CN112221192A - Supercritical extraction method of bamboo green skin layer wax - Google Patents
Supercritical extraction method of bamboo green skin layer wax Download PDFInfo
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- CN112221192A CN112221192A CN202011101735.5A CN202011101735A CN112221192A CN 112221192 A CN112221192 A CN 112221192A CN 202011101735 A CN202011101735 A CN 202011101735A CN 112221192 A CN112221192 A CN 112221192A
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- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
Abstract
The invention discloses a supercritical extraction method of bamboo green skin layer wax, which comprises the following process steps of 1) drying a bamboo raw material until the water content is 8-12%; 2) crushing the bamboo raw material to 10-20 meshes; 3) placing the bamboo powder in supercritical CO2Adding entrainer into the extraction device, extracting for 90min, and collecting the extract from the separation kettle; 4) and (4) carrying out rotary evaporation on the extract liquor to remove the entrainer to obtain the bamboo wax. The method for extracting the bamboo green skin wax provided by the invention has the advantages of simple process, greenness, no toxicity, high bamboo wax extraction rate and high bamboo wax purity, can realize industrial and large-scale production, accords with the national sustainable development strategy, provides a new way for utilizing bamboo processing residues, is beneficial to reducing resource waste and improving the economic value of bamboo, and has high-efficiency economic benefit and social benefit.
Description
Technical Field
The invention relates to a method for extracting bamboo green skin layer wax, belonging to the technical field of agricultural and forestry biomaterials and the field of solid waste utilization.
Background
In recent years, environmental protection is increasingly emphasized in various countries, global wood supply is gradually reduced, reasonable utilization and development of bamboo resources are increasingly emphasized, and bamboo products are becoming one of important consumer goods in developed countries and regions. The bamboo resource cultivation and processing utilization technology in China leads the world and occupies a great position in the global bamboo industry. At present, the bamboo industry in China forms a new industry with potential and vitality from resource cultivation, processing and utilization to export trade and then ecological travel of the bamboo industry. The bamboo material is composed of bamboo green, bamboo yellow and bamboo flesh, the bamboo green is the outermost bamboo skin part of the bamboo culm in terms of color, the bamboo green is green when fresh and is called as the bamboo green, and the surface of the bamboo with yellow in the cavity is called as the bamboo yellow. The surface of the bamboo green is provided with a wax layer, and the bamboo green has super-hydrophobicity and antibacterial performance. When the bamboo is processed, the wax layer of the bamboo green influences the adhesion of the adhesive and the infiltration of the coating, so the bamboo green and the wax layer need to be removed. Therefore, a large amount of bamboo green waste is generated in bamboo processing, and meanwhile, fresh leaves and waste surfaces of branches of bamboos also have a large amount of skin wax, and the waste is green when fresh, and is called bamboo green waste.
At present, the requirement on the utilization of environmental solid wastes in bamboo processing is higher and higher, and the resource utilization of bamboo green wastes also urgently needs high-precision technology leading. The natural waxy components remained in the bamboo green waste materials are environment-friendly and nontoxic, have good adaptability to human bodies and sustainable sources, and are a natural waxy component resource with great development potential.
The existing bamboo green husk layer wax extraction process comprises two types of traditional mechanical separation of bamboo wax and organic solvent extraction of bamboo wax. The yield of the mechanical separation wax is low in the bamboo processing process, a large amount of impurities are doped, the purity is low, and the mechanical separation wax is difficult to be applied as a wax raw material. Although the wax extracted by using the organic solvent has high purity, the organic solvent process causes certain pollution to the environment and is not beneficial to the implementation of the national sustainable development strategy. Supercritical CO2The extraction technology is a new technology researched and developed in recent decades, has the advantages of normal temperature, no toxicity, no solvent residue, environmental protection, easy control of operation parameters, short extraction time, high product quality and the like, is particularly suitable for separation and refining of heat-instable natural products and physiologically active substances, and has wide application prospect in the aspect of extraction of lipids and active substances. The invention aims at the current application situation of the technology for extracting the bamboo green skin layer wax and combines the supercritical CO2An extraction technology, researches and designs an environment-friendly high-efficiency new technology for extracting the wax of the green bamboo peel layer
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the method for extracting the bamboo green skin layer wax, which is environment-friendly, non-toxic and high in practicability. Namely, high-purity natural wax is efficiently separated from the bamboo green raw material and the waste material containing the skin wax component in the bamboo processing residue. The separated bamboo wax can be applied to the fields of food, cosmetics, machinery, construction, chemical industry, medicine and the like. The technical scheme of the invention comprises the following process steps:
s1, drying the raw bamboo green until the water content is 8-12%, and removing impurities affecting wax extraction such as sand, soil and the like;
s2, smashing the bamboo raw material to 10-20 meshes;
s3 placing the bamboo powder in supercritical CO2Adding entrainer into the extraction device, extracting for 90min, and collecting the extract from the separation kettle;
s4, removing entrainer from the extract to obtain bamboo wax.
In the above-mentioned method, the first step of the method,
the supercritical CO2The temperature of the extraction device is 35-55 ℃, the pressure is 25-45 MPa, the temperature of the separation kettle is 20-30 ℃, and the pressure of the separation kettle is 5-15 MPa; the entrainer is 95 wt% ethanol, and the material-liquid ratio is 1: 0.8-1: 1.2.
The entrainer removal temperature is less than 80 ℃.
The invention also discloses the application of the bamboo wax prepared by the method in the fields of food, cosmetics, machinery, construction, chemical industry, medicine and the like.
The method for extracting the bamboo wax provided by the invention is simple in process, green and non-toxic, high in bamboo wax extraction rate and high in bamboo wax purity, can realize industrial and large-scale production, accords with the national sustainable development strategy, provides a new way for utilizing bamboo processing residues, is beneficial to reducing resource waste and improving the economic value of bamboo, and has efficient economic and social benefits.
Drawings
FIG. 1 influence of the moisture content of bamboo green waste on the yield of wax
FIG. 2 influence of bamboo powder mesh number on bamboo wax yield
FIG. 3 influence of extraction temperature on bamboo wax yield
FIG. 4 Effect of extraction pressure on bamboo wax yield
FIG. 5 Effect of separation temperature on bamboo wax yield
FIG. 6 Effect of separation pressure on bamboo wax yield
FIG. 7 Effect of extract-to-liquid ratio (amount of entrainer) on bamboo wax yield
FIG. 8 Effect of extraction time on bamboo wax yield
Detailed Description
Materials and methods
Respectively drying the bamboo green waste materials to different water contents (0-4%, 4-8%, 8-12%, 12-16% and 16-20%);
1. then screening bamboo powder with different meshes (10 meshes, 20 meshes, 30 meshes, 40 meshes and 50 meshes);
2. supercritical CO2The extraction equipment, Huaan supercritical extraction apparatus (model: HA120-50-01), south Tong City Huaan supercritical extraction Co., Ltd;
3. the formula of extraction yield is as follows:
bamboo wax yield (%) ═ m0/m)×100％
Wherein: m, the quality of the moso bamboo green dry powder;
m0and extracting and separating to remove the mass of the entrainer.
When the yield of the extracted wax exceeds 1 percent, the method is regarded as industrialized production, and the yield of the bamboo wax is more than or equal to 2 percent selected in the process optimization as the optimized process parameter range.
Single factor experiment of supercritical extraction
(1) Influence of water content of bamboo green waste on bamboo wax yield
The fixed conditions are as follows: the extraction mesh number is 20 meshes, and the extraction material-liquid ratio is 1:1.2, the extraction time is 90min, the extraction temperature is 45 ℃, the extraction pressure is 35MPa, the separation temperature is 25 ℃, and the separation pressure is 10 MPa. And (3) investigating the influence of the water content (0-4%, 4-8%, 8-12%, 12-16% and 16-20%) of the bamboo green crushed aggregates on the extraction rate, and calculating the extraction yield according to a formula.
The effect of water content on wax yield is shown in FIG. 1.
As shown in figure 1, when the water content of the bamboo green crushed aggregates is 8-12%, the yield of the bamboo wax is more than or equal to 2%, and therefore, the water content of 8-12% is selected as the process range for extracting the bamboo wax.
(2) Influence of bamboo powder mesh number on bamboo wax yield
The fixed conditions are as follows: the water content of the bamboo green crushed aggregates is 8-12%, and the ratio of the extraction material to the extraction liquid is 1:1.2, the extraction time is 90min, the extraction temperature is 45 ℃, the extraction pressure is 35MPa, the separation temperature is 25 ℃, and the separation pressure is 10 MPa. And (4) observing the influence of the extraction mesh number (10 meshes, 20 meshes, 30 meshes, 40 meshes and 50 meshes) on the extraction rate, and calculating the extraction rate according to a formula. The effect of the number of bamboo powder on the yield of bamboo wax is shown in figure 2.
When the mesh number is 10-20 meshes, the yield of the bamboo wax is more than or equal to 2 percent, so that the mesh number of 10-20 meshes is selected as the process range for extracting the bamboo wax.
(3) Influence of extraction temperature on bamboo wax yield
The fixed conditions are as follows: the water content of the bamboo green crushed aggregates is 8-12%, the extraction mesh number is 20 meshes, and the ratio of the extraction material to the extraction liquid is 1:1.2, the extraction time is 90min, the extraction pressure is 35MPa, the separation temperature is 25 ℃, and the separation pressure is 10 MPa. The yield was calculated according to the formula by examining the influence of the extraction temperature (25 ℃, 35 ℃, 45 ℃, 55 ℃, 65 ℃) on the extraction rate, and the results are shown in FIG. 3.
When the extraction temperature is 35-55 ℃, the yield of the bamboo wax is more than or equal to 2 percent, so the extraction temperature of 35-55 ℃ is selected as the process range for extracting the bamboo wax.
(4) Influence of extraction pressure on bamboo wax yield
The fixed conditions are as follows: the water content of the bamboo green crushed aggregates is 8-12%, the extraction mesh number is 20 meshes, and the ratio of the extraction material to the extraction liquid is 1:1.2, the extraction time is 90min, the extraction temperature is 45 ℃, the separation temperature is 25 ℃, and the separation pressure is 10 MPa. The influence of the extraction pressure (15MPa, 25MPa, 35MPa, 45MPa, 55MPa) on the extraction yield is examined, the extraction yield is calculated according to a formula, and the result is shown in figure 4.
When the extraction pressure is 25-45 MPa, the yield of the bamboo wax is more than or equal to 2 percent, so the extraction pressure of 25-45 MPa is selected as the process range for extracting the bamboo wax.
(5) Influence of separation temperature on bamboo wax yield
The fixed conditions are as follows: the water content of the bamboo green crushed aggregates is 8-12%, the number of extraction meshes is 20 meshes, and the ratio of the extraction material to the extraction liquid is 1:1.2, the extraction time is 90min, the extraction temperature is 45 ℃, the extraction pressure is 35MPa, and the separation pressure is 10 MPa. The extraction yield was calculated according to the formula, considering the influence of the separation temperature (15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃) on the extraction yield, and the results are shown in FIG. 5.
When the extraction temperature is 20-30 ℃, the yield of the bamboo wax is more than or equal to 2 percent, so the extraction temperature of 20-30 ℃ is selected as the process range for extracting the bamboo wax.
(6) Influence of separation pressure on bamboo wax yield
The fixed conditions are as follows: the water content of the bamboo green crushed aggregates is 8-12%, the number of extraction meshes is 20 meshes, and the ratio of the extraction material to the extraction liquid is 1:1.2, the extraction time is 90min, the extraction temperature is 45 ℃, the extraction pressure is 35MPa, and the separation temperature is 25 ℃. The influence of the separation pressure (0MPa, 5MPa, 10MPa, 15MPa, 20MPa) on the extraction yield was examined, and the extraction yield was calculated according to the formula, and the results are shown in FIG. 6.
When the extraction pressure is 5-15 MPa, the yield of the bamboo wax is more than or equal to 2 percent, so the extraction pressure of 5-15 MPa is selected as the process range for extracting the bamboo wax.
(7) Influence of extract-to-liquid ratio (amount of entrainer) on bamboo wax yield
The fixed conditions are as follows: the water content of the bamboo green crushed aggregates is 8-12%, the number of extraction meshes is 20 meshes, and the ratio of the extraction material to the extraction liquid is 1:1.2, the extraction time is 90min, the extraction temperature is 45 ℃, the extraction pressure is 35MPa, the separation temperature is 25 ℃, and the separation pressure is 10 MPa. The influence of the ratio of the extraction materials to the liquid (1:0.6, 1:0.8, 1:1, 1:1.2, 1:1.4) on the extraction yield was examined, and the yield was calculated according to the formula, and the results are shown in FIG. 7.
When the ratio of the extraction materials to the liquid is 1: 0.8-1: 1.2, the yield of the bamboo wax is more than or equal to 2 percent, so the extraction material-liquid ratio is selected to be 1: 0.8-1: 1.2 the process range for extracting the bamboo wax.
(8) Influence of extraction time on bamboo wax yield
The fixed conditions are as follows: the water content of the bamboo green crushed aggregates is 8-12%, the number of extraction meshes is 20 meshes, and the ratio of the extraction material to the extraction liquid is 1:1.2, the extraction temperature is 45 ℃, the extraction pressure is 35MPa, the separation temperature is 25 ℃, and the separation pressure is 10 MPa. Examining the influence of the extraction time (30min, 60min, 90min, 120min, 150min) on the extraction yield, the bamboo wax yield was calculated according to the formula, and the results are shown in FIG. 8.
When the extraction time is more than or equal to 90min, the yield of the bamboo wax tends to be constant, so the extraction time of 90min is selected as the process condition for extracting the bamboo wax.
6. Detailed description of the preferred embodiments
Example 1:
a method for extracting bamboo wax from a raw bamboo green material comprises the following steps:
step 1), drying the bamboo raw material until the water content is 10%;
step 2) crushing the bamboo raw material to 10 meshes;
step 3) placing the bamboo powder in supercritical CO2In an extraction plant, supercritical CO2The temperature of the extraction device is 35 ℃, the pressure is 25MPa, the temperature of the separation kettle is 30 ℃, and the pressure of the separation kettle is 15 MPa; adding 95% ethanol as entrainer at a material-liquid ratio of 1:0.8, extracting for 90min, and collecting extractive solution from the separation kettle;
and 4) rotationally evaporating the extract liquor at 50 ℃ to remove the entrainer to obtain the bamboo wax, wherein the yield is 2.5-2.8%.
Example 2:
a method for extracting bamboo wax from a raw bamboo green material comprises the following steps:
step 1), drying the bamboo raw material until the water content is 9%;
step 2) crushing the bamboo raw material to 10 meshes;
step 3) placing the bamboo powder in a supercritical CO2 extraction device, wherein the temperature of the supercritical CO2 extraction device is 40 ℃, the pressure is 30MPa, the temperature of a separation kettle is 25 ℃, and the pressure of the separation kettle is 10 MPa; adding 95% ethanol as entrainer at a material-to-liquid ratio of 1:1, extracting for 90min, and collecting extractive solution from the separation kettle;
and 4) rotationally evaporating the extract liquor at 60 ℃ to remove the entrainer to obtain the bamboo wax, wherein the yield is 2.5-2.7%.
Example 3:
a method for extracting bamboo wax from a raw bamboo green material comprises the following steps:
step 1), drying the bamboo raw material until the water content is 8%;
step 2) crushing the bamboo raw material to 20 meshes;
step 3) placing the bamboo powder in supercritical CO2In an extraction plant, supercritical CO2The temperature of the extraction device is 45 ℃, the pressure is 35MPa, the temperature of the separation kettle is 20 ℃, and the pressure of the separation kettle is 5 MPa; adding 95% ethanol as entrainer at a material-to-liquid ratio of 1:1.2, extracting for 90min, and collecting extractive solution from the separation kettle;
and 4) rotationally evaporating the extract liquor at 70 ℃ to remove the entrainer to obtain the bamboo wax, wherein the yield is 2.6-3.1%.
Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the invention as defined by the appended claims. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A supercritical extraction method of bamboo green skin layer wax is characterized by comprising the following process steps:
s1, drying the bamboo green waste until the water content is 8-12%, and removing impurities affecting wax extraction, such as sand, soil and the like;
s2, smashing the bamboo green waste into 10-20 meshes of bamboo powder;
s3, placing the bamboo powder in supercritical CO2Adding entrainer into the extraction device, extracting for 90min, and collecting the extract from the separation kettle;
and S4, removing the entrainer from the extract to obtain the bamboo wax.
2. The supercritical extraction method of the bamboo green skin layer wax as claimed in claim 1, which is characterized in that:
the bamboo green waste material of S1 is a mixture of bamboo green skin waste materials with waxy skins, such as crushed bamboo skin, fresh bamboo leaves, bamboo branches, bamboo underground stems, etc. during the bamboo green removing process, or the bamboo green waste material extracted from bamboo wax by using only the crushed bamboo green skin peeled from the outer skin layer of the bamboo stem during the bamboo processing process to improve the extraction rate of waxy materials.
3. The supercritical extraction method of the bamboo green skin layer wax as claimed in claim 1, which is characterized in that:
the supercritical CO of S32The temperature of the extraction device is 35-55 ℃, the pressure is 25-45 MPa, the temperature of the separation kettle is 20-30 ℃, the pressure of the separation kettle is 5-15 MPa, the entrainer is 95 wt% ethanol, and the material-liquid ratio is 1: 0.8-1: 1.2.
4. The supercritical extraction method of the bamboo green skin layer wax as claimed in claim 1, which is characterized in that:
and S4, wherein the entrainer removal temperature is less than 80 ℃.
5. The bamboo wax obtained by the method of any one of claims 1 to 3, which can be used in the fields of food, cosmetics, machinery, construction, chemical industry, medicine, etc.
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Citations (4)
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|---|---|---|---|---|
| CN102051261A (en) * | 2010-12-01 | 2011-05-11 | 陕西农产品加工技术研究院 | Method for continuously extracting lacquer wax and lacquer by supercritical CO2 fluid |
| CN103705647A (en) * | 2014-01-02 | 2014-04-09 | 青岛农业大学 | Process method for extracting general flavone of golden camellia leaves by CO2 supercritical method |
| WO2014081881A2 (en) * | 2012-11-20 | 2014-05-30 | Andrew Paul Joseph | Fluid-based extractor |
| CN108892970A (en) * | 2018-05-07 | 2018-11-27 | 贵州西江阿幼民族文化博物馆有限公司 | A kind of extracting method and its application method of vegetalitas batik pigment |
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- 2020-10-15 CN CN202011101735.5A patent/CN112221192A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051261A (en) * | 2010-12-01 | 2011-05-11 | 陕西农产品加工技术研究院 | Method for continuously extracting lacquer wax and lacquer by supercritical CO2 fluid |
| WO2014081881A2 (en) * | 2012-11-20 | 2014-05-30 | Andrew Paul Joseph | Fluid-based extractor |
| CN103705647A (en) * | 2014-01-02 | 2014-04-09 | 青岛农业大学 | Process method for extracting general flavone of golden camellia leaves by CO2 supercritical method |
| CN108892970A (en) * | 2018-05-07 | 2018-11-27 | 贵州西江阿幼民族文化博物馆有限公司 | A kind of extracting method and its application method of vegetalitas batik pigment |
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