation, when the liquid volume of the residual supernatant reaches 2/3 of the volume of the solvent in the steam distillation extractor, the residual supernatant is directly used as the solvent and added into the steam distillation extractor for recycling.
After the extraction by the extraction method, 11.53g of pure paeonol is obtained, which accounts for 1.153% of the moutan bark powder, and the content of paeonol is determined to be 98.3% by an HPLC method.
Example 2
A process for extracting paeonol from cortex moutan by steam distillation comprises the following steps:
d1 preparation of moutan bark powder: selecting clean and disease-free dry moutan bark, crushing, and sieving by a sieve of 80-100 meshes;
d2 steam distillation extraction: adding cortex moutan powder into a steam distillation extractor, adding 9 times of solvent containing 9 wt% of sodium chloride, 9 wt% of HCl and 7 wt% of ethanol, soaking at normal temperature for 2h, heating to boil, performing steam distillation, and distilling to collect distillate;
d3 oil-water separation, collecting volatile oil containing paeonol, collecting paeonol crystal A: d2, enabling the distillate to pass through an oil-water separator, wherein the oil-water separation process is carried out in two stages, the distillate is from a steam distillation extraction device to a first-stage oil-water separator, the temperature of the first-stage oil-water separation is 60-70 ℃, oil-water separation is carried out at high temperature, volatile oil A containing paeonol is collected, aromatic water after the first-stage oil-water separation is left in a second-stage oil-water separator, the temperature of the second-stage oil-water separation is 50-60 ℃, volatile oil B containing paeonol is collected, aromatic water after the second-stage oil-water separation is collected, the volatile oil A containing the paeonol and the volatile oil B are combined into volatile oil containing the paeonol, the volatile oil containing the paeonol and the aromatic water containing the paeonol are separated, the volatile oil is cooled to separate brown yellow large blocks of paeonol crystal A, and 9.21g of paeonol crystal A is dried and weighed;
d4 cooling the aromatic water, and collecting paeonol crystal B: oscillating the aromatic water obtained in the step D3 at the temperature of 2-10 ℃ for crystallization for 1.5h, standing for crystallization for 12h, filtering to obtain a supernatant and an acicular paeonol crystal B, drying, and weighing 3.45 g;
d5 purifying paeonol crystal: mixing the paeonol crystal A and the paeonol crystal B, mixing with 8 times of 70% ethanol, heating to 75 deg.C, stirring for dissolving, freezing at 2-10 deg.C for crystallizing, filtering, and air drying to obtain pure paeonol product.
Specifically, the method also comprises secondary distillation, wherein the secondary distillate is recovered: recovering the supernatant to Soxhlet extractor for secondary distillation, connecting the liquid outlet pipe of the secondary distillate with the liquid inlet of the oil-water separator, recovering paeonol in the secondary distillate, and determining that the separated supernatant still contains paeonol.
Specifically, the oil-water separator adopts a high-temperature demulsification oil-water separator.
Specifically, after the secondary distillation, when the liquid volume of the residual supernatant reaches 2/3 of the volume of the solvent in the steam distillation extractor, the residual supernatant is directly used as the solvent and added into the steam distillation extractor for recycling.
After the extraction by the extraction method, 11.78g of pure paeonol is obtained, which accounts for 1.178% of the moutan bark powder, and the content of paeonol is 99.53% by HPLC.
Example 3
A process for extracting paeonol from cortex moutan by steam distillation comprises the following steps:
d1 preparation of moutan bark powder: selecting clean and disease-free dry moutan bark, crushing, and sieving by a sieve of 80-100 meshes;
d2 steam distillation extraction: adding cortex moutan powder into a steam distillation extractor, adding 10 times of solvent containing 10 wt% of sodium chloride, 8 wt% of HCl and 9 wt% of ethanol, soaking at normal temperature for 1.5h, heating to boil, performing steam distillation, and collecting distillate;
d3 oil-water separation, collecting volatile oil containing paeonol, collecting paeonol crystal A: d2, enabling the distillate to pass through an oil-water separator, wherein the oil-water separation process is carried out in two stages, the distillate is from a steam distillation extraction device to a first-stage oil-water separator, the temperature of the first-stage oil-water separation is 60-70 ℃, oil-water separation is carried out at high temperature, volatile oil A containing paeonol is collected, aromatic water after the first-stage oil-water separation is left in a second-stage oil-water separator, the temperature of the second-stage oil-water separation is 50-60 ℃, volatile oil B containing paeonol is collected, aromatic water after the second-stage oil-water separation is collected, the volatile oil A containing the paeonol and the volatile oil B are combined into volatile oil containing the paeonol, the volatile oil containing the paeonol and the aromatic water containing the paeonol are separated, the volatile oil is cooled to separate brown yellow large blocks of paeonol crystal A, and 9.07g of paeonol crystal A is dried;
d4 cooling the aromatic water, and collecting paeonol crystal B: oscillating the aromatic water obtained in the step D3 at the temperature of 2-10 ℃ for crystallization for 2h, standing for crystallization for 12h, filtering to obtain a supernatant and a needle crystal paeonol crystal B, drying, and weighing 4.12 g;
d5 purifying paeonol crystal: mixing the paeonol crystal A and the paeonol crystal B, mixing with 8 times of 65% ethanol, heating to 70 deg.C, stirring for dissolving, freezing at 2-10 deg.C for crystallizing, filtering, and air drying to obtain pure paeonol product.
Specifically, the method also comprises secondary distillation, wherein the secondary distillate is recovered: recovering the supernatant to Soxhlet extractor for secondary distillation, connecting the liquid outlet pipe of the secondary distillate with the liquid inlet of the oil-water separator, recovering paeonol in the secondary distillate, and determining that the separated supernatant still contains paeonol.
Specifically, the oil-water separator adopts a high-temperature demulsification oil-water separator.
Specifically, after the secondary distillation, when the liquid volume of the residual supernatant reaches 2/3 of the volume of the solvent in the steam distillation extractor, the residual supernatant is directly used as the solvent and added into the steam distillation extractor for recycling.
After the extraction by the extraction method, 12.02g of pure paeonol is obtained, which accounts for 1.202 percent of the moutan bark powder, and the content of paeonol is 99.37 percent by HPLC.
Example 4
A process for extracting paeonol from cortex moutan by steam distillation comprises the following steps:
d1 preparation of moutan bark powder: selecting clean and disease-free dried tree peony bark, crushing, and sieving by a sieve of 80-100 meshes;
d2 steam distillation extraction: adding cortex moutan powder into a steam distillation extractor, adding 9 times of solvent containing 12 wt% of sodium chloride, 9 wt% of HCl and 10 wt% of ethanol, soaking at normal temperature for 2h, heating to boil, performing steam distillation, and collecting distillate;
d3 oil-water separation, collecting volatile oil containing paeonol, collecting paeonol crystal A: d2, enabling the distillate to pass through an oil-water separator, wherein the oil-water separation process is carried out in two stages, the distillate is from a steam distillation extraction device to a first-stage oil-water separator, the temperature of the first-stage oil-water separation is 60-70 ℃, oil-water separation is carried out at high temperature, volatile oil A containing paeonol is collected, aromatic water after the first-stage oil-water separation is left in a second-stage oil-water separator, the temperature of the second-stage oil-water separation is 50-60 ℃, volatile oil B containing paeonol is collected, aromatic water after the second-stage oil-water separation is collected, the volatile oil A containing the paeonol and the volatile oil B are combined into volatile oil containing the paeonol, the volatile oil containing the paeonol and the aromatic water containing the paeonol are separated, the volatile oil is cooled to separate brown yellow large blocks of paeonol crystal A, and 8.56g of paeonol crystal A is dried and weighed;
d4 cooling the aromatic water, and collecting paeonol crystal B: oscillating the aromatic water obtained in the step D3 at the temperature of 2-10 ℃ for crystallization for 2h, standing for crystallization for 12h, filtering to obtain a supernatant and a needle crystal paeonol crystal B, drying, and weighing 3.75 g;
d5 purifying paeonol crystal: mixing the paeonol crystal A and the paeonol crystal B, mixing with 8 times of 70% ethanol, heating to 80 deg.C, stirring for dissolving, freezing at 2-10 deg.C for crystallizing, filtering, and air drying to obtain pure paeonol product.
Specifically, the method also comprises secondary distillation, wherein the secondary distillate is recovered: recovering the supernatant to Soxhlet extractor for secondary distillation, connecting the liquid outlet pipe of the secondary distillate with the liquid inlet of the oil-water separator, recovering paeonol in the secondary distillate, and determining that the separated supernatant still contains paeonol.
Specifically, the oil-water separator adopts a high-temperature demulsification oil-water separator.
Specifically, after the secondary distillation, when the liquid volume of the residual supernatant reaches 2/3 of the volume of the solvent in the steam distillation extractor, the residual supernatant is directly used as the solvent and added into the steam distillation extractor for recycling.
After the extraction by the extraction method, 11.64g of pure paeonol is obtained, which accounts for 1.164 percent of the moutan bark powder, and the content of paeonol is determined to be 98.19 percent by an HPLC method.
The present invention is not limited to the above embodiments, and any structural changes made by the present invention shall be understood as falling within the scope of the present invention, wherein the structural changes are the same as or similar to the technical solutions of the present invention.
The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.

Claims (4)

1. A process for extracting paeonol from moutan bark by a steam distillation method is characterized by comprising the following steps: the method comprises the following steps:
d1 preparation of moutan bark powder: selecting clean and disease-free dried tree peony bark, crushing, and sieving by a sieve of 80-100 meshes;
d2 steam distillation extraction: adding cortex moutan powder into a steam distillation extractor, adding 8-10 times of solvent, soaking at normal temperature for 1-2 hr, heating to boil, performing steam distillation, distilling to collect distillate, wherein the solvent is aqueous solution of sodium chloride, hydrochloric acid, and ethanol, and contains 8-12 wt% sodium chloride, 8-10 wt% wtHCl, and 5-10 wt% ethanol,
d3 separating oil from water, collecting volatile oil containing paeonol, collecting paeonol crystal A: d2, separating the distillate from the oil-water separator to obtain volatile oil containing paeonol and aromatic water containing paeonol, and cooling the volatile oil to separate out brown yellow bulk paeonol crystal A;
the oil-water separation process is two-stage, the distillate is from a steam distillation extraction device to a first-stage oil-water separator, the temperature of the first-stage oil-water separation is 60-70 ℃, oil-water separation is carried out at high temperature, volatile oil A containing paeonol is collected, aromatic water after the first-stage oil-water separation is left in a second-stage oil-water separator, the temperature of the second-stage oil-water separation is 50-60 ℃, volatile oil B containing paeonol is collected, and aromatic water after the second-stage oil-water separation is collected;
d4 cooling the aromatic water, and collecting paeonol crystal B: oscillating the aromatic water in the step D3 at the temperature of 2-10 ℃ for crystallization for 1-2h, standing for crystallization for 12h, and filtering to obtain a supernatant and an acicular paeonol crystal B, wherein when the volume of the supernatant generated in the step D4 is 2/3 of the volume of the liquid in the steam distillation extractor, the supernatant is directly used as a solvent and added into the steam distillation extractor for recycling;
d5 purifying paeonol crystal to obtain pure paeonol.
2. The process for extracting paeonol from moutan bark by steam distillation as claimed in claim 1, wherein: also comprises secondary distillation, and the secondary distillate is recovered: recovering the supernatant to Soxhlet extractor for secondary distillation, connecting the liquid outlet pipe of the secondary distillate with the liquid inlet of the oil-water separator, recovering paeonol in the secondary distillate, and determining that the separated supernatant still contains paeonol.
3. The process for extracting paeonol from moutan bark by steam distillation according to claim 1 or 2, wherein: the oil-water separator adopts a high-temperature demulsification oil-water separator.
4. The process for extracting paeonol from moutan bark by steam distillation according to claim 1 or 2, wherein: the method for purifying paeonol crystals in the step D5 comprises the following steps: mixing paeonol crystal A and paeonol crystal B, mixing with 7-8 times of 60-70% ethanol, heating to 70-80 deg.C, stirring for dissolving, freezing at 2-10 deg.C for crystallizing, filtering, and air drying.
CN201910900133.7A 2019-09-23 2019-09-23 Process for extracting paeonol from moutan bark by steam distillation method Active CN110551012B (en)

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CN113861003A (en) * 2021-11-04 2021-12-31 山东东宇生态科技有限公司 Method for extracting paeonol from moutan bark
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加酸加盐水蒸气蒸馏法提取牡丹皮中丹皮酚的工艺研究;宫春博等;《山东中医药大学学报》;20130320;第37卷(第2期);第910-912页 *

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