CN113073009A - Pretreatment drying method for simultaneously extracting industrial hemp aromatic water and improving CBD content of industrial hemp raw material - Google Patents
Pretreatment drying method for simultaneously extracting industrial hemp aromatic water and improving CBD content of industrial hemp raw material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
Abstract
The invention provides a pretreatment drying method for simultaneously extracting industrial hemp aromatic water and improving the CBD content of an industrial hemp raw material, belonging to the technical field of industrial hemp processing. The method mainly comprises the following steps: (1) taking industrial cannabis sativa flowers and/or leaves, performing vacuum microwave extraction and drying, and simultaneously condensing and collecting aromatic water. (2) And performing damp-heat decarboxylation by microwave to improve the content of CBD. (3) And (5) vacuum microwave drying. The method realizes the comprehensive utilization and extraction of aromatic water under low temperature and low oxygen conditions in the process of drying industrial hemp flowers and/or leaves, and the aromatic water is used for being added into downstream products of industrial hemp, so that the original fragrance and flavor of the industrial hemp are retained; meanwhile, the drying of industrial hemp is completed, the decarboxylation of CBDA is realized, and the dried industrial hemp flower and/or leaf raw material with the improved CBD content is obtained.
Description
Technical Field
The invention belongs to the technical field of industrial hemp flower and/or leaf processing, and particularly relates to a pretreatment drying method for simultaneously extracting industrial hemp aromatic water and improving the CBD content of an industrial hemp raw material.
Background
Industrial Hemp, also known as Hemp (Hemp), is a very low (< 0.3%) content of Tetrahydrocannabinol (THC), the seed, fiber, leaves and other by-products of which are widely used in the textile, materials, cosmetics, pharmaceutical and food industries. Cannabidiol (CBD) is an important non-psychoactive substance in China hemp, can antagonize hallucinogenic effect of THC, and has multiple physiological activities of antioxidation, antitumor, anti-inflammatory, antianxiety, antispasmodic, anti-drug resistance epilepsy and the like.
The industrial hemp flowers and/or leaves contain a large amount of volatile components, have the special fragrance of the industrial hemp flowers and/or leaves, can be used for the fragrance blending of downstream products of the industrial hemp, and highlight the characteristics and the identification degree of the downstream products of the industrial hemp.
At present, the domestic industrial hemp variety with the highest CBD content is 'Yunma No. 7', the CBD content of the variety is about 0.9-1.7%, and compared with foreign countries, the content is low, so that the industrial capacity of the CBD is low, the competitive advantage of enterprises is weak, but the breeding of the variety with high content has long period, large research and development investment and high risk.
The traditional steam distillation method for extracting aromatic water has the defects that the aromatic water is extracted under the conditions of high temperature and oxygen contact, materials extracted by the steam distillation method can be boiled, boiled and denatured, and the subsequent process is not easy to utilize. The research on extracting volatile oil by microwave is also reported, but the reported methods are all in a small test stage and are carried out under the conditions of oxygen and normal pressure, and the problems that the extraction temperature is high, the obtained components are easy to oxidize in the extraction process, steam is generated and easy to reflux, and the efficiency is low exist. At present, few reports are reported on the extraction and application of industrial cannabis sativa flower and/or leaf aromatic water.
The Chinese patent application with the patent application number of CN2018111122748.3 discloses a green solvent-free extraction method of essential oil of industrial cannabis sativa flowers and/or leaves, which is characterized in that fresh flowers and/or leaves of industrial cannabis sativa are selected and put into a microwave solvent-free extraction device, the microwave power is set to be 100-1000W, the extraction temperature is 100-150 ℃, and the extraction time is 5-120 minutes; during microwave solvent-free extraction and heating, evaporating liquid is collected by a condenser pipe, and finally, the cannabis sativa and/or leaf essential oil is obtained by an oil-water separator. However, the method is carried out under the aerobic and normal pressure conditions, and has the problems of high extraction temperature, easy oxidation of the obtained components in the extraction process, easy backflow of generated steam and low efficiency. The method and the process of the invention are fundamentally different from the aromatic water obtained by comprehensive utilization and extraction of vacuum microwave, on one hand, the invention is carried out under the vacuum condition, low temperature and low oxygen, low temperature circulating water is condensed, the extraction temperature is low, the condensation temperature is low, the obtained components are not easy to be oxidized in the extraction process, the generated steam is not easy to be brought away in vacuum, the reflux is not easy, and the efficiency is higher. On the other hand, the invention is not only a single technical unit for extracting the aromatic water, but also an integrated innovation with the moist-heat decarboxylation and drying process, thereby realizing the comprehensive utilization of the aromatic water.
In order to solve the problem of low content of CBD in industrial hemp flowers and/or leaves, cannabidiolic acid (CBDA) contained in the industrial hemp flowers and/or leaves can be converted into CBD after decarboxylation under certain conditions, which is an effective way for improving the content of CBD in industrial hemp raw materials, the traditional main method is high-temperature and high-heat decarboxylation under dry conditions, and the patent application with the Chinese patent application number of CN201910868592.1 discloses 'a pretreatment method for improving the content of CBD in industrial hemp and optimization thereof', the method achieves the purpose of improving the content of CBD by high-temperature drying and conversion, and the influence of the method on the content of CBD in the raw materials is considered from two parameters of temperature and time, so that the optimal high-temperature conversion condition is preferably selected: the drying conversion temperature is 100-150 ℃, the drying conversion time is 1-5 h, and the CBD content of the industrial hemp is obviously improved after the drying conversion. However, the method has the problems of high temperature, large temperature fluctuation, poor controllability of the decarboxylation end point, decarboxylation and CBD degradation damage caused by overhigh temperature or overlong time, and insufficient material thermal denaturation and local gelatinization.
At present, microwave-assisted cannabidiol extraction is reported, and a patent application with the Chinese invention patent application number of CN201910358996.6 discloses a novel method for extracting Cannabidiol (CBD) from industrial cannabis sativa, wherein microwave pretreatment is adopted in the method, ethanol with the volume concentration of 75-95% is used as a solvent, and microwave is adopted to heat the solution to a certain temperature for extraction for 5-10min at 200-500W; the method has the advantages of short extraction heating time, low activity loss, and high product purity. The method is essentially different from the microwave application of the invention, and the effect is different, the microwave of the invention is used in the extraction stage after adding solvent, and the purpose is to accelerate the dissolution of CBD, while the microwave of the invention is used in the pretreatment drying stage of raw materials, and the purpose is to distill aromatic water at low temperature, decarboxylate under low temperature and moist heat, and dry under low temperature.
Disclosure of Invention
The invention aims to solve the technical problems that the traditional decarboxylation drying method for improving the CBD content of the industrial cannabis sativa flowers and/or the leaves is high-temperature drying under the drying condition, the decarboxylation and the CBD degradation are simultaneously damaged, the temperature is high, the energy consumption is high, the period is long, and the aromatic water of the industrial cannabis sativa flowers and/or the leaves is not comprehensively utilized in the drying and decarboxylation process, so that downstream products do not have the special aroma of the industrial cannabis sativa, the characteristics of the products cannot be highlighted, and the like. The invention aims to provide a pretreatment drying method for simultaneously extracting industrial hemp aromatic water and improving the CBD content of an industrial hemp raw material, the industrial hemp aromatic water and application thereof.
In order to solve the technical problems and achieve the purpose of the invention, the invention is realized by the following technical scheme:
a pretreatment drying method for simultaneously extracting industrial hemp aromatic water and improving the CBD content of industrial hemp raw material comprises the following steps:
(1) cutting industrial hemp flowers and/or leaves into sections, opening a sealing door of a vacuum microwave dryer, putting the industrial hemp flowers and/or leaves into a drying disc in the vacuum microwave dryer, closing the sealing door without covering the drying disc, hermetically connecting a condenser on a vacuum tube of the vacuum microwave dryer, and hermetically connecting an aromatic water receiver at the lower end of the condenser;
(2) opening vacuum, adjusting a vacuum evacuation valve, screwing a sealing door, opening cooling water circulation in a condenser on a vacuum tube, opening microwaves to extract aromatic water and dry materials, and cooling a mixture of volatile components and water vapor in the vacuum tube by the condenser to flow into an aromatic water receiver;
(3) vacuum microwave extracting and drying until the materials are nearly dry, closing the microwave, closing the vacuum, unscrewing a sealing door, opening a vacuum emptying valve until no vacuum exists, taking down an aromatic water receiver below a condenser, and collecting the solution in the aromatic water receiver, namely the industrial hemp aromatic water;
(4) closing the cooling water circulation of the condenser, sealing and installing an aromatic water receiver at the lower end of the condenser, opening a sealing door, covering a cover on the drying tray provided with the industrial cannabis sativa flowers and/or leaves in the step (1), placing the drying tray provided with the industrial cannabis sativa flowers and/or leaves and covered with the cover into a vacuum microwave dryer, closing the sealing door and screwing, and starting microwaves to perform the damp-heat decarboxylation reaction;
(5) and (3) after the microwave wet heat decarboxylation, closing the microwave, opening the sealing door, taking out the drying disc, taking away the cover covered on the drying disc, putting the drying disc into a vacuum microwave dryer, opening the vacuum, adjusting the vacuum emptying valve, screwing the sealing door, and opening the microwave to further carry out vacuum microwave drying on the industrial cannabis flowers and/or leaves in the drying disc until the industrial cannabis flowers and/or leaves are dry, namely the dried industrial cannabis flowers and/or leaves with the improved CBD content are obtained.
Further, the industrial cannabis flowers and/or leaves in step (1) of the pretreatment drying method are fresh industrial cannabis flowers and/or leaves, or the industrial cannabis flowers and/or leaves in step (1) are industrial cannabis flowers and/or leaves with a moisture content of 40% or more.
Further, in the pretreatment drying method, in the step (2), the temperature of the cooling water in the condenser is 0 to 10 ℃. The temperature of the cooling water is preferably 0 ℃ to 4 ℃.
Further, the pretreatment drying method comprises the steps of (2) starting vacuum, adjusting a vacuum emptying valve, wherein the vacuum degree is-0.005 MPa to-0.1 MPa, and the temperature of starting microwave is 35-70 ℃.
Further, the material in the step (3) of the pretreatment drying method is nearly dry, and the moisture content of the material is 15-30%.
Further, the microwave is started to carry out the damp-heat decarboxylation reaction in the step (4) of the pretreatment drying method, wherein the microwave temperature is 90-110 ℃, and the time is 30 minutes-5 hours.
Further, the pretreatment drying method step (5) opens the vacuum, adjusts the vacuum emptying valve, the vacuum degree is-0.005 MPa to-0.1 MPa, and the temperature for opening the microwave is 45 ℃ to 100 ℃. The moisture content of the industrial cannabis flowers and/or leaves in the drying tray to the dry state is 0.1% -12.0%.
The invention also provides industrial hemp aromatic water which is prepared by the following method:
(1) taking industrial hemp flowers and/or leaves, cutting the industrial hemp flowers and/or leaves into sections, opening a sealing door of a vacuum microwave dryer, putting the industrial hemp flowers and/or leaves into a drying disc in the vacuum microwave dryer, closing the sealing door without covering the drying disc, connecting a condenser on a vacuum tube of the vacuum microwave dryer, and connecting the lower end of the condenser with an aromatic water receiver in a sealing manner;
(2) opening vacuum, adjusting a vacuum emptying valve, wherein the vacuum degree is-0.005 MPa to-0.1 MPa, tightly closing a sealing door, opening cooling water circulation in a condenser on a vacuum tube, wherein the temperature of the cooling water is 0-10 ℃, preferably the temperature of the cooling water is 0-4 ℃, opening microwaves for extracting aromatic water, the temperature of the microwaves is 35-70 ℃, and cooling a mixture of volatile components and water vapor in the vacuum tube by the condenser to flow into an aromatic water receiver;
(3) and (3) drying the materials by vacuum microwave until the moisture content of the materials is 15-30%, closing the microwave, closing the vacuum, unscrewing a sealing door, opening a vacuum emptying valve until no vacuum exists, taking down the aromatic water receiver below the condenser, and collecting the solution in the aromatic water receiver, namely the industrial hemp aromatic water.
Further, the industrial cannabis flowers and/or leaves used in the industrial cannabis aromatic water are fresh industrial cannabis flowers and/or leaves, or industrial cannabis flowers and/or leaves with the moisture content of more than 40%.
The invention also provides the application of the industrial hemp aromatic water added into downstream products for retaining the original fragrance, flavor or seasoning of industrial hemp, wherein the downstream products include but are not limited to food, health products, medicines or cosmetics.
The industrial hemp aromatic water is a volatile oil-water mixture of flowers and/or leaves of industrial hemp.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention overcomes the defects that the drying is carried out under the high-temperature aerobic condition in the traditional process by the vacuum microwave integrated process, and the defects that the aromatic water extraction and the drying of the industrial hemp flowers and/or leaves can not be carried out simultaneously are overcome, when the industrial hemp aromatic water is extracted, vacuum, microwave, cryocondensation combined action, realized that extract aromatic water and cryodrying go on simultaneously under low temperature and low oxygen condition, the comdenstion water circulative cooling aromatic water of lower temperature is not taken away by the vacuum, reached and extracted industrial hemp aromatic water and the effect that improves industrial hemp raw materials CBD content simultaneously under the low temperature low oxygen, the industrial hemp aromatic water of extraction does not contain the CBD composition, guaranteed that industrial hemp aromatic water is not by oxidation and high thermal destruction, the original fragrance of industrial hemp has been remain, the material is not oxidative destruction simultaneously, the energy consumption is reduced, the drying time has been shortened.
2. The method for extracting the industrial cannabis sativa and/or leaf aromatic water by combining vacuum, microwave and low-temperature condensation ensures that the aromatic water is not oxidized and damaged by high temperature due to low temperature and low oxygen, retains the original aroma of the aromatic water, and simultaneously realizes drying of the extracted material, thereby overcoming the defects that the aromatic water extracted by the traditional steam distillation method is extracted under the condition of high temperature and oxygen contact, the material extracted by the steam distillation method is boiled and boiled to be denatured, and the subsequent utilization is not good.
3. The invention firstly adopts vacuum microwave drying to quickly dry the industrial hemp flowers and/or leaves to the water content of 15-30 percent, then the moisture contained in the industrial hemp flowers and/or leaves absorbs the microwave to generate heat and form a large amount of hot steam under the normal pressure condition by the microwave, the high-temperature hot and humid steam is retained by covering a cover to promote the CBDA decarboxylation, the high-temperature hot and humid steam generated by the microwave has small temperature fluctuation range, easily controlled process parameters, no overheating, the contradiction of decarboxylation while CBD is degraded and destroyed when the time is overlong, the hot and humid condition is higher than that under the drying condition, the required temperature is lower, the decarboxylation reaction at lower temperature is realized, and the defects of the traditional high-temperature high-heat decarboxylation mode under the drying condition that the temperature is high, the temperature waviness is large, the controllability is poor, the decarboxylation efficiency is low, the CBD is degraded and destroyed, Lack of local gelatinization.
4. The invention comprehensively utilizes and extracts aromatic water under the conditions of vacuum microwave, low temperature and low oxygen, simultaneously dries, then performs microwave damp-heat decarboxylation, and further dries by vacuum microwave to obtain the industrial hemp flower and/or leaf raw material with low water content and improved CBD content. By the vacuum microwave integrated process, aromatic water is comprehensively utilized and extracted at low temperature and low oxygen, the CBDA decarboxylation is realized by the vacuum microwave at low temperature and moist heat, the CBD content is increased, the temperature time is well controlled, the moist heat temperature has limit, the ultra-high temperature cannot occur, the CBD is stable at the temperature, the decarboxylation and the CBD degradation cannot occur, and meanwhile, materials are dried. The method comprehensively extracts and utilizes the aromatic water in the decarboxylation drying process, improves the added value of products, greatly improves the productivity of industrial hemp flower and/or leaf raw materials subjected to decarboxylation drying, is simple, is easy to realize industrial production, and has low cost, low energy consumption and short period.
Detailed Description
The present invention will be further understood from the following specific examples, which are not intended to limit the invention thereto.
The content of CBD in the industrial cannabis flowers and/or leaves in the following examples was determined according to the method recommended in Yunnan province Standard DB 53/295.1-2009. The HPLC analysis conditions for determining the CBD content of aromatic water were determined according to the HPLC analysis conditions recommended in the method of Yunnan province Standard DB 53295.1-2009.
The same batch of industrial cannabis sativa flowers and leaves used in the following examples were harvested and naturally dried in the shade, and the total moisture content was found to be 11%, with the CBD content being 0.97%. After the treatment of the following examples 1 to 5, the CBD content of the industrial cannabis sativa flowers and/or leaves after the microwave wet-heat decarboxylation and vacuum microwave drying is remarkably improved.
The moisture content of the industrial cannabis flowers and leaves or the material in each of the following examples refers to the total moisture content of the industrial cannabis flowers and leaves after mixing.
Example 1
(1) Taking 10kg of fresh industrial hemp flowers and leaves, cutting the fresh industrial hemp flowers and leaves into sections, opening a sealing door of a vacuum microwave dryer, putting the industrial hemp flowers and leaves into a drying disc in the vacuum microwave dryer, closing the sealing door without covering the drying disc, connecting a condenser on a vacuum tube of the vacuum microwave dryer in a sealing manner, and connecting an aromatic water receiver at the lower end of the condenser in a sealing manner.
(2) Opening vacuum, adjusting a vacuum emptying valve, keeping the vacuum degree between-0.005 MPa and-0.03 MPa, screwing a sealing door, opening cooling water circulation in a condenser on a vacuum tube, keeping the temperature of the cooling water between 1 ℃ and 4 ℃, starting microwaves to extract aromatic water and dry materials, keeping the temperature of the microwaves between 50 ℃ and 70 ℃, and cooling a mixture formed by mixing volatile components in the vacuum tube and water vapor (water vapor generated by heating fresh industrial hemp flowers and leaves) by the condenser and flowing into an aromatic water receiver.
(3) And (3) performing vacuum microwave extraction and drying until the moisture content of the industrial hemp flowers and leaves is detected to be 30%, closing the microwave, closing the vacuum, unscrewing a sealing door, opening a vacuum emptying valve until no vacuum exists, taking down an aromatic water receiver below a condenser, collecting a solution in the aromatic water receiver to obtain 4.72L of industrial hemp aromatic water, and detecting to obtain the industrial hemp aromatic water without CBD components.
(4) Closing the cooling water circulation of the condenser, sealing and installing an aromatic water receiver at the lower end of the condenser, opening a sealing door, covering a cover on a drying tray which is provided with the industrial cannabis sativa flowers and leaves and has the moisture content of 30% detected in the step (3), placing the drying tray which is provided with the industrial cannabis sativa flowers and leaves and has the moisture content of 30% and is covered with the cover into a vacuum microwave dryer, closing the sealing door and screwing, starting microwaves to carry out the damp-heat decarboxylation reaction, raising the temperature to 90 ℃ of the microwaves, starting timing, controlling the microwave temperature fluctuation to be 90-110 ℃ and carrying out the microwaves for 30 minutes.
(5) Closing the microwave after the microwave is carried out for 30 minutes in the step (4), opening a sealing door, taking out a drying plate in a vacuum microwave dryer, taking a cover covered on the drying plate away, continuously putting the drying plate containing the industrial cannabis flowers and leaves into the vacuum microwave dryer, opening the vacuum, adjusting a vacuum emptying valve, keeping the vacuum degree at-0.03 MPa to-0.06 MPa, screwing the sealing door, opening the microwave, keeping the temperature of the microwave to fluctuate between 50 and 80 ℃, further carrying out vacuum microwave drying on the industrial cannabis flowers and leaves in the drying plate until the moisture content of the industrial cannabis flowers and leaves in the drying plate is 7 percent (the moisture content is 7 percent by sampling determination), closing the microwave, unscrewing the sealing door, closing the vacuum, opening the emptying valve, emptying, opening the sealing door, taking out materials, and obtaining dried industrial cannabis flowers and leaves raw materials with the improved CBD content, the weight of the product was 1.32Kg dry, with a moisture content of 7% and a CBD content of 1.21% as determined.
After the same batch of industrial hemp flowers and leaves which are compared before decarboxylation are collected and naturally dried in the shade, the total moisture content is detected to be 11 percent, and the CBD content is 0.97 percent. Example 1 increased CBD content by 24.74%.
Example 2
Example 2 the procedure was the same as in example 1 except that the following procedure was followed with different specific parameters.
In the step (2), the vacuum degree is maintained at-0.04 MPa to-0.05 MPa, the temperature of cooling water is 5 ℃ to 8 ℃, and the microwave temperature is maintained at 40 ℃ to 65 ℃.
And (3) performing vacuum microwave extraction and drying until the moisture content of the material is 24% by material sampling detection, collecting 4.45L of the obtained industrial hemp aromatic water, and detecting to obtain the industrial hemp aromatic water without CBD components.
And (4) opening a sealing door, covering a cover on a drying tray filled with the industrial cannabis sativa flowers and leaves with the detected moisture content of 24%, putting the drying tray filled with the industrial cannabis sativa flowers and leaves with the detected moisture content of 24% and covered with the cover into a vacuum microwave dryer, closing the sealing door and screwing. When the microwave is started to carry out the damp-heat decarboxylation reaction, the temperature is raised to the microwave temperature of 90 ℃, the timing is started, the microwave temperature fluctuation is 90-110 ℃, and the microwave lasts for 1.5 hours.
And (5) turning off the microwave after the microwave in the step (4) is used for 1.5 hours. The vacuum degree is maintained between-0.07 MPa and-0.1 MPa when the vacuum emptying valve is adjusted. The microwave temperature is maintained to fluctuate between 45 ℃ and 80 ℃, and the vacuum microwave drying is further carried out until the moisture content of the industrial hemp flowers and leaves in the drying tray is 0.1 percent by sampling detection. The obtained dried raw material of dried industrial cannabis flowers and leaves with improved CBD content weighed 1.23Kg of dried product, the moisture was 0.1%, and the CBD content was 1.38% by detection.
In this example 2, after detecting that the same batch of industrial cannabis sativa flowers and leaves are naturally dried in the shade before the beginning of step (1), the CBD content is detected to be 0.97%, and in this example 2, the CBD content is increased by 42.27%.
Example 3
Example 3 the procedure was the same as in example 1 except that the following procedure was followed with different specific parameters.
The vacuum degree in the step (2) is maintained between-0.07 MPa and-0.1 MPa. The temperature of the cooling water is 9-10 ℃. The microwave temperature is maintained at 35-45 DEG C
And (3) performing vacuum microwave extraction and drying until the water content of the material is 15% in the material sampling detection. 3.73L of industrial hemp aromatic water is collected and detected, and the industrial hemp aromatic water does not contain CBD components.
And (4) opening a sealing door, covering a cover on a drying tray filled with the industrial cannabis sativa flowers and leaves with the detected moisture content of 15%, putting the drying tray filled with the industrial cannabis sativa flowers and leaves with the detected moisture content of 15% and covered with the cover into a vacuum microwave dryer, closing the sealing door and screwing. When the microwave is started to carry out the damp-heat decarboxylation reaction, the temperature is raised to the microwave temperature of 90 ℃, the timing is started, the microwave temperature fluctuation is 90-110 ℃, and the microwave lasts for 3 hours.
And (5) turning off the microwave after the microwave is used for 3 hours in the step (4). The vacuum is started, and the vacuum degree is maintained between-0.005 MPa and-0.029 MPa when the vacuum emptying valve is adjusted. The microwave temperature is maintained to be fluctuated between 55 ℃ and 99 ℃, the vacuum microwave drying is further carried out until the moisture content of the industrial hemp flowers and leaves in the drying tray is 12 percent by sampling detection, the obtained dried industrial hemp flowers raw material with the improved CBD content weighs 1.39Kg of dried product, the moisture content is 12 percent, and the detected CBD content is 1.59 percent.
In this example 3, before the beginning of step (1), the same batch of industrial cannabis sativa flowers and leaves are naturally dried in the shade after being harvested, and the CBD content is detected to be 0.97%, which is 63.92% higher in this example 3.
Example 4
Example 4 the procedure was the same as in example 1 except that the following procedure was carried out with different specific parameters.
Step (1) 10kg of industrial cannabis flowers and leaves with 40% moisture content are taken.
The vacuum degree in the step (2) is maintained between-0.02 MPa and-0.049 MPa. The temperature of the cooling water is 1-3 ℃. The microwave temperature is maintained at 41-59 ℃.
And (3) performing vacuum microwave extraction and drying until the water content of the material is 18% in the material sampling detection. 1.67L of industrial hemp aromatic water was collected and detected to be free of CBD component.
And (4) opening a sealing door, covering a cover on a drying tray filled with the industrial cannabis sativa flowers and leaves with the detected moisture content of 18%, putting the drying tray filled with the industrial cannabis sativa flowers and leaves with the detected moisture content of 18% and covered with the cover into a vacuum microwave dryer, closing the sealing door and screwing. And (3) starting microwaves to carry out the damp-heat decarboxylation reaction, heating to the microwave temperature of 90 ℃, starting timing, wherein the microwave temperature fluctuation is 90-110 ℃, and carrying out the microwaves for 4 hours.
And (5) turning off the microwave after the microwave in the step (4) is used for 4 hours. The vacuum degree is maintained between-0.05 MPa and-0.07 MPa when the vacuum emptying valve is adjusted. The microwave temperature is maintained to fluctuate between 45 ℃ and 90 ℃, and the vacuum microwave drying is further carried out until the moisture content of the industrial cannabis sativa flowers and the leaves in the drying tray is 6%, the obtained dried industrial cannabis sativa dried product raw material with the improved CBD content weighs 5.33Kg of dried product, the moisture content is 6%, and the detected CBD content is 1.67%. In this example 4, before the beginning of step (1), the same batch of industrial cannabis sativa flowers and leaves are naturally dried in the shade after being harvested, and the CBD content is detected to be 0.97%, which is 72.16% higher in this example 4.
Example 5
Example 5 the procedure was the same as in example 1 except that the following procedure was followed with different specific parameters.
Step (1) 10kg of industrial cannabis sativa and leaves with a moisture content of 57% are taken.
The vacuum degree in the step (2) is maintained between-0.02 MPa and-0.04 MPa. The temperature of the cooling water is 8-10 ℃, and the microwave temperature is maintained at 45-70 ℃.
And (3) performing vacuum microwave extraction and drying until the moisture content of the material is 26% by sampling detection. 1.55L of industrial hemp aromatic water is collected and detected, and the industrial hemp aromatic water does not contain CBD components.
And (4) opening a sealing door, covering a cover on a drying tray filled with the industrial cannabis flowers and leaves with the moisture content of the detected material of 26%, putting the drying tray filled with the industrial cannabis flowers and leaves with the moisture content of the detected material of 26% and covered with the cover into a vacuum microwave dryer, closing the sealing door and screwing. And (3) starting microwaves to carry out the damp-heat decarboxylation reaction, heating to the microwave temperature of 90 ℃, starting timing, wherein the microwave temperature fluctuation is 90-110 ℃, and carrying out the microwaves for 5 hours.
And (5) turning off the microwave after the microwave in the step (4) is turned off for 5 hours. The vacuum degree is maintained between-0.05 MPa and-0.07 MPa when the vacuum emptying valve is adjusted. The microwave temperature is maintained to fluctuate between 44 ℃ and 89 ℃, and the vacuum microwave drying is further carried out until the moisture content of the industrial hemp flowers and leaves in the drying tray is 4 percent by sampling detection. The dried industrial cannabis sativa raw material with the improved CBD content weighed 4.12Kg of dried product, had a moisture content of 4% and was tested to have a CBD content of 1.63%.
In this example 5, before the beginning of step (1), the same batch of industrial cannabis sativa flowers and leaves are naturally dried in the shade after being harvested, and the CBD content is detected to be 0.97%, which is 68.04% higher in this example 5.
The above examples show that: the method can simultaneously obtain industrial hemp aromatic water and dry industrial hemp flower and/or leaf dry product raw materials with the CBD content improved. 10kg of fresh industrial hemp flowers and leaves or 10kg of industrial hemp flowers and leaves with the water content of more than 40 percent can produce 1.55L-4.72L of industrial hemp aromatic water, the industrial hemp aromatic water retains the original fragrance and flavor of industrial hemp, the extracted aromatic water does not contain CBD, and the aromatic water can be added into downstream products for retaining the original fragrance, flavor or seasoning of industrial hemp, and the downstream products include but are not limited to food, health products, medicines or cosmetics. The obtained dried industrial cannabis flowers and dried leaves raw materials with the improved CBD content are improved by 24.74-72.16% compared with the CBD content of the natural dried industrial cannabis flowers and leaves after the same batch of industrial cannabis flowers and leaves are harvested, and the method provides high-quality raw materials for the CBD industry, saves raw material resources, and has better economic benefit and production benefit.
Claims (10)
1. A pretreatment drying method for simultaneously extracting industrial hemp aromatic water and improving the CBD content of industrial hemp raw materials is characterized by comprising the following steps:
(1) cutting industrial hemp flowers and/or leaves into sections, opening a sealing door of a vacuum microwave dryer, putting the industrial hemp flowers and/or leaves into a drying disc in the vacuum microwave dryer, closing the sealing door without covering the drying disc, hermetically connecting a condenser on a vacuum tube of the vacuum microwave dryer, and hermetically connecting an aromatic water receiver at the lower end of the condenser;
(2) opening vacuum, adjusting a vacuum evacuation valve, screwing a sealing door, opening cooling water circulation in a condenser on a vacuum tube, opening microwaves to extract aromatic water and dry materials, and cooling a mixture of volatile components and water vapor in the vacuum tube by the condenser to flow into an aromatic water receiver;
(3) vacuum microwave extracting and drying until the materials are nearly dry, closing the microwave, closing the vacuum, unscrewing a sealing door, opening a vacuum emptying valve until no vacuum exists, taking down an aromatic water receiver below a condenser, and collecting the solution in the aromatic water receiver, namely the industrial hemp aromatic water;
(4) closing the cooling water circulation of the condenser, sealing and installing an aromatic water receiver at the lower end of the condenser, opening a sealing door, covering a cover on the drying tray provided with the industrial cannabis sativa flowers and/or leaves in the step (1), placing the drying tray provided with the industrial cannabis sativa flowers and/or leaves and covered with the cover into a vacuum microwave dryer, closing the sealing door and screwing, and starting microwaves to perform the damp-heat decarboxylation reaction;
(5) and (3) after the microwave wet heat decarboxylation, closing the microwave, opening the sealing door, taking out the drying disc, taking away the cover covered on the drying disc, putting the drying disc into a vacuum microwave dryer, opening the vacuum, adjusting the vacuum emptying valve, screwing the sealing door, and opening the microwave to further carry out vacuum microwave drying on the industrial cannabis flowers and/or leaves in the drying disc until the industrial cannabis flowers and/or leaves are dry, namely the dried industrial cannabis flowers and/or leaves with the improved CBD content are obtained.
2. The pretreatment drying method for simultaneously extracting industrial hemp aromatic water and increasing the CBD content of industrial hemp raw material according to claim 1, wherein: the industrial cannabis flowers and/or leaves in the step (1) are fresh industrial cannabis flowers and/or leaves, or the industrial cannabis flowers and/or leaves in the step (1) are industrial cannabis flowers and/or leaves with the moisture content of more than 40%.
3. The pretreatment drying method for simultaneously extracting industrial hemp aromatic water and increasing the CBD content of industrial hemp raw material according to claim 1, wherein: in the step (2), the temperature of the cooling water in the condenser is 0-10 ℃.
4. The pretreatment drying method for simultaneously extracting industrial hemp aromatic water and increasing the CBD content of industrial hemp raw material according to claim 1, wherein: and (3) starting vacuum in the step (2), adjusting a vacuum emptying valve, wherein the vacuum degree is-0.005 MPa to-0.1 MPa, and the temperature of starting the microwave is 35-70 ℃.
5. The pretreatment drying method for simultaneously extracting industrial hemp aromatic water and increasing the CBD content of industrial hemp raw material according to claim 1, wherein: the material in the step (3) is nearly dry, and the moisture content of the material is 15-30%.
6. The pretreatment drying method for simultaneously extracting industrial hemp aromatic water and increasing the CBD content of industrial hemp raw material according to claim 1, wherein: and (4) starting microwaves to carry out the damp-heat decarboxylation reaction, wherein the temperature of the microwaves is 90-110 ℃, and the time is 30 minutes-5 hours.
7. The pretreatment drying method for simultaneously extracting industrial hemp aromatic water and increasing the CBD content of industrial hemp raw material according to claim 1, wherein: and (5) starting vacuum, adjusting a vacuum emptying valve, wherein the vacuum degree is-0.005 MPa to-0.1 MPa, and the temperature for starting the microwave is 45-100 ℃. The moisture content of the industrial cannabis flowers and/or leaves in the drying tray to the dry state is 0.1% -12.0%.
8. The industrial hemp aromatic water is characterized by being prepared by the following method:
(1) taking industrial hemp flowers and/or leaves, cutting the industrial hemp flowers and/or leaves into sections, opening a sealing door of a vacuum microwave dryer, putting the industrial hemp flowers and/or leaves into a drying disc in the vacuum microwave dryer, closing the sealing door without covering the drying disc, connecting a condenser on a vacuum tube of the vacuum microwave dryer, and connecting the lower end of the condenser with an aromatic water receiver in a sealing manner;
(2) opening vacuum, adjusting a vacuum emptying valve, closing a sealing door, opening cooling water circulation in a condenser, wherein the temperature of the cooling water is 0-10 ℃, opening microwaves for extracting aromatic water, the temperature of the microwaves is 35-70 ℃, and cooling a mixture of volatile components and water vapor in a vacuum tube by the condenser to flow into an aromatic water receiver;
(3) and (3) drying the materials by vacuum microwave until the moisture content of the materials is 15-30%, closing the microwave, closing the vacuum, unscrewing a sealing door, opening a vacuum emptying valve until no vacuum exists, taking down the aromatic water receiver below the condenser, and collecting the solution in the aromatic water receiver, namely the industrial hemp aromatic water.
9. The industrial hemp aromatic water of claim 8, wherein: the industrial cannabis flowers and/or leaves in the step (1) are fresh industrial cannabis flowers and/or leaves, or the industrial cannabis flowers and/or leaves in the step (1) are industrial cannabis flowers and/or leaves with the moisture content of more than 40%.
10. Use of an industrial hemp aromatic water according to claim 8 or 9 added to downstream products including but not limited to food, health care, pharmaceutical or cosmetic products for retaining the original aroma, flavor or taste of industrial hemp.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6128831A (en) * | 1999-06-03 | 2000-10-10 | Durance; Timothy Douglas | Process for drying medicinal plants |
| US20040049059A1 (en) * | 2000-10-17 | 2004-03-11 | Adam Mueller | Method for producing an extract from cannabis plant matter, containing a tetrahydrocannabinol and a cannabidiol and cannabis extracts |
| US20150313273A1 (en) * | 2012-11-16 | 2015-11-05 | Nuwave Research Inc. | Apparatus and method for dehydration using microwave radiation |
| CN105258480A (en) * | 2014-07-18 | 2016-01-20 | 陈长清 | Efficient continuous vacuum microwave drying machine |
| CN205957663U (en) * | 2016-08-26 | 2017-02-15 | 江西锦程农业开发有限公司 | Chrysanthemum tea vacuum microwave drying equipment |
| US20180000857A1 (en) * | 2016-06-29 | 2018-01-04 | CannScience Innovations Inc. | Decarboxylated cannabis resins, uses thereof and methods of making same |
| CN108949363A (en) * | 2018-09-26 | 2018-12-07 | 常德华馥生物技术有限公司 | A kind of Solventless Extraction Process of industrial hemp floral leaf essential oil |
| US20200246495A1 (en) * | 2017-08-30 | 2020-08-06 | Enwave Corporation | Method and Apparatus for Pasteurizing and Dehydrating Cannabis |
| US20210023471A1 (en) * | 2017-04-18 | 2021-01-28 | Premium Extracts, Inc. | Method and apparatus for dehydration and decarboxylation of cannabis |
| CN112386948A (en) * | 2020-10-30 | 2021-02-23 | 云南芙雅生物科技有限公司 | Decarboxylation of cannabidiolic acid in industrial cannabis extracts |
-
2021
- 2021-04-21 CN CN202110429927.7A patent/CN113073009A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6128831A (en) * | 1999-06-03 | 2000-10-10 | Durance; Timothy Douglas | Process for drying medicinal plants |
| US20040049059A1 (en) * | 2000-10-17 | 2004-03-11 | Adam Mueller | Method for producing an extract from cannabis plant matter, containing a tetrahydrocannabinol and a cannabidiol and cannabis extracts |
| US20150313273A1 (en) * | 2012-11-16 | 2015-11-05 | Nuwave Research Inc. | Apparatus and method for dehydration using microwave radiation |
| CN105258480A (en) * | 2014-07-18 | 2016-01-20 | 陈长清 | Efficient continuous vacuum microwave drying machine |
| US20180000857A1 (en) * | 2016-06-29 | 2018-01-04 | CannScience Innovations Inc. | Decarboxylated cannabis resins, uses thereof and methods of making same |
| CN205957663U (en) * | 2016-08-26 | 2017-02-15 | 江西锦程农业开发有限公司 | Chrysanthemum tea vacuum microwave drying equipment |
| US20210023471A1 (en) * | 2017-04-18 | 2021-01-28 | Premium Extracts, Inc. | Method and apparatus for dehydration and decarboxylation of cannabis |
| US20200246495A1 (en) * | 2017-08-30 | 2020-08-06 | Enwave Corporation | Method and Apparatus for Pasteurizing and Dehydrating Cannabis |
| CN108949363A (en) * | 2018-09-26 | 2018-12-07 | 常德华馥生物技术有限公司 | A kind of Solventless Extraction Process of industrial hemp floral leaf essential oil |
| CN112386948A (en) * | 2020-10-30 | 2021-02-23 | 云南芙雅生物科技有限公司 | Decarboxylation of cannabidiolic acid in industrial cannabis extracts |
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