CN115418113A - Aloe peel extract and preparation method and application thereof - Google Patents
Aloe peel extract and preparation method and application thereof Download PDFInfo
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- CN115418113A CN115418113A CN202211010409.2A CN202211010409A CN115418113A CN 115418113 A CN115418113 A CN 115418113A CN 202211010409 A CN202211010409 A CN 202211010409A CN 115418113 A CN115418113 A CN 115418113A
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- Prior art keywords
- aloe
- peel
- extract
- aloe peel
- ultraviolet
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/34—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using natural dyestuffs
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/36—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using mordant dyes ; using metallisable dyes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Coloring (AREA)
- Cosmetics (AREA)
Abstract
The invention provides an aloe peel extract and a preparation method and application thereof, belonging to the technical field of textile dyes. The aloe peel extract is prepared by taking aloe peel as a raw material and carrying out crushing, enzymolysis extraction, solvent extraction and reduced pressure distillation and concentration on the aloe peel; wherein the Aloe peel extract comprises Aloesin, 7-O-Methyloeresin A, aloe-emodin, aloin A, and Aloin B, and 1g of dried Aloe peel extract comprises 730.702 + -28.871 mg total phenolic compounds with gallic acid equivalent and 683.240 + -13.199 mg total flavonoids with catechin equivalent; further can be applied to dyeing procedures and obtain fabrics with bright colors and ultrahigh ultraviolet-proof effect. The invention develops the waste aloe peel into a natural dye, improves the economic value of aloe, obtains a green, natural and nontoxic dye, and simultaneously obtains the fabric which has bright color and ultrahigh ultraviolet-proof effect.
Description
Technical Field
The invention relates to an aloe peel extract, a preparation method and application thereof, in particular to a method for mordanting fabrics by taking aloe peel as a raw material and preparing the aloe peel extract as an ultraviolet-proof dye, and belongs to the technical field of textile dyes.
Background
The plant dye has been traced to Xuanyuan' Xuanyuan yellow fir for a long time. Since summer, people began to dye fabrics with blue grass as a natural dye; in the following commercial period, the plant dyeing technology mainly using plant dyes and ore dyes is fully developed and matured in spring, autumn and warring countries; in the Qinhan period, scale management appears, and the dyeing technology and the color spectrum are further improved; the process of planting, preparing and dyeing the dyeing raw materials reaches a peak from hour to generation, and the number of the related dyes is hundreds of dyes. In 1856, the first aniline dye, "aniline violet", was discovered by british chemists w.h.perkin, so that the research, production and use of synthetic dyes began to evolve dramatically and gradually replaced natural dyes. However, some synthetic dyes have a detrimental effect on the environment during use and cause allergic, toxic, carcinogenic reactions in people who come into contact with the dyes. Under the call of increasing environmental threat and health concern, environmental-friendly and nonhazardous natural dye is paid attention again to the public as a feasible green product.
Aloe, a perennial evergreen herb of Liliaceae of Liliales, is an important raw material in the pharmaceutical, food and skin care product industries, and has the chemical components with the effects of moisturizing, resisting bacteria, diminishing inflammation, preventing sunburn and the like. Currently, in the production process of aloe products, a large amount of waste aloe peels are generated, which are generally used as fertilizers, feeds, fermentation substrates of biogas and the like, and the aloe peels are rich in natural polyphenols and flavonoids (such as chromone, anthraquinone and anthrone) capable of effectively absorbing ultraviolet rays, wherein the natural polyphenols and flavonoids have a large amount of conjugated systems, which can absorb ultraviolet rays and convert ultraviolet radiation heat into heat energy, and thus resources are wasted. Therefore, an application way is needed to be found to improve the utilization rate of the aloe peel, exert the economic value of the aloe to the maximum extent and realize sustainable development.
The energy of ultraviolet radiation is significantly higher than that of visible radiation, which may cause various chemical reactions in the human body and harm human health. Although it is considered as a healthy behavior, excessive exposure to uv radiation may induce different cellular reactions, manifested as pigmentation, sunburn, skin aging, cancer and DNA damage, for this reason, people mainly prevent uv radiation by applying sunscreens such as sunblocks, wearing sun screens and sun umbrellas, but the sunblocks are not durable in use, expensive and may cause some damage to the skin; many sun-blocking clothes in the market are finished by adopting a synthetic organic ultraviolet absorbent, namely, the problems of poor washing durability, environmental pollution caused by the production process and the like exist; the sunshade umbrella causes inconvenience to the walking and the like. In the case of textiles, prolonged exposure to uv light can lead to chemical and physical changes such as breaking of various chemical bonds in the fabric, discoloration and degradation of the textile fibers, and increased crystallinity.
The prior art CN109295730a discloses an ultraviolet blocking agent and an ultraviolet resistant treatment process of a nylon skin coat fabric using the ultraviolet blocking agent, wherein the following are specifically disclosed: the ultraviolet blocking agent consists of the following substances in parts by weight: 68-75 parts of modified polyurethane, 5-9 parts of an antibacterial agent, 4-7 parts of 2-hydroxy-4-methoxybenzophenone, 2-4.5 parts of nano zinc oxide powder, 2-4 parts of nano titanium dioxide powder, 5-8 parts of solvent oil, 3-6 parts of TDI trimer curing agent and 2-6 parts of polyethylene glycol, wherein the antibacterial agent comprises 5-15 parts of aloe juice, so that the technical problems that the UPF of the skin garment fabric can reach more than 50+ and the skin garment fabric has a good sun-proof effect but does not contain the antibacterial agent and has poor antibacterial performance in the prior art are solved. CN106223043A discloses a dyeing process for cotton-aloe fiber blended yarn, wherein the related raw materials are aloe fiber and cotton, and the fresh leaves of aloe contain a plurality of active ingredients such as anthraquinone, saccharides, amino acids, vitamins and the like, so that the aloe fiber blended yarn has the effects of improving human immunity, resisting aging and treating rheumatic and rheumatoid arthritis, and has good skin care effect.
CN107760055a discloses a "method for purifying aloe natural dye", which adopts 95% ethanol extraction and ultrasonic wave assisted dye extraction, and ensures that the dyed fabric has a drug health care effect, but mainly realizes the drug health care effect in aloe extract, such as: the method has the advantages of resisting aging (glycoprotein), promoting healing, strengthening heart and activating blood (calcium isocitrate), improving immunity and regeneration (aloin A, wound hormone and polypeptide mannan), beautifying value (polysaccharide and multiple vitamins) and the like, and the related purification method is suitable for ensuring better medicine health-care effect, has high cost and is not suitable for industrial mass production.
The research on the in-vitro ionizing radiation resistance of the persimmon tannin aloe composite material is disclosed in Ning Jinliang, 2019: the ionization radiation resistant material prepared by compounding aloe freeze-dried powder with persimmon tannin has the ionization radiation resistant performance on normal cells (human liver cells (L02), human immortalized epidermal cells (HaCat)) and tumor cells (human liver cancer cells (HepG 2)). Wherein, the aloe freeze-dried powder is provided by Guangdong original green bioengineering limited company, and the content of the effective components in the aloe freeze-dried powder can be quantitatively measured by using O-acetyl as a correction standard.
Therefore, there is a need for a low-cost, green, natural, non-toxic ultraviolet finishing agent for textiles, which has good washing durability after finishing on textiles.
Disclosure of Invention
The invention provides an aloe peel extract and a preparation method and application thereof, aiming at the problems of waste of aloe peel, the defects of the existing ultraviolet-proof dye/ultraviolet blocking agent and the fact that the aloe peel is rich in natural polyphenol and flavonoid substances capable of effectively absorbing ultraviolet rays. In the technical scheme, the (waste) aloe peel is used as a raw material, a specific preparation method and adaptive control conditions are adopted to prepare the ultraviolet-proof dye, and the ultraviolet-proof dye is applied to textiles, so that the textiles are endowed with an ultraviolet-proof function, the industrial and resource utilization of the aloe peel is finally realized, and the dye and the textiles which are low in cost, green, natural, non-toxic and have the ultraviolet-proof function are provided.
In order to achieve the technical purpose, the following technical scheme is proposed:
the technical scheme provides that: an Aloe peel extract is prepared by taking Aloe peel as a raw material and performing crushing, enzymolysis extraction, solvent extraction and reduced pressure distillation and concentration, wherein the Aloe peel extract comprises Aloesin, 7-O-Methyloeresin A, aloe-emodin, aloin A and Aloin B, and the Aloe peel extract respectively relates to the following structural formulas:
the dry state aloe peel extract comprises 730.702 + -28.871 mg total phenols with gallic acid equivalent and 683.240 + -13.199 mg total flavonoids with catechin equivalent per 1g dry state aloe peel extract.
The technical scheme provides that: a method for preparing aloe peel extract comprises the following steps:
1) Crushing: cleaning aloe peel, drying at 40 deg.C, pulverizing, and sieving with 40 mesh sieve to obtain aloe peel powder;
2) Enzymolysis extraction: adding cellulase and deionized water into the obtained aloe peel powder, wherein the cellulase is 15-55g per kg of aloe peel powder, and the deionized water is 8-25L per kg of aloe peel powder, mixing uniformly, heating to 65 deg.C at a speed of 1 deg.C/min to obtain aloe peel primary extract with pH of 4.5-6.5;
3) Solvent extraction: adding solvent medium into the primary aloe peel extractive solution, controlling pH, heating at 25-65 deg.C for 20-100min, and vacuum filtering to obtain final aloe peel extractive solution;
4) Concentration: distilling the obtained final extractive solution of Aloe bark under reduced pressure, and lyophilizing at-60 deg.C under 1.33Pa for 48 hr to obtain Aloe bark extract.
Preferably, in the step 1), the aloe peel is waste aloe peel without mesophyll, and the waste aloe peel is formed after preparing aloe gel by using fresh aloe as a raw material, so that the resource recycling of the waste aloe peel is realized, and the problem of raw material waste is reduced.
Preferably, in the step 3), when the pH is controlled to be 4-7, the solvent medium is glacial acetic acid, and then the yellow-green ultraviolet-proof dye can be obtained; when the pH is controlled to be 7-8, the solvent medium is one or the mixture of sodium carbonate and sodium bicarbonate, and then the reddish brown ultraviolet-proof dye can be obtained.
The technical scheme provides that: the obtained aloe peel extract is used for ultraviolet-proof dye, namely the ultraviolet-proof dye is used for mordant dyeing of fabrics, wherein the fabrics comprise natural fibers, regenerated fibers and synthetic fibers, the mordant dyeing method comprises pre-mordant dyeing, one-bath mordant dyeing and post-mordant dyeing, and the mordant comprises one or the mixture of any two of copper ions, ferrous ions, aluminum ions and tannin.
In the technical scheme, the involved enzymolysis extraction mechanism comprises the following steps:
the active ingredients in the aloe bark are mostly present in the cytoplasm of plant cells. During extraction, the solvent needs to overcome the mass transfer resistance from the cell wall and the intercellular substance. The cell wall is a compact structure formed by cellulose, hemicellulose, pectin and other substances, and proper enzymes (such as cellulase, hemicellulase and pectinase) are selected for pretreating the Chinese medicinal materials, so that the cellulose, the hemicellulose and the pectin forming the cell wall can be decomposed, the structure of the cell wall is damaged, local collapse, dissolution and loosening are generated, the resistance from the cell wall and intercellular substance during solvent extraction is reduced, the cell dissolution rate of effective components is accelerated, the extraction efficiency is improved, and the extraction time is shortened;
the involved solvent extraction mechanism: the flavonoids in the aloe peel have poor water solubility, but are easily dissolved in hot alkaline water, so that the acidic components are extracted in the form of salt. The extracted substances are basically the same under different pH conditions, but the concentrations are different, so that different hues can be shown after dyeing, the conditions such as pH and the like can be adjusted according to actual production needs, and the higher the extraction concentration is, the better the extraction concentration is;
furthermore, preservation of the aloe peel extract involved: the dye is extracted to be liquid, which is not convenient for storage and transportation, so that the dye is preserved in a solid form by vacuum distillation, freeze drying or vacuum drying
By adopting the technical scheme, the beneficial technical effects brought are as follows:
1. the natural ultraviolet-proof dye provided by the invention is obtained by taking aloe peel (particularly, the aloe peel discarded after mesophyll is removed in the aloe product processing process) as a raw material and performing crushing, enzymolysis extraction, solvent extraction and reduced pressure distillation concentration, and can be used for dyeing fibers such as natural fibers, regenerated fibers, synthetic fibers and the like, so that an effective way for increasing the economic value of industrial wastes is provided, and the environmental pollution is reduced;
2. in the invention, the Aloe peel extract is obtained by taking Aloe peel as a raw material and performing crushing, enzymolysis extraction, solvent extraction and reduced pressure distillation and concentration, wherein the Aloe peel extract comprises Aloesin, 7-O-Methyloeresin A, aloe-emodin, aloin A and Aloin B; and, every 1 gram of the dried aloe peel extract comprises 730.702 +/-28.871 mg total phenolic substances with gallic acid equivalent and 683.240 +/-13.199 mg total flavonoid compounds with catechin equivalent, namely, the dried aloe peel extract contains a large amount of active ingredients, so that the functional application of the aloe peel extract can be further developed, such as: an anti-ultraviolet dye;
3. in the extraction process of the aloe peel, the step 1) limits drying at 40 ℃, which ensures the stability of effective components and contents thereof in the aloe peel and the effectiveness of the extraction process, such as: the temperature is too high, which causes part of the components in the aloe peel extract to be lost at high temperature (for example, free anthraquinone is heated under normal pressure and is easy to sublimate); if the temperature is too low, the drying is slow, the overall efficiency of the preparation process is influenced, and the aloe peel is easy to mildew in a low-temperature and humid environment, so that the product quality of the aloe peel extract and the stability of the extraction process are influenced. Wherein, the aloe peel powder is controlled to pass through a 40-mesh sieve, and further, the particle size of the aloe peel powder involved in the subsequent extraction process is controlled, so that the specific surface area between the aloe peel powder and the cellulase is large, the extraction efficiency is further improved, the target components in the aloe extract are separated to the maximum extent, and the aloe peel extract is ensured on the premise of being applied to the subsequent application (ultraviolet-proof dye) of the aloe peel extract;
in the step 2), cellulase is added, so that the extraction efficiency can be effectively improved, and meanwhile, the effective components in the target product dye can be directionally reserved. Wherein, the further restriction is that the cellulase and the deionized water are added into the obtained aloe peel powder according to the usage of 15-55g cellulase per kilogram of aloe peel powder and 8-25L deionized water per kilogram of aloe peel powder, so as to effectively ensure that the primary aloe peel extract obtained under the condition can obtain the maximum value by measuring the absorbance by an ultraviolet spectrophotometer when used for an ultraviolet-proof dye after the subsequent treatment;
wherein, the substance extracted within the range of the dosage of the deionized water can obtain the maximum value when an ultraviolet spectrophotometer is used for measuring the absorbance. If the dosage of the deionized water is too small, the viscosity of an extraction system is too high, and the release of effective components is hindered; on the contrary, if the usage amount of the deionized water is too small, the effective components can be diluted, and the waste of water resources is caused;
in addition, the temperature is further limited to be increased to 65 ℃ at the rate of 1 ℃/min, so that the extraction efficiency and the quality are ensured, and if the temperature increase rate is too high, the temperature is rapidly increased, so that the cellulase is inactivated without fully exerting the effect, and the release of effective components is not facilitated; on the contrary, the heating rate is too slow, so that the cellulase can fully play a role, but the extraction period is prolonged, and further, the energy waste and the like are caused;
in the step 3), extraction solvent media with different pH values are used, the color tone of the dye in subsequent dyeing can be adjusted, a precondition guarantee is provided for the application of the aloe peel extract, and the applicability of the aloe peel extract is further improved, wherein the constant temperature heating is further limited to be 20-100min at 25-65 ℃, namely, the re-extraction of the effective components in the aloe peel is guaranteed, a precondition guarantee is provided for the next step of concentration, and if the temperature is too low, the effective components are difficult to extract; if the temperature is too high, the active ingredients are deteriorated, degraded and the like, and the types and the contents of the active ingredients in the aloe peel extract cannot be ensured.
In the step 4), "freeze-drying for 48h under the conditions of pressure of 1.33Pa and temperature of-60 ℃ is limited, so that the concentration quality and efficiency of the aloe peel final extract are ensured, and the types and the stock of active ingredients in the aloe peel extract are ensured;
4. the aloe peel extract is used in the ultraviolet-proof dye, and different mordant methods and mordants are used, so that the dyeing depth and color tone can be adjusted, the practicability of the dye is further ensured, and the application range of the dye is improved;
5. the invention not only provides a technology for efficiently utilizing industrial waste aloe skin, but also develops a low-cost, green, natural and nontoxic dye and textile with an ultraviolet-proof function, wherein the related aloe skin extract (ultraviolet-proof dye) is a green, environment-friendly and nontoxic reagent from the raw material to the processing process, and the used reagent to the final finished product, and can improve the utilization rate of the waste aloe skin, and the related cost, energy consumption and product stability are low.
Drawings
FIG. 1 is a composition analysis of aloe vera bark extract using UV spectroscopy as in example 4;
FIG. 2 is a composition analysis of aloe vera skin extract using infrared spectroscopy in example 4;
FIG. 3 shows the dyeing effect of silk dyed with UV-resistant dye after pre-mordant of example 5, which is no mordant, aluminum ion, copper ion and ferrous ion;
FIG. 4 shows the dyeing effect (different dyeing temperatures) of the silk mordants in one bath with the anti-UV dye and no mordant, aluminum ions, copper ions, ferrous ions, and tannin in example 6;
FIG. 5 shows the dyeing effect (different dyeing time) of the silk mordants in one bath with the anti-UV dye and no mordant, aluminum ion, copper ion, ferrous ion, and tannin in example 6;
FIG. 6 shows the dyeing effect (different bath pH) of the silk mordants in the same bath with the anti-UV dye in example 6, wherein no mordant, aluminum ion, copper ion, ferrous ion and tannin are used as the mordants.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The Aloe peel extract is obtained by taking Aloe peel as a raw material and performing crushing, enzymolysis extraction, solvent extraction and reduced pressure distillation and concentration, wherein the Aloe peel extract comprises Aloesin, 7-O-Methylaloeresin a, aloe-emodin, aloin a and Aloin B, and the Aloe peel extract respectively relates to the following structural formulas:
the dry state aloe peel extract comprises 730.702 + -28.871 mg gallic acid equivalent and 683.240 + -13.199 mg catechin equivalent of total phenols and flavonoids compounds based on 1g of dry state aloe peel extract.
Example 2
The preparation method of the aloe peel extract comprises the following steps:
1) Crushing: cleaning aloe peel, drying at 40 deg.C, pulverizing, and sieving with 40 mesh sieve to obtain aloe peel powder;
2) Enzymolysis extraction: adding cellulase and deionized water into the obtained aloe peel powder, wherein the cellulase is 15-55g per kg of aloe peel powder, and the deionized water is 8-25L per kg of aloe peel powder, mixing uniformly, heating to 65 deg.C at a speed of 1 deg.C/min to obtain aloe peel primary extract with pH of 4.5-6.5;
3) Solvent extraction: adding solvent medium into the primary extractive solution, controlling pH, heating at 25-65 deg.C for 20-100min, and vacuum filtering to obtain final extractive solution;
4) Concentration: distilling the obtained final extractive solution of Aloe skin under reduced pressure, and lyophilizing at-60 deg.C under 1.33Pa for 48 hr to obtain Aloe skin extract.
In the step 1), the aloe bark is the waste aloe bark without mesophyll, and the waste aloe bark is generally formed by taking fresh aloe as a raw material and preparing aloe gel, so that the resource recycling of the waste aloe bark is realized, and the problem of raw material waste is reduced.
In the step 3), when the pH is controlled to be 4-7, the solvent medium is glacial acetic acid, and then the yellow-green ultraviolet-proof dye can be obtained; when the pH is controlled to be 7-8, the solvent medium is one or the mixture of sodium carbonate and sodium bicarbonate, and then the red-brown ultraviolet-proof dye can be obtained.
Example 3
Based on examples 1-2, this example provides that the obtained aloe peel extract is used as an ultraviolet-proof dye, namely, the ultraviolet-proof dye is used for mordant dyeing of fabrics, wherein the fabrics comprise natural fibers, regenerated fibers and synthetic fibers, the mordant dyeing method comprises pre-mordant dyeing, co-mordant dyeing and post-mordant dyeing, and the mordant comprises one or a mixture of any two or more of copper ions, ferrous ions, aluminum ions and tannin.
Example 4
Based on examples 1-3, this example further analyzes the components of the aloe vera bark extract to further illustrate the present technique.
1. Ultraviolet spectrum is adopted to carry out component analysis on aloe peel extract
As a result, as shown in FIG. 1, five absorption bands appear in the spectrum at wavelengths of 200-400nm, and it is concluded that the aloe dye may have a long-chain conjugated chromophore or a polycyclic aromatic hydrocarbon chromophore, and at least 4-5 conjugated chromophores and auxochromes are contained in the molecule. Among them, the absorption peaks at 210nm and 252nm indicate the presence of aromatic rings in the aloe dye. The weak absorption band around 294nm indicates that the aloe dye contains a ketone or aldehyde. The absorption peak at 268nm is due to the p-quinone structure, while the absorption peak at 340nm is due to the benzoyl structure.
2. Analyzing the components of the aloe peel extract by infrared spectroscopy
The results are shown in FIG. 2, 3402 cm -1 The nearby broadband band represents the tensile vibration of the phenolic hydroxyl group, 2930 cm -1 The low intensity peak at (A) represents the aromatic-CH stretching vibration, 1592 cm -1 The high intensity peak at (1) corresponds to the double-bonded conjugated ketone group of polyphenol/flavone, 1415 cm -1 The strong peak in (B) belongs to-C-O stretching vibration, corresponding to double-bond conjugated ketone group in polyphenol/flavone, in 1259 cm -1 And 621 cm -1 The peaks of (a) represent the in-plane and out-of-plane-C-O bending vibrations of polyphenols and flavonoids.
3. Analysis of the content of total phenols and total flavonoids in the aloe peel extract
The total phenols and the total flavonoids are important secondary metabolites synthesized by plants, and can protect the plants from ultraviolet radiation, wherein the total phenol content in the aloe dye is calculated by a gallic acid calibration curve: y =5.3294x +0.00838 2 =0.9978 (0.02-0.3 mg/mL), total flavone content calculated from catechin calibration curve: y =0.4418x +0.00478 2 =0.9962（0.02-0.3 mg/mL）；
The results showed that 1g of the total phenols and flavonoids in the dried aloe vera skin extract contained 730.702 ± 28.871mg (gallic acid equivalents) and 683.240 ± 13.199mg (catechin equivalents), respectively.
In conclusion, the substance components and the content of the aloe peel extract can be deduced through ultraviolet spectrum analysis, fourier transform spectrum analysis and total polyphenol and flavone content analysis.
Example 5
This example provides a method for preparing an aloe vera skin extract, comprising the steps of:
1) Crushing: cleaning waste aloe peel, drying at 40 deg.C in a drying oven, pulverizing with a universal pulverizer, and sieving with 40 mesh sieve to obtain aloe peel powder;
2) Enzymolysis extraction: adding 35g cellulase (activity is more than or equal to 35U/mg) per kg of aloe peel powder and 25L deionized water per kg of aloe peel powder, mixing, heating to 65 deg.C at a rate of 1 deg.C/min, and obtaining aloe peel primary extract with pH of 5.5;
3) Solvent extraction: deep extracting with alkaline solvent medium, i.e. adding sodium carbonate powder into the primary aloe peel extractive solution, controlling pH to 8, heating at 65 deg.C for 1 hr, and vacuum filtering to obtain final aloe peel extractive solution;
4) Concentration: distilling the obtained final extractive solution of Aloe skin under reduced pressure, and freeze drying for 48 hr to obtain Aloe skin extract, i.e. ultraviolet-proof dye.
The technical scheme is further explained based on the aloe peel extract obtained above for dyeing silk.
1. Dyeing process
Wherein, after pre-mordant dyeing is carried out by taking a mordant-free agent, aluminum ions, copper ions and ferrous ions as mordants, the obtained aloe skin extract is used for dyeing silk, and the specific steps are as follows:
x1: pre-mordanting, wherein the mass of a mordant accounts for 8 percent of the weight of the silk fabric, and the bath ratio is 1:50, primary dyeing at 40 ℃, heating to 90 ℃ at a speed of 1 ℃/min, and keeping the temperature for 45 min;
x2: dyeing, cooling the mordant bath to room temperature, taking out the silk, putting the silk into the dye bath, primarily dyeing the silk at 40 ℃, heating the silk to 90 ℃ at the speed of 1 ℃/min, and keeping the temperature for 60 min;
x3: cooling the dye bath to room temperature, fully washing with water, and drying in the air to obtain the dye bath.
2. Evaluation of dyeing Effect
Wherein the criteria by which the data is received include,
washing fastness: and (3) detecting the soaping color fastness according to a method specified in GB/T3921-2008 textile color fastness test soaping color fastness.
Rubbing fastness: and detecting the color fastness to rubbing according to a method specified in GB/T3920-2008 color fastness test for textiles color fastness to rubbing.
3. Evaluation of ultraviolet protection Effect
According to AATCC 61-2013 color fastness to washing: the accelerated method washes the dyed fabric for 5, 10, 15, 20 and 25 times, and then adopts a textile anti-ultraviolet performance tester to test the anti-ultraviolet performance of the textile.
The color fastness and the ultraviolet ray protection effect of silk dyed using the aloe skin extract obtained above were measured according to the above criteria, and the results are shown in the following tables 1 to 2 and fig. 3.
Example 6
This example provides a method for preparing an aloe skin extract, including the following steps:
1) Crushing: cleaning waste aloe peel, drying at 40 deg.C in a drying oven, pulverizing with a universal pulverizer, and sieving with 40 mesh sieve to obtain aloe peel powder;
2) Enzymolysis extraction: adding cellulase and deionized water into the obtained aloe peel powder according to 15g cellulase (activity is more than or equal to 35U/mg) used per kg aloe peel powder and 15L deionized water used per kg aloe peel powder, mixing uniformly, heating to 65 ℃ at a speed of 1 ℃/min, and obtaining an aloe peel primary extract with pH of 5.5;
3) Solvent extraction: extracting with acidic solvent medium, i.e. adding glacial acetic acid into the primary aloe peel extractive solution, controlling pH to 5, heating at 65 deg.C for 1 hr, and vacuum filtering to obtain final aloe peel extractive solution;
4) Concentration: distilling the obtained final extractive solution under reduced pressure, and freeze drying for 48 hr to obtain Aloe skin extract.
The technical scheme is further explained based on the application of the aloe peel extract (namely, the ultraviolet-proof dye) obtained above in the dyeing of silk.
1. Dyeing process
After pre-mordanting by taking a mordant-free agent, aluminum ions, copper ions and ferrous ions as mordants, carrying out one-bath mordanting on silk by using the obtained ultraviolet-proof dye, wherein the method comprises the following steps of:
y1: preparing a dye bath, adding a corresponding mordant into the obtained aloe peel extract, wherein the mass of the mordant accounts for 8% of the weight of the silk fabric, adjusting the pH of the dye bath to 3-7, and the bath ratio is 1:50;
y2: dyeing, namely primarily dyeing the silk at 40 ℃, heating to 50-90 ℃ at a speed of 1 ℃/min, and preserving heat for 30-90 min;
y3: cooling the dye bath to room temperature, fully washing with water, and drying in the air to obtain the dye bath.
2. Evaluation of dyeing Effect
The color depth (K/S) of the dyed fabric was measured using a color measuring and matching instrument, and the results are shown in tables 3 to 5 below and FIGS. 4 to 6.
3. Evaluation of ultraviolet protection Effect
The ultraviolet resistance of the textiles was measured using a textile ultraviolet resistance tester, and the results are shown in table 6 below.
Example 7
In this example, the extraction conditions involved in the preparation process of the ultraviolet-proof dye are considered to further explain the technical scheme.
Selecting four factors of cellulase addition, enzymolysis liquid pH, enzymolysis temperature and enzymolysis time, respectively investigating the influence of the four factors on the extraction efficiency of the ultraviolet-proof dye, and representing the extraction efficiency by using the absorbance at the maximum absorption wavelength of an ultraviolet spectrum. The results obtained are shown in table 7 below.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. An Aloe peel extract is characterized in that Aloe peel is taken as a raw material and is obtained by crushing, enzymolysis extraction, solvent extraction and reduced pressure distillation and concentration, wherein the Aloe peel extract comprises Aloesin, 7-O-Methyloeresin A, aloe-emodin, aloin A and Aloin B;
the dry state aloe peel extract comprises 730.702 + -28.871 mg total phenols with gallic acid equivalent and 683.240 + -13.199 mg total flavonoids with catechin equivalent per 1g dry state aloe peel extract.
2. A preparation method of an aloe peel extract is characterized by comprising the following steps:
1) Crushing: cleaning aloe peel, drying at 40 deg.C, pulverizing, and sieving to obtain aloe peel powder;
2) Enzymolysis extraction: adding cellulase and deionized water into the obtained aloe peel powder, wherein the cellulase is 15-55g per kg of aloe peel powder, and the deionized water is 8-25L per kg of aloe peel powder, mixing uniformly, heating to 65 deg.C at a speed of 1 deg.C/min to obtain aloe peel primary extract with pH of 4.5-6.5;
3) Solvent extraction: adding solvent medium for controlling pH value into the primary aloe peel extractive solution, heating at constant temperature, and vacuum filtering to obtain final aloe peel extractive solution;
4) Concentration: distilling the obtained final extractive solution of Aloe skin under reduced pressure, and freeze drying to obtain Aloe skin extract.
3. The method for preparing an aloe vera skin extract according to claim 2, wherein the aloe vera skin is waste aloe vera skin after mesophyll removal in step 1).
4. The method for preparing the aloe vera skin extract according to claim 2, wherein the aloe vera skin powder is sieved through a 40 mesh sieve in step 1).
5. The method for preparing an aloe vera skin extract according to claim 2, wherein in the constant-temperature heating of the step 3), controlling: heating at 25-65 deg.C for 20-100min.
6. The method for preparing an aloe vera skin extract according to claim 2, wherein, in the step 3), the solvent medium is glacial acetic acid while controlling the pH to 4 to 7; when the pH is controlled to be 7-8, the solvent medium is one or the mixture of two of sodium carbonate and sodium bicarbonate.
7. The method for preparing an aloe vera skin extract according to claim 2, wherein in the freeze-drying of the step 4), controlling: freeze-drying at-60 deg.C under 1.33Pa for 48h.
8. Use of an aloe bark extract as defined in any one of claims 1 to 7 in uv protection dyes.
9. The aloe vera skin extract as claimed in claim 8, wherein the ultraviolet protection dye is used for mordanting fabrics, wherein the fabrics comprise natural fibers, regenerated fibers and synthetic fibers, and the mordanting method comprises pre-mordanting, co-mordanting and post-mordanting, wherein the mordanting agent comprises one or a mixture of any two or more of copper ions, ferrous ions, aluminum ions and tannin.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101258922A (en) * | 2008-04-23 | 2008-09-10 | 云南元江万绿生物（集团）有限公司 | Comprehensive utilization aloe skin processing method |
| CN111494285A (en) * | 2020-06-04 | 2020-08-07 | 珠海萱嘉君行健康产业发展有限公司 | Method for extracting antibacterial substance based on aloe peel or aloe wastewater and application of antibacterial substance |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101258922A (en) * | 2008-04-23 | 2008-09-10 | 云南元江万绿生物（集团）有限公司 | Comprehensive utilization aloe skin processing method |
| CN111494285A (en) * | 2020-06-04 | 2020-08-07 | 珠海萱嘉君行健康产业发展有限公司 | Method for extracting antibacterial substance based on aloe peel or aloe wastewater and application of antibacterial substance |
Non-Patent Citations (6)
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| 曹颖;: "芦荟皮中蒽醌类抗菌剂的提取工艺研究", 印染助剂, no. 05, 20 May 2017 (2017-05-20), pages 1152 * |
| 曹颖;: "芦荟皮中蒽醌类抗菌剂的提取工艺研究", 印染助剂, no. 05, pages 1152 * |
| 李琪;刘超;张阳阳;: "酶法提取芦荟中蒽醌类抗菌物质的研究", 农产品加工(学刊), no. 19, 20 October 2013 (2013-10-20), pages 2 * |
| 李琪;刘超;张阳阳;: "酶法提取芦荟中蒽醌类抗菌物质的研究", 农产品加工(学刊), no. 19, pages 2 * |
| 韩艳梅;林红;陈宇岳;: "芦荟蒽醌类化合物用于真丝绸抗紫外处理", 丝绸, no. 02 * |
| 韩艳梅;林红;陈宇岳;: "芦荟蒽醌类化合物用于真丝绸抗紫外处理", 丝绸, no. 02, 20 February 2009 (2009-02-20) * |
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