阅读说明：本技术 一种木质素基防晒霜的制备方法 (Preparation method of lignin-based sunscreen cream ) 是由 陈海燕 刘子夜 冯印 张群 崔鹏程 胡楠楠 于 2020-08-21 设计创作，主要内容包括：本发明公开了一种木质素基防晒霜的制备方法,包括以下步骤：S1超临界二氧化碳萃取白桦树皮粉末；S2正交试验确定最佳提取工艺,高沸醇溶剂提取法提取木质素提取物；S3木质素提取物的毒性试验,筛选木质素提取物；S4将木质素提取物与纯乳液、乙醇混合搅拌,得到不同木质素基防晒霜；S5进行UV测定确定木质素添加量,得到所述的木质素基防晒霜产品；本发明的有益效果是：通过超临界二氧化碳技术、高沸醇溶剂提取法,再经过毒害试验和UV测定,利用纯乳液和乙醇,形成木质素基防晒霜；通过采用碱性物质以及抗氧化植物油、表面活性剂、保湿剂、乳化剂以及防腐剂,实现防晒霜的高防晒性能；通过正交试验,实现高纯度木质素提取。(The invention discloses a preparation method of lignin-based sunscreen cream, which comprises the following steps: s1 extracting birch bark powder with supercritical carbon dioxide; s2 orthogonal test to determine the best extraction process, extracting lignin extract with high boiling alcohol solvent; s3 toxicity test of lignin extract, screening the lignin extract; s4, mixing and stirring the lignin extract, the pure emulsion and ethanol to obtain different lignin-based sunscreen creams; s5, performing UV measurement to determine the addition amount of lignin, and obtaining the lignin-based sunscreen cream product; the invention has the beneficial effects that: forming lignin-based sunscreen cream by using a supercritical carbon dioxide technology, a high-boiling alcohol solvent extraction method, a poisoning test and UV (ultraviolet) measurement and using pure emulsion and ethanol; the high sun-screening performance of the sun-screening cream is realized by adopting alkaline substances, antioxidant vegetable oil, a surfactant, a humectant, an emulsifier and a preservative; through orthogonal experiments, high-purity lignin extraction is realized.)

1. A preparation method of lignin-based sunscreen cream is characterized by comprising the following steps: the method comprises the following steps:

s1 extracting cortex Betulae Pendulae powder with supercritical carbon dioxide, and vacuum drying the obtained extract to obtain cortex Betulae Pendulae extract residue;

s2, after determining the best extraction process through an orthogonal test, extracting lignin in the birch bark extract residue by adopting a high-boiling-point alcohol solvent extraction method to obtain a lignin extract;

s3, subjecting the obtained lignin extract to toxicity test to determine the toxicity of the lignin extract, and obtaining qualified lignin extract;

s4, mixing and stirring the qualified lignin extract, pure emulsion and ethanol according to different proportions to obtain lignin-based sunscreen creams with different gradient concentrations;

s5, performing UV measurement on the lignin-based sunscreen cream with different gradient concentrations, and determining the lignin-based sunscreen cream with the most appropriate lignin addition amount to obtain the lignin-based sunscreen cream product.

2. The preparation method of the lignin-based sunscreen cream according to claim 1, characterized in that: the pure emulsion comprises, by weight, 5-15 parts of glycerol, 0-6 parts of petrolatum, 1-3 parts of cetyl alcohol, 0-6 parts of sunflower seed oil, 1-10 parts of tocopherol, 1-10 parts of sodium hydroxide, 1-10 parts of disodium EDTA, 0.1-1.5 parts of phenoxyethanol, 0.1-0.5 part of propylene glycol, 0-6 parts of sweet almond oil, 1-3 parts of tocopherol acetate, 1-3 parts of dioctyl ether, 1-3 parts of dimethiconol, 5-15 parts of glycerol stearate, 5-15 parts of PEG30 stearate, 0.1-0.5 part of acrylic acid ((esters))/C-30 alkanol acrylate cross-linked polymer, 0.1-0.5 part of benzyl alcohol, 1-10 parts of butylated hydroxytoluene and 1-10 parts of carbomer, the balance being water.

3. The preparation method of the lignin-based sunscreen cream according to claim 1, characterized in that: the orthogonal test is designed by using the extraction temperature, the extraction time, the liquid-solid ratio and the volume fraction of the solvent.

4. The preparation method of the lignin-based sunscreen cream according to claim 1, characterized in that: the toxicity test is to adopt zebra fish as an experimental object, take zebra fish wild-type embryos (n ═ 30) 6h after fertilization and larval fish (n ═ 30) 3 days after fertilization as an administration group, prepare lignin extracts according to experimental gradient concentration, add the lignin extracts in an oral way, record abnormal phenotype and death rate of the administration group, repeat three times of experiments of the lignin extracts with each gradient concentration, and judge qualified lignin-based sunscreen cream.

5. The preparation method of the lignin-based sunscreen cream according to claim 4, characterized in that: the concentration of the experimental gradient is 10, 50 and 100 g/mL.

6. The preparation method of the lignin-based sunscreen cream according to claim 1, characterized in that: the mixing and stirring requirements are that the addition amount of the lignin extract accounts for less than 5% of the total weight of the lignin-based sunscreen cream.

7. The preparation method of the lignin-based sunscreen cream according to claim 1, characterized in that: the different gradient concentrations are lignin-based sunscreen cream with the mass fractions of 0%, 0.5%, 1.0%, 2.0% and 5.0%, respectively.

Technical Field

The invention relates to the field of application of lignin, in particular to a preparation method of lignin-based sunscreen cream.

Background

The lignin is an amorphous aromatic polymer which is mainly formed by connecting structural units of guaiacyl (G), syringyl (S) and p-hydroxyphenyl (H) through carbon-carbon bonds and ether bonds. Wherein, the functional groups of lignin mainly comprise methoxyl, phenolic hydroxyl, aliphatic hydroxyl and carboxyl, the lignin which accounts for over 5 million tons in the pulping and biorefinery industry is generated as waste material every year, however, only 2 to 5 percent of the lignin is utilized, and the others are mainly used for burning and landfill, which not only causes serious resource waste but also brings heavy pressure to the environment, therefore, the expansion of the use field of the lignin becomes one of the problems to be solved at present.

On the other hand, lignin is a natural high molecular compound rich in aromatic structures, so that the lignin can be used as a dye dispersant or a sunscreen additive, the high-value utilization of the lignin is pushed to a new height, but the industrial lignin extraction has a darker color, which completely limits the development of the lignin in the directions.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide a preparation method of lignin-based sunscreen cream, so as to at least achieve the aims of high-purity lignin extraction and high sunscreen performance.

The purpose of the invention is realized by the following technical scheme:

a preparation method of a lignin-based sunscreen cream comprises the following steps:

s1 extracting cortex Betulae Pendulae powder with supercritical carbon dioxide, and vacuum drying the obtained extract to obtain cortex Betulae Pendulae extract residue;

s2, after determining the best extraction process through an orthogonal test, extracting lignin in the birch bark extract residue by adopting a high-boiling-point alcohol solvent extraction method to obtain a lignin extract;

s3, subjecting the obtained lignin extract to toxicity test to determine the toxicity of the lignin extract, and obtaining qualified lignin extract;

s4, mixing and stirring the qualified lignin extract, pure emulsion and ethanol according to different proportions to obtain lignin-based sunscreen creams with different gradient concentrations;

s5, performing UV measurement on the lignin-based sunscreen cream with different gradient concentrations, and determining the lignin-based sunscreen cream with the most appropriate lignin addition amount to obtain the lignin-based sunscreen cream product.

Preferably, for the purpose of further realizing high sun-screening performance, the pure emulsion comprises, by weight, 5-15 parts of glycerin, 0-6 parts of petrolatum, 1-3 parts of cetyl alcohol, 0-6 parts of sunflower seed oil, 1-10 parts of tocopherol, 1-10 parts of sodium hydroxide, 1-10 parts of disodium EDTA, 0.1-1.5 parts of phenoxyethanol, 0.1-0.5 parts of propylene glycol, 0-6 parts of sweet almond oil, 1-3 parts of tocopherol acetate, 1-3 parts of dioctyl ether, 1-3 parts of dimethiconol, 5-15 parts of glycerol stearate, 5-15 parts of PEG30 stearate, 0.1-0.5 parts of acrylic acid ((esters))/C-30 alkanol acrylate cross-linked polymer, 0.1-0.5 parts of benzyl alcohol, 0-15 parts of glycerin stearate, 5-15 parts of PEG30 stearate, 0.1-0.5 parts of acrylic acid esters))/C-30 alkanol acrylate cross-linked polymer, and the like, 1-10 parts of butylated hydroxytoluene, 1-10 parts of carbomer and the balance of water; by adopting various alkaline substances, various antioxidant vegetable oils, surfactants, humectants, emulsifiers and preservatives, the raw materials of the lignin and various pure emulsions are quickly fused under the action of the surfactants, and the sunscreen cream is used for a long time under the action of the preservatives, meanwhile, various aromatic hydrocarbons are adopted in the formula, so that the product smell of the sunscreen cream is more aromatic, the protection of the sunscreen cream on the face skin can be enhanced by adopting the various humectants and the antioxidant vegetable oils, finally, the alkaline substances are used as the activating components of the surfactants, the uniformity of the emulsion state of the whole sunscreen cream is realized, and the purpose of high sunscreen performance in the sunscreen cream is further realized.

Preferably, for the purpose of further realizing high-purity lignin extraction, the orthogonal test is designed by taking the extraction temperature, the extraction time, the liquid-solid ratio and the volume fraction of the solvent as the basis; through the orthogonal test, each condition of the lignin extraction stage is determined, so that accurate and efficient lignin extraction is realized, and meanwhile, the orthogonal test can also determine the lignin extraction condition with higher purity, so that the aim of extracting the lignin with high purity is fulfilled.

Preferably, in order to further achieve the purpose of no toxicity of the lignin addition, the toxicity test is to adopt zebra fish as an experimental object, take 6h of zebra fish wild-type embryo (n ═ 30) after fertilization and 3 days of larva fish (n ═ 30) after fertilization as administration groups, prepare lignin extracts according to experimental gradient concentration, add the lignin extracts in an oral mode, record abnormal expression and death rate of the administration groups, repeat three times of experiments of the lignin extracts with each gradient concentration, and judge qualified lignin-based sunscreen cream; the concentration of the experimental gradient is 10, 50 and 100 g/mL; through a toxicity test, the toxicity effect of the adopted lignin concentration on the skin of animals is determined, and the sensitivity of the skin of the zebra fish is utilized to sensitively detect whether the added lignin concentration has influence on the skin or not, so that the aim of adding no toxicity is fulfilled.

Preferably, in order to further achieve high sunscreen performance, the mixing and stirring requirements are that the addition amount of the lignin extract accounts for less than 5% of the total weight of the lignin-based sunscreen cream; the addition range of the lignin extract is limited, so that the skin is prevented from being damaged by excessive lignin, and meanwhile, the stability of the emulsion state of the sunscreen cream is not influenced by adding a proper amount of the lignin extract, and the overall sunscreen performance of the sunscreen cream can be improved.

Preferably, for the purpose of further achieving high sun-screening performance, the different gradient concentrations are 0%, 0.5%, 1.0%, 2.0%, 5.0% of lignin-based sunscreen cream by mass fraction; the lignin-based sunscreen cream with different gradient concentrations is prepared, and then the UV determination is carried out, so that the proper lignin addition amount is judged, the lignin resource is saved, and the sunscreen performance of the sunscreen cream can be improved.

The invention has the beneficial effects that:

1. the method comprises the steps of extracting betulin in birch barks by combining a supercritical carbon dioxide technology and a high-boiling-point alcohol solvent extraction method, then extracting lignin in birch bark extract residues by using the high-boiling-point alcohol solvent extraction method, fully utilizing biological industrial wastes, simultaneously extracting high-purity lignin with light color, determining proper lignin addition amount by a toxicity test and UV measurement, and then uniformly forming sunscreen cream with the lignin and pure emulsion by using pure emulsion and ethanol.

2. By adopting various alkaline substances, various antioxidant vegetable oils, surfactants, humectants, emulsifiers and preservatives, the raw materials of the lignin and various pure emulsions are quickly fused under the action of the surfactants, and the sunscreen cream is used for a long time under the action of the preservatives, meanwhile, various aromatic hydrocarbons are adopted in the formula, so that the product smell of the sunscreen cream is more aromatic, the protection of the sunscreen cream on the face skin can be enhanced by adopting the various humectants and the antioxidant vegetable oils, finally, the alkaline substances are used as the activating components of the surfactants, the uniformity of the emulsion state of the whole sunscreen cream is realized, and the purpose of high sunscreen performance in the sunscreen cream is further realized.

3. Through the orthogonal test, each condition of the lignin extraction stage is determined, so that accurate and efficient lignin extraction is realized, and meanwhile, the orthogonal test can also determine the lignin extraction condition with higher purity, so that the aim of extracting the lignin with high purity is fulfilled.

4. Through a toxicity test, the toxicity effect of the adopted lignin concentration on the skin of animals is determined, and the sensitivity of the skin of the zebra fish is utilized to sensitively detect whether the added lignin concentration has influence on the skin or not, so that the aim of adding no toxicity is fulfilled.

5. The lignin-based sunscreen cream with different gradient concentrations is prepared, and then the UV determination is carried out, so that the proper lignin addition amount is judged, the lignin resource is saved, and the sunscreen performance of the sunscreen cream can be improved.

Drawings

FIG. 1 is an electron microscope image of mouse skin tissue in the anti-UV experiment of the invention,

wherein, a) is an electron microscope image of a normal group, b) is an electron microscope image of a lignin-based sunscreen cream group, and c) is an electron microscope image of a blank group.

Detailed Description

The technical solutions of the present invention are further described in detail below with reference to the accompanying drawings, but the scope of the present invention is not limited to the following.