CN115418113B - Aloe bark extract and preparation method and application thereof - Google Patents
Aloe bark extract and preparation method and application thereof Download PDFInfo
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- CN115418113B CN115418113B CN202211010409.2A CN202211010409A CN115418113B CN 115418113 B CN115418113 B CN 115418113B CN 202211010409 A CN202211010409 A CN 202211010409A CN 115418113 B CN115418113 B CN 115418113B
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- aloe
- extract
- ultraviolet
- skin
- dye
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- 239000000284 extract Substances 0.000 title claims abstract description 83
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
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- 238000000034 method Methods 0.000 claims abstract description 26
- 239000004744 fabric Substances 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 21
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229930003935 flavonoid Natural products 0.000 claims abstract description 12
- 235000017173 flavonoids Nutrition 0.000 claims abstract description 12
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- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 claims abstract description 7
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000005487 catechin Nutrition 0.000 claims abstract description 7
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- 235000002961 Aloe barbadensis Nutrition 0.000 claims abstract description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 5
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- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
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- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims 2
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- AFHJQYHRLPMKHU-WEZNYRQKSA-N aloin B Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1[C@H]1C2=CC(CO)=CC(O)=C2C(=O)C2=C(O)C=CC=C21 AFHJQYHRLPMKHU-WEZNYRQKSA-N 0.000 abstract description 9
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- AFHJQYHRLPMKHU-UHFFFAOYSA-N isobarbaloin Natural products OC1C(O)C(O)C(CO)OC1C1C2=CC(CO)=CC(O)=C2C(=O)C2=C(O)C=CC=C21 AFHJQYHRLPMKHU-UHFFFAOYSA-N 0.000 abstract description 9
- YDQWDHRMZQUTBA-UHFFFAOYSA-N Aloe emodin Chemical compound C1=CC=C2C(=O)C3=CC(CO)=CC(O)=C3C(=O)C2=C1O YDQWDHRMZQUTBA-UHFFFAOYSA-N 0.000 abstract description 8
- AFHJQYHRLPMKHU-XXWVOBANSA-N Aloin Natural products O=C1c2c(O)cc(CO)cc2[C@H]([C@H]2[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O2)c2c1c(O)ccc2 AFHJQYHRLPMKHU-XXWVOBANSA-N 0.000 abstract description 5
- 229930182559 Natural dye Natural products 0.000 abstract description 5
- CPUHNROBVJNNPW-UHFFFAOYSA-N aloin A Natural products OC1C(O)C(O)C(CO)OC1OC1C2=CC(CO)=CC(O)=C2C(=O)C2=C(O)C=CC=C21 CPUHNROBVJNNPW-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000978 natural dye Substances 0.000 abstract description 5
- WRLXHKDQSQMWSH-UHFFFAOYSA-N 7-O-methylaloeresin A Natural products COC1=CC(C)=C(C(C=C(CC(C)=O)O2)=O)C2=C1C1OC(CO)C(O)C(O)C1OC(=O)C=CC1=CC=C(O)C=C1 WRLXHKDQSQMWSH-UHFFFAOYSA-N 0.000 abstract description 4
- HKIKAXXIWJHWLY-QEVGBQTESA-N Aloesin Natural products O=C(CC=1Oc2c([C@H]3[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O3)c(O)cc(C)c2C(=O)C=1)C HKIKAXXIWJHWLY-QEVGBQTESA-N 0.000 abstract description 4
- HKIKAXXIWJHWLY-ZIIYPAMZSA-N Aloesin Chemical compound C=12OC(CC(=O)C)=CC(=O)C2=C(C)C=C(O)C=1[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O HKIKAXXIWJHWLY-ZIIYPAMZSA-N 0.000 abstract description 4
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- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 238000010298 pulverizing process Methods 0.000 abstract description 2
- 239000003086 colorant Substances 0.000 abstract 1
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- 150000008442 polyphenolic compounds Chemical class 0.000 description 7
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- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 5
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- WQZGKKKJIJFFOK-QTVWNMPRSA-N D-mannopyranose Chemical compound OC[C@H]1OC(O)[C@@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-QTVWNMPRSA-N 0.000 description 1
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- YWORCEHQVMOKDM-UHFFFAOYSA-H tricalcium;1-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]C(=O)C(O)C(C([O-])=O)CC([O-])=O.[O-]C(=O)C(O)C(C([O-])=O)CC([O-])=O YWORCEHQVMOKDM-UHFFFAOYSA-H 0.000 description 1
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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 bark extract and a preparation method and application thereof, belonging to the technical field of textile dyes. The aloe peel extract is prepared from aloe peel by pulverizing, performing enzymolysis extraction, extracting with solvent, and concentrating under reduced pressure; wherein the Aloe vera skin extract comprises Aloesin, 7-O-Methylaloeresin A, aloe-emodin, aloin A, and Aloin B, and 1 gram of dry Aloe vera skin extract comprises 730.702 + -28.871 mg gallic acid equivalent total phenolic and 683.240 + -13.199 mg catechin equivalent total flavonoids; further can be applied to dyeing procedures and can obtain fabrics with vivid colors and ultra-high anti-ultraviolet effect. The invention develops the waste aloe skin into a natural dye, improves the economic value of aloe, obtains a green, natural and nontoxic dye, and simultaneously obtains the fabric with vivid color and ultra-high anti-ultraviolet effect.
Description
Technical Field
The invention relates to an aloe skin extract and a preparation method and application thereof, in particular to a method for preparing an aloe skin extract by taking aloe skin as a raw material and then mordanting fabrics by taking the aloe skin extract as an ultraviolet-proof dye, belonging to the technical field of textile dyes.
Background
Plant dyes have long been available and can be traced to Xuanyuan's world at the earliest. Starting from summer, people began to dye fabrics with blue grass as the natural dye; the plant dyeing technology mainly comprising vegetable dye and ore dye is fully developed in the following period of business weeks and matures in the period of spring and autumn war; by the time of Qin-Han period, scale management appears, and dyeing technology and chromatography are further improved; the number of the related dyes reaches the peak from the time of early generation to the time of early generation, and the number of the related dyes is hundreds. In 1856, the uk chemist w.h.perkin found the first aniline dye "aniline violet", so that research, production and use of synthetic dyes began to develop rapidly and gradually replaced natural dyes. However, some synthetic dyes have a detrimental effect on the environment during use and cause allergic, toxic, carcinogenic reactions to persons in contact therewith. With an increasing environmental threat and health concern, environmentally friendly, nonhazardous natural dyes are receiving renewed public attention as a viable green product.
Aloe, perennial evergreen herb of lily family, is an important raw material in medicine, food and skin care product industry, and its chemical components have the functions of moisturizing, antibiosis, antiphlogosis, sun protection, etc. Currently, in the production process of aloe products, a large amount of waste aloe skin is generated, which is generally used as a fertilizer, a feed, a fermentation substrate of biogas, etc., and aloe skin is 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 capable of absorbing ultraviolet rays and converting ultraviolet radiation heat into heat energy, which causes resource waste. Therefore, an application way is needed to be found to improve the utilization rate of aloe skin, exert the economic value of aloe to the greatest extent and realize sustainable development.
The energy of ultraviolet radiation is obviously higher than that of visible light radiation, and various chemical reactions of human bodies can be possibly initiated, so that the human health is endangered. Although mild sunlight is considered to be a healthy behavior, excessive exposure to ultraviolet radiation may induce various cellular reactions, manifested by pigmentation, sunburn, skin aging, cancer and DNA damage, for which people mainly prevent ultraviolet radiation by applying sun-screening cream, wearing sun-screening clothing, supporting sun-screening umbrella, etc., but sun-screening cream is not durable in use, expensive in price and causes some damage to skin; many sun-proof clothes in the market are finished by adopting a synthetic organic ultraviolet absorbent, namely, the problems of poor washing durability, environmental pollution in the production process and the like exist; the support of the sunshade can give inconvenience to the rows, etc. In the case of textiles, the long-term exposure to ultraviolet rays will lead to chemical and physical changes such as breakage of different chemical bonds in the textile, fading degradation of textile fibers, and increase of crystallinity.
The prior art CN109295730A discloses an ultraviolet blocking agent and an ultraviolet resistant treatment process of nylon skin clothing fabric using the ultraviolet blocking agent, wherein the ultraviolet resistant treatment process specifically comprises the following steps: the ultraviolet blocking agent consists of the following substances in parts by weight: 68-75 parts of modified polyurethane, 5-9 parts of 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, 2-6 parts of polyethylene glycol and 5-15 parts of antibacterial agent including aloe juice, so as to solve the technical problems of ultraviolet resistant glue used in skin clothing fabric in the prior art, and the UPF of the skin clothing fabric can reach more than 50+ and has better sun-proof effect, but the skin clothing fabric does not contain antibacterial agent and has poorer antibacterial performance. The CN106223043A discloses a dyeing process of cotton-aloe fiber blended yarn, wherein the raw materials involved are aloe fiber and cotton, and the aloe fresh leaves are relied on to contain various active ingredients such as anthraquinone, saccharide, amino acid, vitamin and the like, so that the dyeing process has the effects of improving human immunity, resisting aging, treating rheumatic arthritis and rheumatoid arthritis, and simultaneously has good skin care effect, and cotton fiber and aloe fiber are uniformly colored, dyeing temperature and fixation temperature are reduced by preprocessing the blended yarn.
CN107760055A discloses a "purification method of aloe natural dye", which adopts 95% ethanol extraction and ultrasonic wave to assist in extracting dye, and ensures that the dyed fabric has medicine health care effect, but mainly realizes medicine health care effect in aloe extract, such as: anti-aging (glycoprotein), healing promoting, heart strengthening and blood activating (calcium isocitrate), immunity and regeneration (aloin A, wound hormone and polysaccharide peptide mannose), and beauty value (polysaccharide and multivitamin), etc., namely, the related purification method is suitable for ensuring better medicine health care effect, and the related purification method has high cost and is not suitable for industrialized mass production.
In vitro anti-ionizing radiation research of persimmon tannin aloe composite material, ning Jinliang, 2019, discloses: the aloe freeze-dried powder is compounded with persimmon tannin to prepare an ionizing radiation resistant material, and the ionizing radiation resistant material has ionizing 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 Yuan green bioengineering Co., ltd, and the content of the effective components in the aloe freeze-dried powder can be measured by using O-acetyl as a correction standard.
Thus, there is an urgent need for a low cost, green, natural, non-toxic ultraviolet finish for textiles that has good wash durability after finishing on the textiles.
Disclosure of Invention
Aiming at the problems of aloe skin waste and the defects of the existing ultraviolet-proof dye/ultraviolet blocking agent in the prior art, the invention provides an aloe skin extract and a preparation method and application thereof based on the fact that aloe skin is rich in natural polyphenol and flavonoid substances capable of effectively absorbing ultraviolet rays. In the technical scheme, the (waste) aloe skin is used as a raw material, a specific preparation method and the corresponding control conditions are adopted to prepare the ultraviolet-proof dye, the ultraviolet-proof dye is applied to textiles, namely, the ultraviolet-proof dye is endowed to the textiles, and finally, the industrialization and recycling of the aloe skin are realized.
In order to achieve the technical purpose, the following technical scheme is provided:
the technical proposal is as follows: an Aloe skin extract is prepared from Aloe skin by pulverizing, performing enzymolysis extraction, extracting with solvent, and concentrating under reduced pressure, wherein the Aloe skin extract comprises Aloesin, 7-O-Methylaloeresin A, aloe-emodin, aloin A, and Aloin B, and the structural formulas are as follows:
；
The dry aloe skin extract comprises 730.702 +/-28.871 mg of total phenols with gallic acid equivalent and 683.240 +/-13.199 mg of total flavonoids with catechin equivalent per 1g of dry aloe skin extract.
The technical proposal is as follows: a preparation method of aloe peel extract comprises the following steps:
1) Crushing: taking aloe peel as a raw material, cleaning, drying at 40 ℃, crushing, and sieving with a 40-mesh sieve to obtain aloe peel powder;
2) And (3) enzymolysis extraction: adding cellulase and deionized water into aloe powder, mixing, and heating to 65deg.C at a rate of 1deg.C/min to obtain aloe peel primary extract with pH of 4.5-6.5;
3) Extracting a solvent: adding solvent medium into the initial extract of aloe skin, controlling pH, heating at 25-65deg.C for 20-100min, and vacuum filtering to obtain final extract of aloe skin;
4) Concentrating: distilling the obtained aloe skin final extractive solution under reduced pressure, and lyophilizing at-60deg.C under 1.33Pa for 48 hr to obtain aloe skin extract.
Preferably, in step 1), the aloe skin is a waste aloe skin from which mesophyll is removed, and the waste aloe skin is generally formed by using fresh aloe as a raw material and preparing aloe gel, so that the resource recycling of the waste aloe skin 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 color anti-ultraviolet dye can be obtained; when the pH is controlled to be 7-8, the solvent medium is one or two of sodium carbonate and sodium bicarbonate, and the ultraviolet-proof dye with reddish brown color can be obtained subsequently.
The technical proposal is as follows: the obtained aloe skin 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 a mixture of more than two of copper ions, ferrous ions, aluminum ions and tannins.
In the technical scheme, the enzymolysis extraction mechanism comprises:
The active ingredients in aloe skin are present in the cytoplasm of plant cells. During the extraction process, the solvent needs to overcome the mass transfer resistance from the cell wall and the cell matrix. The cell wall is a compact structure formed by cellulose, hemicellulose, pectic substance and other substances, and proper enzymes (such as cellulase, hemicellulase and pectic enzyme) are selected for pretreatment of the Chinese medicinal materials, so that the cellulose, the hemicellulose and the pectin which form the cell wall can be decomposed, the structure of the cell wall is destroyed, local collapse, dissolution and loosening are generated, the resistance from the cell wall and the cell matrix during solvent extraction is reduced, the cell dissolution rate of the effective components is accelerated, the extraction efficiency is improved, and the extraction time is shortened;
The solvent extraction mechanism involved: flavonoid substances in aloe skin are relatively poor in water solubility, but are easily dissolved in hot alkaline water, so that acidic components are extracted in the form of salt. The substances extracted under different pH conditions are basically the same but have different concentrations, so that different hues can be displayed after dyeing, conditions such as pH can be adjusted according to actual production requirements, and the higher the non-extraction concentration is, the better;
Furthermore, the preservation of aloe peel extract involved: considering that the dye is liquid after being extracted, the dye is unfavorable for storage and transportation, the dye is stored in a solid form by adopting a reduced pressure distillation, freeze drying or vacuum drying method
By adopting the technical scheme, the beneficial technical effects brought are as follows:
1. The natural ultraviolet-proof dye provided by the invention is prepared by taking aloe skin (especially aloe skin discarded after mesophyll removal in the aloe product processing process) as a raw material, 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 environment pollution is reduced;
2. In the invention, aloe peel extract is obtained by taking Aloe peel as a raw material, and carrying out crushing, enzymolysis extraction, solvent extraction and reduced pressure distillation concentration, wherein the Aloe peel extract comprises Aloesin, 7-O-Methylaloeresin A, aloe-emodin, aloin A and Aloin B; and, based on each 1 gram of dry aloe skin extract, the dry aloe skin 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 dry aloe skin extract contains a large amount of active ingredients, so that the functional application of the aloe skin extract can be further developed, for example: an ultraviolet-proof dye;
3. In the present invention, the "drying at 40 ℃ condition" defined in step 1) in the aloe skin extraction process ensures the stability of the active ingredients and their contents in aloe skin, and the effectiveness of the extraction process, such as: excessive temperature will cause loss of part of the components in the aloe skin extract at high temperature (e.g. free anthraquinone is heated under normal pressure and is easily sublimated); when the temperature is too low, the drying is slower, the overall efficiency of the preparation process is affected, and the aloe skin is easy to mould in a low-temperature humid environment, so that the product quality of aloe skin extract and the stability of the extraction process are affected. The aloe powder is further controlled to pass through a 40-mesh sieve, and further, the particle size of the aloe powder in the subsequent extraction process is controlled, so that the specific surface area between the aloe powder and the cellulase is large, the extraction efficiency is further improved, the target components in the aloe extract are separated to the greatest extent, and the follow-up application of the aloe extract (ultraviolet-proof dye) is ensured on the premise;
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, further limit "use 15-55g cellulase per kilogram of aloe skin powder, use 8-25L deionized water per kilogram of aloe skin powder, add cellulase and deionized water to aloe skin powder obtained", guarantee effectively that the initial extract of aloe skin obtained under this condition, after the subsequent treatment, when using for ultraviolet-proof dyestuffs, can make the ultraviolet spectrophotometer measure absorbance and can obtain the maximum value;
Wherein, the substance extracted in the dosage range of the deionized water can obtain the maximum value when the ultraviolet spectrophotometer is used for measuring the absorbance. If the dosage of deionized water is too small, the viscosity of the extraction system is too high, so that the release of active ingredients is hindered; conversely, if the deionized water is used too little, the effective components are diluted, and the waste of water resources is caused;
In addition, the extraction efficiency and quality are ensured by further limiting the heating to 65 ℃ at the speed of 1 ℃/min, if the heating speed is too high, the temperature can be rapidly increased, so that the cellulase is inactivated after not fully playing a role, and the release of active ingredients is not facilitated; conversely, the heating rate is too slow, so that the cellulase can fully play a role, but the extraction period can be prolonged, and further energy waste and the like can be caused;
In the step 3), extraction solvent media with different pH values are used, the color tone of the dye in the subsequent dyeing can be adjusted, a precondition guarantee is provided for the application of the aloe skin extract, and the applicability of the aloe skin extract is further improved, wherein the condition of heating at constant temperature of 25-65 ℃ for 20-100min is further limited, so that the re-extraction of active ingredients in aloe skin is ensured, and a precondition guarantee is provided for the next concentration, and if the temperature is too low, the active ingredients are difficult to extract; if the temperature is too high, the active ingredients are deteriorated, degraded, etc., and the kinds and contents of the active ingredients in the aloe skin extract cannot be ensured.
In the step 4), the method is limited to' freeze-drying for 48 hours under the conditions that the pressure is 1.33Pa and the temperature is minus 60 ℃, so that the concentration quality and efficiency of the aloe skin final extract are ensured, and the variety and the storage quantity of active ingredients in the aloe skin extract are ensured;
4. the aloe skin extract is used in the ultraviolet-proof dye, and different mordant methods and mordants are used, so that the dyeing depth and the dyeing 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 dye and textile with low cost, environment friendliness, naturalness and no toxicity and ultraviolet resistance, wherein the related aloe skin extract (ultraviolet resistance dye) is a green, environment-friendly and nontoxic reagent from raw materials to a final finished product in the processing process, the utilization rate of the waste aloe skin can be improved, and the related cost, energy consumption and product stability are low.
Drawings
FIG. 1 is a graph showing the analysis of the components of aloe vera skin extract using ultraviolet spectrum in example 4;
FIG. 2 is a graph showing the analysis of the components of aloe vera skin extract using infrared spectroscopy in example 4;
FIG. 3 shows the dyeing effect of silk dyed with UV-proof dye after pre-mordant-free, aluminum ion, copper ion, and ferrous ion as mordants in example 5;
FIG. 4 shows the dyeing effect (different dyeing temperatures) of mordant-free, aluminum ion, copper ion, ferrous ion, and tannin-free mordant and UV-resistant dye one-bath mordant silk in example 6;
FIG. 5 shows the dyeing effect (different dyeing times) of mordant-free, aluminum ion, copper ion, ferrous ion, and tannin-free mordant and UV-resistant dye one-bath mordant silk in example 6;
Fig. 6 shows the dyeing effect (different dye bath pH) of mordant-free, aluminum ion, copper ion, ferrous ion, and tannin-free mordant and uv-resistant dye one-bath mordant silk in example 6.
Detailed Description
In the following, it is obvious that the embodiments described are only some embodiments of the present invention, but not all embodiments, by clearly and completely describing the technical solutions in the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The Aloe skin extract is prepared by taking Aloe skin as a raw material, and carrying out crushing, enzymolysis extraction, solvent extraction and reduced pressure distillation concentration, wherein the Aloe skin extract comprises Aloesin, 7-O-Methylaloeresin A, aloe-emodin, aloin A and Aloin B, and the structural formulas respectively relate to the following structural formulas:
；
The dry aloe skin extract comprises 730.702 +/-28.871 mg gallic acid equivalent and 683.240 +/-13.199 mg catechin equivalent total phenols and flavonoid compounds per 1g of dry aloe skin extract.
Example 2
The preparation method of the aloe peel extract comprises the following steps:
1) Crushing: taking aloe peel as a raw material, cleaning, drying at 40 ℃, crushing, and sieving with a 40-mesh sieve to obtain aloe peel powder;
2) And (3) enzymolysis extraction: adding cellulase and deionized water into aloe powder, mixing, and heating to 65deg.C at a rate of 1deg.C/min to obtain aloe peel primary extract with pH of 4.5-6.5;
3) Extracting a solvent: adding solvent medium into the initial extract of aloe skin, controlling pH, heating at 25-65deg.C for 20-100min, and vacuum filtering to obtain final extract of aloe skin;
4) Concentrating: distilling the obtained aloe skin final extractive solution under reduced pressure, and lyophilizing at-60deg.C under 1.33Pa for 48 hr to obtain aloe skin extract.
In step 1), the aloe skin is a waste aloe skin from which mesophyll is removed, and the waste aloe skin is generally formed by taking fresh aloe as a raw material and preparing aloe gel, so that the resource recycling of the waste aloe skin 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 two of sodium carbonate and sodium bicarbonate, and the ultraviolet-proof dye with reddish brown color can be obtained subsequently.
Example 3
Based on embodiments 1-2, the present embodiment provides that the obtained aloe skin 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 a mixture of more than two of copper ions, ferrous ions, aluminum ions and tannins.
Example 4
Based on examples 1-3, the present example further analyzed the components of aloe skin extract to further illustrate the present technical scheme.
1. Component analysis of aloe skin extract by ultraviolet spectrum
As a result, as shown in FIG. 1, five absorption bands appear in the spectrum in the wavelength range of 200-400nm, and it can be inferred that aloe dye may have one long-chain conjugated chromophore or one polycyclic aromatic hydrocarbon chromophore, and that the molecule contains at least 4-5 conjugated chromophores and a color assisting group. Wherein, 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 absorbance peak at 268nm is caused by the p-quinone structure, while the absorbance peak at 340nm is caused by the benzoyl structure.
2. Component analysis of aloe bark extract by infrared spectrum
As a result, as shown in FIG. 2, the broad band around 3402 cm -1 represents the stretching vibration of phenolic hydroxyl groups, the low intensity peak at 2930 cm -1 represents the aromatic-CH stretching vibration, the high intensity peak at 1592 cm -1 corresponds to the double bond conjugated ketone group of polyphenol/flavone, the strong peak at 1415 cm -1 belongs to the-C-O stretching vibration, corresponds to the double bond conjugated ketone group in polyphenol/flavone, and the peaks at 1259 cm -1 and 621 cm -1 represent the in-plane and out-of-plane-C-O bending vibration of polyphenol and flavone.
3. Analysis of total phenols and total flavonoids content in aloe bark extract
The total phenols and total flavonoids are important secondary metabolites synthesized by plants and can protect the plants from ultraviolet irradiation, wherein the total phenol content in aloe dye is calculated by gallic acid calibration curve: y=5.3294x+0.00838, r 2 = 0.9978 (0.02-0.3 mg/mL), total flavone content calculated from catechin calibration curve: y=0.4418x+0.00478, r 2 =0.9962 (0.02-0.3 mg/mL);
The results show that total phenols and flavonoids in 1g of dry aloe peel extract contained 730.702.+ -. 28.871mg (gallic acid equivalent) and 683.240.+ -. 13.199mg (catechin equivalent), respectively.
In summary, the material composition and the content of the aloe peel extract can be deduced through ultraviolet spectrum, fourier transform spectrum analysis and total polyphenol and flavone content analysis.
Example 5
The embodiment provides a preparation method of aloe peel extract, which comprises the following steps:
1) Crushing: taking waste aloe peel as a raw material, cleaning, drying in a drying oven at 40 ℃, crushing by a universal crusher, and sieving by a 40-mesh sieve to obtain aloe peel powder;
2) And (3) enzymolysis extraction: adding cellulase and deionized water into aloe powder, mixing, and heating to 65deg.C at a rate of 1deg.C/min to obtain aloe peel primary extract with pH of 5.5, wherein 35g cellulase (activity not less than 35U/mg) is used per kg aloe peel powder, and 25L deionized water is used per kg aloe peel powder;
3) Extracting a solvent: deep extracting with alkaline solvent medium, namely adding sodium carbonate powder into the initial aloe peel extract, controlling pH to 8, heating at 65deg.C for 1 hr, and vacuum filtering to obtain final aloe peel extract;
4) Concentrating: and (3) distilling the aloe skin final extract under reduced pressure, and freeze-drying for 48h to obtain aloe skin extract, thereby obtaining the ultraviolet-proof dye.
Based on the aloe skin extract obtained above, the method is used for dyeing silk, so as to further explain the technical scheme.
1. Dyeing
Wherein, after pre-mordant-free mordant, aluminum ion, copper ion and ferrous ion are used as mordants, the obtained aloe skin extract is used for dyeing silk, and the specific steps are as follows:
X1: pre-mordant, wherein the mordant mass ratio is 8% of the weight of silk fabric, and the bath ratio is 1:50, primary dyeing at 40 ℃, heating to 90 ℃ at 1 ℃/min, and preserving heat for 45 min;
x2: dyeing, namely taking out silk after the mordant bath is cooled to room temperature, putting the silk into a dye bath, performing primary dyeing at 40 ℃, heating to 90 ℃ at 1 ℃/min, and preserving heat for 60 min;
x3: and cooling the dye bath to room temperature, washing with water fully, and airing to obtain the dye bath.
2. Evaluation of dyeing Effect
Wherein the standard according to which the data is stored is,
Washing fastness: the soaping-resistant color fastness was detected according to the method specified in GB/T3921-2008 textile color fastness to soaping test.
Rubbing fastness: the rubbing color fastness was measured according to the method specified in GB/T3920-2008 fabrics color fastness to rubbing test.
3. Evaluation of ultraviolet-proof Effect
According to AATCC 61-2013 fastness to washing: and (3) washing the dyed fabric for 5, 10, 15, 20 and 25 times by an acceleration method, and testing the ultraviolet resistance of the fabric by adopting an ultraviolet resistance tester of the fabric.
The color fastness and ultraviolet-proof effect of silk dyed with the aloe skin extract obtained above were measured according to the above standards, respectively, and the results obtained are shown in tables 1-2 and fig. 3 below.
Example 6
The embodiment provides a preparation method of aloe peel extract, which comprises the following steps:
1) Crushing: taking waste aloe peel as a raw material, cleaning, drying in a drying oven at 40 ℃, crushing by a universal crusher, and sieving by a 40-mesh sieve to obtain aloe peel powder;
2) And (3) enzymolysis extraction: adding cellulase and deionized water into aloe powder, mixing, and heating to 65deg.C at a rate of 1deg.C/min to obtain aloe peel primary extract with pH of 5.5, wherein 15g cellulase (activity not less than 35U/mg) is used per kg aloe peel powder, and 15L deionized water is used per kg aloe peel powder;
3) Extracting a solvent: deep extracting with acidic solvent medium, namely adding glacial acetic acid into the initial extract of aloe skin, controlling pH to 5, heating at 65deg.C for 1 hr, and vacuum filtering to obtain final extract of aloe skin;
4) Concentrating: and (3) distilling the obtained aloe skin final extract under reduced pressure, and freeze-drying for 48h to obtain aloe skin extract.
The aloe skin extract (namely ultraviolet-proof dye) obtained based on the above is used for dyeing silk, so as to further explain the technical scheme.
1. Dyeing
After mordant-free, aluminum ion, copper ion and ferrous ion are used as mordants for pre-mordant dyeing, the obtained ultraviolet-proof dye is used for one-bath mordant dyeing of silk, and the method comprises the following steps of:
Y1: preparing a dye bath, adding a corresponding mordant into the obtained aloe skin extract, wherein 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 to 1:50;
y2: dyeing, namely, primarily dyeing silk at 40 ℃, heating to 50-90 ℃ at 1 ℃/min, and preserving heat for 30-90 min;
Y3: and cooling the dye bath to room temperature, washing with water fully, and airing 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 and FIGS. 4 to 6 below.
3. Evaluation of ultraviolet-proof Effect
The ultraviolet resistance of the textile was measured using an ultraviolet resistance tester, and the results are shown in table 6 below.
Example 7
The extraction conditions involved in the preparation process of the ultraviolet-proof dye are examined in the embodiment to further explain the technical scheme.
The method comprises the steps of selecting four factors of cellulase addition amount, enzymolysis liquid pH, enzymolysis temperature and enzymolysis time, respectively examining the influence of the four factors on the extraction efficiency of the ultraviolet-proof dye, and representing the extraction efficiency by using absorbance at the maximum absorption wavelength of an ultraviolet spectrum. The results obtained are shown in Table 7 below.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (4)
1. A preparation method of aloe peel extract used for ultraviolet-proof dye is characterized by comprising the following steps:
1) Crushing: taking aloe peel as a raw material, cleaning, drying at 40 ℃, crushing, and sieving with a 40-mesh sieve to obtain aloe peel powder;
2) And (3) enzymolysis extraction: adding cellulase and deionized water into aloe powder, mixing, and heating to 65deg.C at a rate of 1deg.C/min to obtain aloe peel primary extract with pH of 4.5-6.5;
3) Extracting a solvent: adding solvent medium for controlling pH value into the initial extract of aloe skin, heating at 25-65deg.C for 20-100min, and vacuum filtering to obtain final extract of aloe skin;
4) Concentrating: distilling the obtained aloe skin final extract under reduced pressure, and freeze drying at-60deg.C under 1.33Pa for 48 hr to obtain aloe skin extract for ultraviolet-proof dye;
The aloe skin extract for the ultraviolet-proof dye in the dry state comprises 730.702 +/-28.871 mg of total phenolic substances with gallic acid equivalent and 683.240 +/-13.199 mg of total flavonoid compounds with catechin equivalent per 1 g of aloe skin extract for the ultraviolet-proof dye in the dry state.
2. The method of preparing aloe skin extract for ultraviolet-screening dye according to claim 1, wherein in step 1), the aloe skin is discarded aloe skin after mesophyll removal.
3. The method for preparing aloe vera skin extract for use in uv-blocking dyes according to claim 1, wherein in step 3), the solvent medium is glacial acetic acid when the pH is controlled to be 4-7; when the pH is controlled to 7-8, the solvent medium is one or two of sodium carbonate and sodium bicarbonate.
4. The method for preparing aloe vera skin extract for ultraviolet-proof dye according to claim 1, wherein in the use of the ultraviolet-proof dye, 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 a mixture of any two or more of copper ions, ferrous ions, aluminum ions and tannins.
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| 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 |
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| 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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