CN110934769A - Preparation method and application of light-color bagasse-based lignin - Google Patents
Preparation method and application of light-color bagasse-based lignin Download PDFInfo
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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Abstract
The invention discloses a preparation method and application of light-colored bagasse-based lignin. The light-color bagasse-based lignin prepared by the method has the advantages of light particle color, small particle size, high ultraviolet protection performance and wide application prospect in the field of fine chemical engineering, and the content of phenolic hydroxyl groups is 1.5-2.5 mmol/g. In addition, the synergistic effect generated by mixing the sunscreen composition with a commercial sunscreen agent further enhances the ultraviolet protection effect, and has good market potential in the field of sunscreen and skin care.
Description
Technical Field
The invention belongs to the technical field of lignin preparation, and particularly relates to a preparation method and application of light-color bagasse-based lignin.
Background
Lignocellulose is an important component of biomass resources and is mainly composed of cellulose, lignin and hemicellulose. The lignin content is second to cellulose, is the biomass resource with the second highest reserves in the world, and is known as one of the most abundant green resources which can be utilized by human in the 21 st century. Bagasse is a main byproduct in the sugar industry of sugarcane, and is a renewable biomass resource with rich source and low price. The components contain a large amount of lignin. The primary application of lignin is direct combustion for power generation. However, as the only aromatic polymer in plants, the unique properties of lignin are endowed by the special structure of lignin, so that the high-value utilization of lignin is increasingly becoming a research hotspot. The lignin in the plant contains a large number of conjugated structures such as benzene rings, carbonyl groups, double bonds and the like, can effectively absorb ultraviolet rays in sunlight, and a large number of phenolic hydroxyl groups can effectively remove free radicals, so that the plant lignin has good ultraviolet resistance and oxidation resistance.
Currently, in the field of synthesis and preparation of sunscreen creams, the ultraviolet blocking agents mainly used include chemical sunscreens (avobenzone, octyl methoxycinnamate and the like) and physical sunscreens (titanium dioxide and zinc oxide). The chemical sunscreen agent has good sunscreen effect, but the organic compounds have poor photostability and certain irritation, are easy to cause skin allergy and inflammation, and are not suitable for fragile and sensitive skin. Compared with chemical sunscreens, physical sunscreens have higher safety, but also have the defects of difficult application, too heavy weight, whitening skin after use and the like. Some natural products such as extracts of coffee, soy, papaya, rose, and helichrysum have been sought as alternatives. These natural products do provide sunscreen benefits, but the blended sunscreen benefits are not ideal, only partially block uv light, and have limited blocking effectiveness, which is far less effective than synthetic sunscreen agents.
Lignin is a natural aromatic biomacromolecule with wide sources, has a good ultraviolet absorption characteristic in a broad-spectrum range, has high safety and good biocompatibility, and is one of research hotspots for high-value utilization of lignin by using the lignin as an additive to prepare the sunscreen cream. Qian Yong et al (Qian Y, Qiu X, Zhu S.Lignin: characteristic-isolated sun block for broad-spectrum sunscreen [ J ]. Green Chemistry, 2015, 17: 320-324.) prove for the first time that lignin has high-efficiency broad-spectrum sunscreen performance, alkali lignin is used as a raw material, and is blended with commercial sunscreen skin care products after purification, when the addition amount of the lignin is 2 wt%, the SPF value of the commercial SPF15 sunscreen skin care products is respectively increased to 35, and after 2h of ultraviolet irradiation, the ultraviolet absorption of the frost body is remarkably increased, which indicates that the lignin and the chemical sunscreen have synergistic effect. However, the lignin-based sunscreens prepared using the alkali lignin are very dark in color. Zhang H, Bai Y, Yu B, et al, A reactive process for lignin color reduction: fractionation of lignin using methane/water solvent [ J ]. Green Chem, 2017, 19: 5152-. Although the operation method is simple and feasible, the color of part of lignin is obviously reduced after classification, the dark apparent color is still shown, and the lignin cannot be fully utilized. Recently the authors (Zhang H, Liu X, Fu S, Chen Y.Industrial & engineering chemistry Research, 2019, 58, 13858 & 13867) produced light colored lignin microspheres of bamboo acetate, which also have a whiteness value of only 17.52%. Sang et al (Lee S C, TranT M T, Choi J W, et al, Lignin for white natural fruits [ J ]. International Journal of biological macromolecules, 2018, 122: 549-. The light lignin also showed synergistic effects with commercial sunscreens, but the process for isolating the light lignin was complex to operate, long-lasting, costly and low in lignin yield.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of light-color bagasse-based lignin.
Another object of the present invention is to provide the use of the above-mentioned light-colored bagasse-based lignin.
The technical scheme of the invention is as follows:
a preparation method of light-color bagasse-based lignin comprises the following steps:
(1) grinding bagasse into powder, sieving with a 55-65 mesh sieve, washing with water to remove most of sucrose and soluble impurities, drying, and grinding again to sieve with a 55-65 mesh sieve;
(2) preparing a p-toluenesulfonic acid solution, heating to 80-90 ℃, adding the material obtained in the step (1), keeping the temperature, stirring and reacting for 10-30 min;
(3) carrying out suction filtration on the material obtained in the step (2) to obtain a filtrate, fully diluting the filtrate with distilled water, standing for at least 24h, and separating out to obtain a bagasse-based lignin precipitate;
(4) washing the bagasse-based lignin precipitate with distilled water to neutrality, filtering, and freeze drying to obtain the light-color bagasse-based lignin with particle size of 200-300nm, phenolic hydroxyl group content of 1.5-2.5mmol/g, and whiteness of 22-38%.
In a preferred embodiment of the present invention, in the step (2), the concentration of the p-toluenesulfonic acid solution is 40 to 50 wt%.
Further preferably, in the step (2), the ratio of the p-toluenesulfonic acid solution to the material obtained in the step (1) is 55-65 mL: 2-4 g.
In a preferred embodiment of the present invention, in the step (3), the filtrate is diluted with distilled water to a concentration of p-toluenesulfonic acid of 3 to 5 wt%.
The other technical scheme of the invention is as follows:
the light-colored bagasse-based lignin prepared by the preparation method is applied to preparation of sunscreen compositions.
In a preferred embodiment of the invention, the amount of said light-colored bagasse-based lignin in said sunscreen composition is from 2 to 5 wt%.
The invention adopts another technical scheme as follows:
a sunscreen composition contains light-colored bagasse-based lignin prepared by the above preparation method as effective component.
In a preferred embodiment of the invention, the light-colored bagasse-based lignin is present in an amount of 2-5 wt%.
The invention has the beneficial effects that:
1. the method takes waste bagasse as a raw material, utilizes the p-toluenesulfonic acid to separate and extract lignin in one step, has mild reaction conditions, short reaction time, simple operation and no pollution in the whole process, can recycle the p-toluenesulfonic acid, and has low preparation cost.
2. The light-color bagasse-based lignin prepared by the method has the advantages of light particle color, small particle size, high ultraviolet protection performance and wide application prospect in the field of fine chemical engineering, and the content of phenolic hydroxyl groups is 1.5-2.5 mmol/g. In addition, the synergistic effect generated by mixing the sunscreen composition with a commercial sunscreen agent further enhances the ultraviolet protection effect, and has good market potential in the field of sunscreen and skin care.
Drawings
FIG. 1 is a graph showing the change in UV transmittance of light-colored bagasse-based lignin in different amounts mixed with a pure emulsion in example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of light-colored bagasse-based lignin prepared according to example 1 of the present invention.
FIG. 3 is a graph comparing the color of light-colored bagasse-based lignin produced in example 1 of the present invention with commercial alkali lignin.
FIG. 4 is a graph comparing the color of different loadings of light-colored bagasse-based lignin and commercial sunscreen creams in examples 2 and 3 of the present invention before and after mixing.
Detailed Description
The technical solution of the present invention will be further illustrated and described below with reference to the accompanying drawings by means of specific embodiments.
Example 1
(1) The bagasse is used as a raw material, and is mechanically ground into powder and sieved by a 60-mesh sieve, and the bagasse powder is washed by distilled water for multiple times to remove most of soluble sugar and impurities in the bagasse;
(2) preparing a 40 wt% p-toluenesulfonic acid solution, measuring 60mL into a round-bottom flask, heating in a water bath to 90 ℃, adding 2.5g of the material obtained in the step (1), and stirring for reaction for 15 min;
(3) and (3) after the reaction is finished, pouring the material obtained in the step (2) into a Buchner funnel for suction filtration to obtain filtrate, transferring the filtrate into a glass beaker, diluting the filtrate with distilled water until the concentration of the p-toluenesulfonic acid solution is 4 wt%, and standing for 24h to precipitate a large amount of bagasse-based lignin.
(4) The bagasse-based lignin precipitate was washed with distilled water repeatedly by centrifugation 3-4 times to neutrality, and then freeze-dried for 24 hours to give a light-colored bagasse-based lignin as shown in fig. 2 and 3, and the whiteness value was determined to be 37.23%.
The light-colored bagasse-based lignin prepared in this example was mixed with a blank emulsion (skin-caring emulsion for strengthening and beautifying) having no sunscreen effect in amounts of 1%, 2%, 5% and 10% by mass, respectively, and the ultraviolet transmittance change of the mixed emulsion was measured after stirring for 24 hours at normal temperature and pressure, with the results shown in fig. 1. The sun protection index of the mixed emulsion was calculated and the results are listed in table 1.
TABLE 1 results of the Effect of bagasse-based lignin addition on emulsion Sun protection index
| Sample (I) | Sun Protection Factor (SPF) |
| Emulsion (skin-care emulsion for strengthening body and beautifying skin) | 1.01±0.01 |
| Emulsion +1 wt% bagasse-based lignin | 1.62±0.07 |
| Emulsion +2 wt% bagasse-based lignin | 1.89±0.21 |
| Emulsion +5 wt% bagasse-based lignin | 2.59±0.24 |
| Emulsion +10 wt% bagasse-based lignin | 9.40±0.94 |
As can be seen from table 1, the sun protection index of the blank emulsion is very low; when 1 wt% and 2 wt% of bagasse-based lignin were added, the sun protection index of the mixed emulsion was slightly increased; when 5 wt% of light-colored bagasse-based lignin was added, the sun protection index rose to 2.59; when 10 wt% of light-colored bagasse-based lignin was added, there was a significant increase in the sun protection index of the mixed emulsion, as high as 9.40. The result shows that the light-color bagasse-based lignin has excellent ultraviolet protection performance and has good application prospect in the fields of sunscreen skin care products and the like.
Example 2
(1) The bagasse is used as a raw material, and is mechanically ground into powder and sieved by a 60-mesh sieve, and the bagasse powder is washed by distilled water for multiple times to remove most of soluble sugar and impurities in the bagasse;
(2) preparing a 40 wt% p-toluenesulfonic acid solution, measuring 60mL into a round-bottom flask, heating in a water bath to 90 ℃, adding 2.5g of the material obtained in the step (1), and stirring for reaction for 25 min;
(3) and (3) after the reaction is finished, pouring the material obtained in the step (2) into a Buchner funnel for suction filtration to obtain filtrate, transferring the filtrate into a glass beaker, diluting the filtrate with distilled water until the concentration of the p-toluenesulfonic acid solution is 4 wt%, and standing for 24h to precipitate a large amount of bagasse-based lignin.
(4) Washing bagasse-based lignin precipitate with distilled water repeatedly by centrifugation for 3-4 times to neutrality, and freeze-drying for 24h to obtain light-colored bagasse-based lignin, with a whiteness value of 30.49%.
The light-colored bagasse-based lignin prepared in this example was mixed with a commercial physical sunscreen cream (bevacizi baby sunscreen cream) in an amount of 2% and 5% by mass, respectively, and the sunscreen index of the mixed cream was measured and calculated after stirring for 24 hours at normal temperature and pressure, and the results are shown in table 2.
TABLE 2 results of the Effect of bagasse-based lignin addition on the Sun protection index of physical sunblocks
| Sample (I) | Sun Protection Factor (SPF) |
| Commercial physical sunscreen cream (Bei Qin baby sunscreen cream) | 13.26±3.50 |
| Commercial physical sunscreen cream +2 wt% bagasse-based lignin | 14.79±2.58 |
| Commercial physical sunscreen +5 wt% bagasse-based lignin | 41.86±4.70 |
As can be seen from table 2, the commercial physical sunscreen itself was determined to have a sun protection index of 13.26; when 2 wt% bagasse-based lignin was added, the sun protection index of the mixed frost was slightly increased, but not to a significant extent; when 5 wt% of light-colored bagasse-based lignin is added, the sun protection index of the mixed cream body is remarkably improved to 41.86, which is more than 3 times of that of the original commercial physical sun protection cream, and the color change after mixing is not obvious (figure 4 (left)), so that the basic requirements of people on the sun protection index of the sun protection cream and no skin pollution are completely met.
Example 3
(1) The bagasse is used as a raw material, and is mechanically ground into powder and sieved by a 60-mesh sieve, and the bagasse powder is washed by distilled water for multiple times to remove most of soluble sugar and impurities in the bagasse;
(2) preparing a 40 wt% p-toluenesulfonic acid solution, measuring 60mL into a round-bottom flask, heating in a water bath to 90 ℃, adding 2.5g of the material obtained in the step (1), and stirring for reaction for 30 min;
(3) and (3) after the reaction is finished, pouring the material obtained in the step (2) into a Buchner funnel for suction filtration to obtain filtrate, transferring the filtrate into a glass beaker, diluting the filtrate with distilled water until the concentration of the p-toluenesulfonic acid solution is 4 wt%, and standing for 24h to precipitate a large amount of bagasse-based lignin.
(4) Washing bagasse-based lignin precipitate with distilled water repeatedly by centrifugation for 3-4 times to neutrality, and freeze-drying for 24h to obtain light-colored bagasse-based lignin with a whiteness value of 22.07%.
The light-colored bagasse-based lignin prepared in this example was mixed with a commercial chemical sunscreen cream (sitaflo moisturizing sunscreen cream) in an amount of 2% by mass and 5% by mass, and the sunscreen index of the mixed cream body was calculated by testing after stirring for 24 hours at normal temperature and pressure, and the results are shown in table 3.
TABLE 3 results of the Effect of bagasse-based lignin addition on the sun protection index of chemical sunscreen
| Sample (I) | Sun Protection Factor (SPF) |
| Commercial chemical sunscreen cream (Sitafu moisturizing sunscreen cream) | 11.00±0.08 |
| Commercial chemical sunscreen cream +2 wt% bagasse-based lignin | 21.20±2.27 |
| Commercial chemical sunscreen cream +5 wt% bagasse-based lignin | 44.02±3.24 |
As can be seen from table 3, the commercial chemical sunscreen itself was determined to have a sun protection index of 11.00; when 2 wt% of bagasse-based lignin is added, the sun protection index of the mixed frost is obviously improved, and the sun protection index reaches 21.20; when 5 wt% of light-colored bagasse-based lignin was added, the sun protection index of the mixed cream body was further increased to 44.02, which is 4 times that of the original commercial chemical sunscreen cream. Due to the synergistic effect between lignin and chemical sunscreen agents, the addition of a small amount of lignin can significantly enhance sunscreen performance with insignificant color change after mixing (fig. 4 (right)). The results show that the light-color bagasse-based lignin is light in color, does not stain the skin, is expected to replace the traditional sun-screening agent, becomes a new-generation green natural high-molecular ultraviolet protective agent, and has wide market prospect.
Example 4
(1) The bagasse is used as a raw material, and is mechanically ground into powder and sieved by a 60-mesh sieve, and the bagasse powder is washed by distilled water for multiple times to remove most of soluble sugar and impurities in the bagasse;
(2) preparing a 50 wt% p-toluenesulfonic acid solution, measuring 60mL into a round-bottom flask, heating in a water bath to 90 ℃, adding 2.5g of the material obtained in the step (1), and stirring for reaction for 10 min;
(3) and (3) after the reaction is finished, pouring the material obtained in the step (2) into a Buchner funnel for suction filtration to obtain filtrate, transferring the filtrate into a glass beaker, diluting the filtrate with distilled water until the concentration of the p-toluenesulfonic acid solution is 4 wt%, and standing for 24h to precipitate a large amount of bagasse-based lignin.
(4) Washing bagasse-based lignin precipitate with distilled water repeatedly by centrifugation for 3-4 times to neutrality, and freeze-drying for 24h to obtain light-colored bagasse-based lignin.
Example 5
(1) The bagasse is used as a raw material, and is mechanically ground into powder and sieved by a 60-mesh sieve, and the bagasse powder is washed by distilled water for multiple times to remove most of soluble sugar and impurities in the bagasse;
(2) preparing a 50 wt% p-toluenesulfonic acid solution, measuring 60mL into a round-bottom flask, heating in a water bath to 90 ℃, adding 2.5g of the material obtained in the step (1), and stirring for reaction for 15 min;
(3) and (3) after the reaction is finished, pouring the material obtained in the step (2) into a Buchner funnel for suction filtration to obtain filtrate, transferring the filtrate into a glass beaker, diluting the filtrate with distilled water until the concentration of the p-toluenesulfonic acid solution is 4 wt%, standing for 24h, and precipitating a large amount of bagasse-based lignin.
(4) Washing bagasse-based lignin precipitate with distilled water repeatedly by centrifugation for 3-4 times to neutrality, and freeze-drying for 24h to obtain light-colored bagasse-based lignin.
Example 6
(1) The bagasse is used as a raw material, and is mechanically ground into powder and sieved by a 60-mesh sieve, and the bagasse powder is washed by distilled water for multiple times to remove most of soluble sugar and impurities in the bagasse;
(2) preparing a 50 wt% p-toluenesulfonic acid solution, measuring 60mL into a round-bottom flask, heating in a water bath to 80 ℃, adding 2.5g of the material obtained in the step (1), and stirring for reaction for 20 min;
(3) and (3) after the reaction is finished, pouring the material obtained in the step (2) into a Buchner funnel for suction filtration to obtain filtrate, transferring the filtrate into a glass beaker, diluting the filtrate with distilled water until the concentration of the p-toluenesulfonic acid solution is 4 wt%, and standing for 24h to precipitate a large amount of bagasse-based lignin.
(4) Washing bagasse-based lignin precipitate with distilled water repeatedly by centrifugation for 3-4 times to neutrality, and freeze-drying for 24h to obtain light-colored bagasse-based lignin.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (8)
1. A preparation method of light-color bagasse-based lignin is characterized by comprising the following steps: the method comprises the following steps:
(1) grinding bagasse into powder, sieving with a 55-65 mesh sieve, washing with water to remove most of sucrose and soluble impurities, drying, and grinding again to sieve with a 55-65 mesh sieve;
(2) preparing a p-toluenesulfonic acid solution, heating to 80-90 ℃, adding the material obtained in the step (1), keeping the temperature, stirring and reacting for 10-30 min;
(3) carrying out suction filtration on the material obtained in the step (2) to obtain a filtrate, fully diluting the filtrate with distilled water, standing for at least 24h, and separating out to obtain a bagasse-based lignin precipitate;
(4) washing the bagasse-based lignin precipitate with distilled water to neutrality, filtering, and freeze drying to obtain the bagasse-based lignin with particle size of 200-300nm, phenolic hydroxyl group content of 1.5-2.5mmol/g, and whiteness of 22-38%.
2. The method of claim 1, wherein: in the step (2), the concentration of the p-toluenesulfonic acid solution is 40-50 wt%.
3. The method of claim 2, wherein: in the step (2), the ratio of the p-toluenesulfonic acid solution to the material obtained in the step (1) is 55-65 mL: 2-4 g.
4. The method of claim 1, wherein: in the step (3), the filtrate is diluted with distilled water until the concentration of p-toluenesulfonic acid is 3 to 5 wt%.
5. Use of light-colored bagasse-based lignin prepared by a process as claimed in any one of claims 1 to 4 for the preparation of sunscreen compositions.
6. The use of claim 5, wherein: the bagasse-based lignin is present in the sunscreen composition in an amount of 2-5 wt%.
7. A sunscreen composition characterized by: the effective component of the light-color bagasse-based lignin comprises the light-color bagasse-based lignin prepared by the preparation method of any one of claims 1 to 4.
8. A sunscreen composition according to claim 7 wherein: the content of the bagasse-based lignin is 2-5 wt%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111803402A (en) * | 2020-08-21 | 2020-10-23 | 长春科技学院 | Preparation method of lignin-based sunscreen cream |
| CN112480429A (en) * | 2020-12-09 | 2021-03-12 | 国际竹藤中心 | Preparation method and application of bamboo nano lignin sun-screening agent |
| CN112552925A (en) * | 2020-12-14 | 2021-03-26 | 北部湾海洋新材料研究院 | Drought-resistant water-retaining material for agriculture and forestry |
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| CN115838482A (en) * | 2022-11-09 | 2023-03-24 | 广东工业大学 | Light-color lignin and preparation method and application thereof |
| CN115838482B (en) * | 2022-11-09 | 2024-05-10 | 广东工业大学 | Light-colored lignin and preparation method and application thereof |
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