A method for continuous extraction of cinnamic essential oil with water vapor and water

Abstract

The present application relates to the technical field of plant essential oil extraction process, and particularly relates to a method for extracting cinnamon essential oil by using steam and water in a continuous mode. The method comprises the following steps: weighing cinnamon bark, cinnamon twigs and cinnamon leaves, drying, crushing, sieving and obtaining cinnamon powder; placing the cinnamon powder in brine and soaking, filtering, putting the filtered cinnamon powder into an extraction tank, adding industrial water, stirring uniformly and obtaining a mixture; heating the mixture in the extraction tank to a micro-boiling state, continuously introducing catalytic steam above the liquid surface of the extraction tank, continuously extracting for 1-3 hours and obtaining essential oil mixed with steam; condensing the essential oil mixed with steam by using a condensing device, flowing into an oil-water separation device for oil-water separation and obtaining cinnamon essential oil. The method for extracting essential oil by using catalytic steam is combined with the traditional water extraction method, emulsification caused by high temperature or explosive boiling is effectively avoided, the yield of essential oil is high, the quality of the oil is good and the extraction efficiency is high.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of plant essential oil extraction, and particularly relates to a method for extracting cinnamon essential oil by using water vapor and water in series. BACKGROUND

[0002] Cinnamon, also known as Chinese cinnamon or cassia bark, is the dried bark of a plant in the Lauraceae family, which is grayish brown or yellowish brown in color, has a strong aromatic odor, and is mainly produced in southern provinces such as Guangdong and Fujian. Cinnamon is rich in nutrients and has high medicinal value, and has the effects of dispelling cold and relieving pain, dilating blood vessels, resisting gastric ulcers, inhibiting bacteria, and resisting oxidation, and is usually used as a spice and a traditional Chinese medicine. The main functional components of cinnamon are volatile oils, terpenes, and flavanols, and the content of volatile oil is 1.0-2.3%. Cinnamon essential oil is a mixture of volatile, transparent liquid with a light yellow or brownish yellow color extracted from the bark, branches or leaves of the cinnamon plant, and is a natural edible spice with a special aroma of cinnamon and good functional activity. Cinnamon essential oil is complex in composition, including aldehydes, esters, aromatics, terpenes, and ketones, and the compositions of essential oils obtained by different extraction processes differ greatly. According to the requirements of the pharmacopoeia, the main component of cinnamon essential oil is cinnamyl aldehyde, and the content of cinnamyl aldehyde should be greater than 75%. Studies have found that cinnamon essential oil has a mild performance, can effectively calm and relieve pain, dispel wind and invigorate the stomach, and can also effectively promote blood circulation in the human body, resist aging, relieve muscle spasms, astringe the skin, and remove skin warts. Therefore, cinnamon essential oil has great application prospects in the fields of health foods, daily chemicals, cosmetics, and biological medicines, and has great research and utilization value.

[0003] At present, the common extraction methods of cinnamon essential oil include traditional steam distillation and new supercritical carbon dioxide extraction, but steam distillation extraction has problems such as high temperature, easy emulsification, low extraction efficiency, and low oil purity. Although supercritical carbon dioxide extraction can improve the extraction efficiency and oil purity to some extent, the extremely high equipment cost seriously limits the industrial production of this method. Therefore, it is necessary to explore a new method for extracting cinnamon essential oil to improve the extraction efficiency and oil purity of cinnamon essential oil and to easily realize industrial production. SUMMARY

[0004] The first object of the present application is to provide a method for extracting cinnamon essential oil by using water vapor and water in series, and the second object of the present application is to provide cinnamon essential oil extracted by the method.

[0005] The present application is realized by the following technical solutions:

[0006] According to the first aspect of the present application, a method for extracting cinnamon essential oil by using water vapor and water in series is provided, which comprises the following steps:

[0007] S1, weigh the cassia bark, cassia twig and cassia leaves, mix them evenly, dry them, then crush them, and sieve them to obtain cassia powder;

[0008] S2, immerse the cassia powder obtained in step S1 in brine, then filter it, and put the filtered cassia powder into an extraction tank, add water, and stir them evenly to obtain a mixture;

[0009] S3, heat the mixture in the extraction tank in step S2 to a micro-boiling state, then continuously introduce catalytic water vapor above the liquid surface of the extraction tank, and continuously extract for 1-3 hours to obtain essential oil mixed with water vapor;

[0010] S4, condense the essential oil mixed with water vapor obtained in step S3 through a condensing device, then flow it into an oil-water separation device to separate oil and water, and obtain cassia essential oil.

[0011] In some embodiments, in step S1, before crushing, the cassia bark, cassia twig and cassia leaves are cleaned, dried in an oven at 60°C, mechanically crushed, and sieved through a 40-60 mesh sieve.

[0012] In some embodiments, in step S2, the concentration of the brine is 2-5 wt%, the mass ratio of the brine to the cassia powder is 5-7:1, and the immersion time is 0.5-3 hours.

[0013] In some embodiments, in step S2, the mass ratio of water to the cassia powder is 7-15:1.

[0014] In some embodiments, in step S3, the temperature to which the mixture in the extraction tank is heated to a micro-boiling state is 90-100°C.

[0015] In some embodiments, in step S3, the position at which the catalytic water vapor is introduced into the extraction tank is 10-30 cm above the liquid surface.

[0016] In some embodiments, in step S3, the preparation method of the catalytic water vapor is: passing water vapor through a column filled with a catalyst to obtain catalytic water vapor, the passing time is 20-60 seconds, and the temperature range is 100-130°C; wherein the catalyst is a mixture of foamed iron and foamed manganese with a mass ratio of 3:1. The conductivity of the catalytic water vapor obtained is different when the water vapor passes through the column filled with the catalyst for different times. The longer the water vapor passes through the column filled with the catalyst, the higher the conductivity of the catalytic water vapor obtained.

[0017] The conductivity of the catalytic water vapor is higher than that of the water vapor without catalysis, which is more conducive to the penetration of the oily components in the cassia cells to the outside of the cells, and can avoid the emulsification effect when the essential oil is taken out by water vapor, which is more conducive to the separation and collection of the essential oil.

[0018] In some embodiments, in step S3, the pressure of the catalytic water vapor is 0.1-0.3 MPa, and the conductivity is 0.2-0.4 ms / m.

[0019] In some embodiments, in step S4, tap water is used for condensation or tap water is combined with chilled water for condensation.

[0020] According to a second aspect of the present application, the cinnamomum oil extracted by the above-mentioned method for extracting cinnamomum oil with catalytic water vapor and water is provided.

[0021] The yield of the cinnamomum oil of the present application is 1.3-2.1%, the percentage content of cinnamaldehyde in the cinnamomum oil is 80.0-84.0 wt%, the percentage content of coumarin is 1.5-1.7 wt%, the percentage content of o-methoxycinnamaldehyde is 9.0-11.0 wt%, and the percentage content of cinnamyl acetate is 1.2-1.7 wt%.

[0022] Compared with the prior art, the present application has the following advantages:

[0023] (1) In the present application, the catalytic water vapor extraction method is combined with the traditional water extraction method during extraction. Compared with the traditional water extraction method, the present application reduces the extraction temperature, effectively avoids the emulsification caused by high temperature or boiling, and has high oil yield and good oil quality. Compared with the traditional water vapor extraction method, the present application reduces the extraction time and improves the oil yield. The present application can effectively improve the extraction efficiency and oil quality of cinnamomum oil, improve the oil yield and production efficiency, and has the advantages of simple operation, high extraction efficiency, low process cost, etc., and can be applied to industrial production.

[0024] (2) In the present application, the raw material is mechanically pulverized and broken before extraction, which can more effectively destroy the cell wall structure of the cinnamomum cell, improve the extraction rate, reduce the extraction time, and improve the oil yield and production efficiency.

[0025] (3) In the present application, the cinnamomum powder is soaked in salt water before extraction, which can more quickly promote the penetration of water into the cinnamomum cell, saturate the cinnamomum cell, and fully contact the cinnamomum powder with water, thereby accelerating the exudation of cinnamomum oil, improving the extraction rate, reducing the extraction time, and improving the oil yield and production efficiency.

[0026] (4) In the present application, after the mixture in the extraction tank is heated to micro-boiling, catalytic water vapor is continuously introduced into the extraction tank above the liquid level, which can improve the penetration efficiency of the oily components in the cinnamomum cell, improve the oil yield of the essential oil, improve the efficiency of essential oil separation and collection, and improve the production efficiency. At the same time, the emulsification effect of water vapor on the essential oil is avoided, the color of the oil product is more transparent, and the quality is better.

[0027] (5) Through the extraction process of the present application, the cinnamon essential oil yield can reach 1.3-2.1%, the oil quality is high, the percentage content of cinnamyl aldehyde in the cinnamon essential oil is 80.0-84.0wt%, the percentage content of coumarin is 1.5-1.7wt%, the percentage content of o-methoxycinnamaldehyde is 9.0-11.0wt%, and the percentage content of cinnamyl acetate is 1.2-1.7wt%. BRIEF DESCRIPTION OF DRAWINGS

[0028] Figure 1 The GC-MS spectrum of the cinnamon essential oil of Example 2 of the present application is shown in the figure, wherein 1 is cis-cinnamyl aldehyde; 2 is trans-cinnamyl aldehyde; 3 is coumarin; 4 is cinnamyl acetate; and 5 is o-methoxycinnamaldehyde. DETAILED DESCRIPTION

[0029] The present application will be further described in detail below in conjunction with specific examples. If not otherwise specified, the raw materials used in the following tests are commercially available, and the experimental methods not otherwise specified are all conventional methods known in the art.

[0030] The cinnamon essential oil yield is calculated according to the following formula: Cinnamon essential oil yield (%) = (cinnamon essential oil mass / cinnamon powder mass)*100%.

[0031] Example 1

[0032] The method for extracting cinnamon essential oil by water vapor and water in succession in this example comprises the following steps:

[0033] (1) 0.88 kg of cassia bark, 3.56 kg of cassia branch and 3.56 kg of cassia leaves are weighed and uniformly mixed, dried in a 60℃ oven, mechanically pulverized, and then sieved through a 60-mesh sieve to obtain cinnamon powder.

[0034] (2) The cinnamon powder obtained in step (1) is placed in 40 L of salt water with a concentration of 2wt% and soaked for 0.5 h, then filtered, and the filtered cinnamon powder is placed in an extraction tank, 7 times the weight of industrial water is added, stirred uniformly, and a mixture is obtained.

[0035] (3) The temperature of the mixture in the extraction tank in step (2) is heated to 94℃ to make the mixture micro-boil, then catalytic water vapor with a pressure of 0.1 MPa and an electrical conductivity of 0.22 ms / m is continuously introduced about 20 cm above the liquid surface of the extraction tank to continuously extract for 1.5 h to obtain essential oil mixed water vapor; wherein, the preparation method of the catalytic water vapor is: the water vapor passes through a column filled with a catalyst to obtain catalytic water vapor, the passing time is about 20 s, and the temperature is about 100℃; wherein, the catalyst is a mixture of foamed iron and foamed manganese with a mass ratio of 3:1.

[0036] (4) The essential oil mixed water vapor obtained in step (3) is condensed by a tap water condensing device and then flows into an oil-water separation device for oil-water separation to obtain 108.80 g of cinnamon essential oil. The yield of the cinnamon essential oil is 1.36% by calculation.

[0037] Example 2

[0038] The method for water vapor co-water continuous extraction of cinnamon essential oil in this example comprises the following steps:

[0039] (1) 0.88 kg of cassia bark, 3.56 kg of cassia twig and 3.56 kg of cassia leaf are weighed and uniformly mixed, dried in a 60°C oven, mechanically pulverized, and then sieved through a 60-mesh sieve to obtain cinnamon powder.

[0040] (2) The cinnamon powder obtained in step (1) is placed in 48 L of 4wt% salt water and soaked for 2 h, then filtered, and the filtered cinnamon powder is placed in an extraction tank, 10 times the weight of industrial water is added, stirred uniformly, and a mixture is obtained.

[0041] (3) The temperature of the mixture in the extraction tank in step (2) is heated to 97°C to make the mixture micro-boil, and then catalytic water vapor with a pressure of 0.2 MPa and an electrical conductivity of 0.40 ms / m is continuously introduced about 20 cm above the liquid surface of the extraction tank to continuously extract for 3 h to obtain essential oil mixed water vapor; wherein the preparation method of the catalytic water vapor is: water vapor is passed through a column filled with a catalyst to obtain catalytic water vapor, the passing time is about 40 s, and the temperature is about 120°C; wherein the catalyst is a mixture of foamed iron and foamed manganese in a mass ratio of 3:1.

[0042] (4) The essential oil mixed water vapor obtained in step (3) is condensed by a tap water condensing device and then flows into an oil-water separation device for oil-water separation to obtain 108.80 g of cinnamon essential oil. The yield of the cinnamon essential oil is 1.36% by calculation.

[0043] Example 3

[0044] The method for water vapor co-water continuous extraction of cinnamon essential oil in this example comprises the following steps:

[0045] (1) 0.88 kg of cassia bark, 3.56 kg of cassia twig and 3.56 kg of cassia leaf are weighed and uniformly mixed, dried in a 60°C oven, mechanically pulverized, and then sieved through a 60-mesh sieve to obtain cinnamon powder.

[0046] (2) The cinnamon powder obtained in step (1) is placed in 56 L of salt water with a concentration of 5wt% and soaked for 3 h, then filtered, and the filtered cinnamon powder is placed in an extraction tank, 15 times the weight of industrial water is added to the cinnamon powder, and stirred uniformly to obtain a mixture.

[0047] (3) The temperature of the mixture in the extraction tank in step (2) is heated to 100℃ to make the mixture micro-boil, then catalytic water vapor with a pressure of 0.1 MPa and an electrical conductivity of 0.31 ms / m is continuously introduced about 20 cm above the liquid surface of the extraction tank to carry out continuous extraction for 2 h to obtain essential oil mixed water vapor; wherein the preparation method of the catalytic water vapor is: the water vapor passes through a column filled with a catalyst to obtain catalytic water vapor, the passing time is about 30 s, and the temperature is about 100℃; wherein the catalyst is a mixture of foamed iron and foamed manganese with a mass ratio of 3:1.

[0048] (4) The essential oil mixed water vapor obtained in step (3) is condensed by a tap water condensing device and then flows into an oil-water separation device for oil-water separation to obtain 129.60 g of cinnamon essential oil, and the yield of cinnamon essential oil is calculated to be 1.62%.

[0049] Comparative Example 1

[0050] This comparative example is a traditional co-water extraction method for cinnamon essential oil, which comprises the following steps:

[0051] (1) 0.88 kg of cassia bark, 3.56 kg of cassia twig and 3.56 kg of cassia leaf are weighed and uniformly mixed, dried in a 60℃ oven, and then mechanically pulverized, and then passed through a 60 mesh sieve to obtain cinnamon powder.

[0052] (2) The cinnamon powder obtained in step (1) is placed in 48 L of salt water with a concentration of 2wt% and soaked for 0.5 h, then filtered, and the filtered cinnamon powder is placed in an extraction tank, 7 times the weight of industrial water is added to the cinnamon powder, and stirred uniformly to obtain a mixture.

[0053] (3) The temperature of the mixture in the extraction tank in step (2) is heated to 105℃ to make the mixture boil, and continuous extraction is carried out for 5 h to obtain essential oil mixed water vapor.

[0054] (4) The essential oil mixed water vapor obtained in step (3) is condensed by a tap water condensing device and then flows into an oil-water separation device for oil-water separation to obtain 75.20 g of cinnamon essential oil, and the yield of cinnamon essential oil is calculated to be 0.94%.

[0055] Comparative Example 2

[0056] This comparative example is a traditional water vapor extraction method for cinnamon essential oil, which comprises the following steps:

[0057] (1) Take 0.88 kg of cassia, 3.56 kg of cassia twig and 3.56 kg of cassia leaves, uniformly mix, dry in a 60°C oven, then mechanically crush, and then pass through a 60 mesh sieve to obtain cassia powder.

[0058] (2) Place the cassia powder obtained in step (1) in 48 L of 2wt% salt water, soak for 0.5 h, then filter, and place the filtered cassia powder in a steam extraction tank.

[0059] (3) Introduce uncatalyzed steam (uncatalyzed steam is obtained by direct evaporation of water) with a steam pressure of 0.2 MPa and an electrical conductivity of 0.02 ms / m into the extraction tank in step (2) to continuously extract for 6 h to obtain essential oil mixed steam.

[0060] (4) After condensing the essential oil mixed steam obtained in step (3) through a tap water condensing device, flow into an oil-water separation device for oil-water separation to obtain 60.00 g of cassia essential oil, and calculate that the cassia essential oil yield is 0.75%.

[0061] Test Example

[0062] This test example detects and analyzes the quality indicators of the cassia essential oil extracted in Examples 1-3 and Comparative Examples 1-2, mainly including color, state, aroma, oil yield and characteristic component content, etc.

[0063] The qualitative and quantitative test methods of the components of cassia essential oil are as follows:

[0064] The composition and proportion of each component of cassia essential oil are qualitatively and quantitatively analyzed by GC-MS / GC-FID, and the test method is as follows: accurately take 50 mg of cassia essential oil sample, dissolve in ethyl acetate, filter with a PTFE filter (0.22 μm), and then perform GC-MS / GC-FID analysis test. The test parameters are as follows: HP-5 capillary column (30.0 mm x 0.25 mm x 0.25 mm), vaporization chamber temperature: 250°C; detector temperature: 250°C; injection mode: split; split ratio 20:1; injection amount: 1.0 μL; column nitrogen flow rate: 3 mL / min; helium flow rate: 30 mL / min; air flow rate: 300 mL / min; temperature rising program: initial temperature 80°C, 3°C / min to 230°C and hold for 10 min.

[0065] The GC-MS spectrum of the cassia essential oil of Example 2 is shown in Figure 1 , wherein 1—cis-cinnamaldehyde; 2—trans-cinnamaldehyde; 3—coumarin; 4—cinnamyl acetate; 5—o-methoxycinnamaldehyde. From Figure 1As can be seen, the composition of the cinnamon essential oil extracted by the present application comprises cinnamaldehyde, coumarin, cinnamyl acetate and o-methoxycinnamaldehyde.

[0066] It is found that the quality indexes of the cinnamon essential oil of examples 1-3 and comparative examples 1-2 are shown in table 1.

[0067] Table 1 Quality indexes of the cinnamon essential oil of examples 1-3 and comparative examples 1-2

[0068]

[0069] As can be seen from table 1, the quality indexes of the cinnamon essential oil extracted by all the examples of the present application meet the theoretical quality evaluation standard. It can also be seen that the oil yield and cinnamaldehyde characteristic index of the cinnamon essential oil extracted by examples 1-3 of the present application are obviously higher than those of comparative examples 1-2, which indicates that the method of water vapor and water continuous extraction of cinnamon essential oil of the present application has more advantages in oil yield and cinnamaldehyde characteristic index than the traditional water extraction method and the traditional water vapor extraction method, and is more conducive to promoting industrial production.

[0070] The above only describes some embodiments of the present application. For those skilled in the art, without departing from the concept of the present application, several modifications and improvements can be made, which are all within the protection scope of the present application.

Claims

1. A process for the co-extraction of water and steam of essential oil from cinnamon characterized in that, The method comprises the following steps: S1, weighing and mixing cassia bark, cassia twig and cassia leaf, drying and then crushing, and sieving to obtain cassia powder; S2, placing the cassia powder obtained in step S1 in brine and soaking, then filtering, and putting the filtered cassia powder into an extraction tank, adding water, and stirring to obtain a mixture; S3, heating the mixture in the extraction tank in step S2 to micro-boiling, then continuously introducing catalytic water vapor above the liquid surface of the extraction tank, and continuously extracting for 1-3 h to obtain essential oil mixed with water vapor; the preparation method of the catalytic water vapor is as follows: passing water vapor through a column filled with a catalyst to obtain catalytic water vapor, the passing time is 20-60 s, and the temperature range is 100-130℃; wherein the catalyst is a mixture of foamed iron and foamed manganese in a mass ratio of 3:1; S4, condensing the essential oil mixed with water vapor obtained in step S3 through a condensing device, then flowing into an oil-water separation device for oil-water separation, and obtaining cassia essential oil.

2. The method of claim 1, wherein the water vapor co-water continuous extraction of the cinnamon essential oil is characterized by, In step S1, before crushing, the cassia bark, cassia twig and cassia leaf are impurity-removed, dried in a 60℃ oven, mechanically crushed after drying, and sieved through a 40-60 mesh sieve.

3. The method of claim 1 or 2, wherein the method is characterized by, In step S2, the concentration of the brine is 2-5 wt%, the mass ratio of the brine to the cassia powder is 5-7:1, and the soaking time is 0.5-3 h.

4. The method of claim 3, wherein the water vapor co-water continuous extraction of the cinnamon essential oil is characterized by, In step S2, the mass ratio of the water to the cassia powder is 7-15:

1.

5. The method of claim 3, wherein the water vapor co-water continuous extraction of the cinnamon essential oil is characterized by, In step S3, the temperature for heating the mixture in the extraction tank to micro-boiling is 90-100℃.

6. The method of claim 4 or 5, wherein the method is characterized by, In step S3, the position for introducing the catalytic water vapor into the extraction tank is 10-30 cm above the liquid surface.

7. The method of claim 1, wherein the water vapor co-water continuous extraction of cinnamon essential oil is characterized by, In step S3, the pressure of the catalytic water vapor is 0.1-0.3 MPa, and the conductivity is 0.2-0.4 ms / m.

8. The cassia essential oil extracted by the method of any one of claims 1-7.

9. The cinnamon essential oil of claim 8, wherein, The yield of the cassia essential oil is 1.3-2.1%, the percentage content of cinnamaldehyde in the cassia essential oil is 80.0-84.0 wt%, the percentage content of coumarin is 1.5-1.7 wt%, the percentage content of o-methoxycinnamaldehyde is 9.0-11.0 wt%, and the percentage content of cinnamyl acetate is 1.2-1.7 wt%.

Images